i

GA-Al4690
uc-77
ASSESSMENT OF GRADE H-451
GRAPHITE FOR REPLACEABLE FUEL
AND REFLECTOR ELEMENTS IN HTGR
bY
G. B. ENGLE
Prepared under
Contract EY-76-C-03-0167
Project Agreement No. 17
for the San Francisco Operations Office
Department of Energy
\
DATE PUBLISHED: DECEMBER 1977
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rponrored by t he United Stater Government. Neither t h e
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or usefulness of any information, apparatus. product or
process disclosed, or reprerenu that its usc would not
GA-A14690
uc-77
ASSESSMENT OF GRADE H-451
GRAPHITE FOR REPLACEABLE FUEL
AND REFLECTOR ELEMENTS IN HTGR
Prepared under
Contract EY-76-C-03-0167
Project Agreement No. 17
for the San Francisco Operations Office
Department of Energy
GENERAL ATOMIC PROJECT 3224
DATE PUBLISHED: DECEMBER 1977
GENERAL ATOMIC COMPANY
ABSTRACT
Experi mental data f or grade H-451 graphi te are presented and assessed
to support l i censi ng of H-451 graphi te f or use as f uel element bl ocks i n a
hi gh-temperature gas-cooled reactor (HTGR). Addi ti onal data from the l i ter-
ature on graphi te grades si mi l ar to grade H-451 are presented to supplement
the H-451 data. Eval uati on programs at General Atomic Company (GA) coveri ng
characteri zati on, i rradi ati on, and oxi dati on studi es, al ong wi th studi es
carri ed out i n the Great Lakes Carbon Corporati on H-451 development program,
are reported.
Grade H-451 i s a hi gh-puri ty graphi te manufactured by extrusi on as l ogs
432 mm i n di ameter by 864 mm i n l ength from a speci al bl end of near-i sotropi c
petrol eum coke usi ng conventi onal graphi te manufacturi ng processes.
type, preproducti on, and producti on l ogs have been eval uated by systemat-
i cal l y measuring physi cal and mechanical properti es, i mpuri ty content, and
f ati gue behavi or. Control l ed i rradi ati on experi ments, carri ed out i n i nstru-
mented capsul es, wer e uti l i zed to provi de data over the temperature and
fl uence l i f e of f uel el ements i n an HTGR.
ci ents were taken from l i terature val ues on H-451 and graphi tes s i mi l ar to
H-451. Oxi dati on rates i n helium-water mi xtures and the ef f ect of oxi dati on
burnoff on strength and el asti c modulus of H-451 are reported.
Proto-
I rradi ati on-i nduced creep coef f i -
Grade H-451 shows an improvement i n radi al strength and thermal con-
ducti vi ty over H-327, a needle-coke graphi te, which i s currentl y used f or
HTGR repl aceabl e f uel and ref l ector el ements.
ani sotropy f actor. Overal l , H-451 w i l l provi de better saf ety margi ns i n the
Fort St. Vrai n (FSV) reactor and more f l exi bi l i ty i n desi gn f or f uture HTGRs.
Grade H-451 a+o has a l ower
iii.
n
Q
.
CONTENTS
8
ABSTRACT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i i i
1 . SUMMARY AND CONCLUSI ONS . . . . . . . . . . . . . . . . . . . . 1-1
1.1. I nt r oduct i on . . . . . . . . . . . . . . . . . . . . . . . 1-1
1.2. Concept and Need f or a Near - I sot r opi c Fuel El ement
Gr aphi t e . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
1.3. Devel opment Pr ogr amat GLCC . . . . . . . . . . . . . . . 1-2
1.4. Char act er i zat i on Pr ogr am. . . . . . . . . . . . . . . . . 1-5
Di st r i but i on of Pr oper t i es Wi t hi n I ndi vi dual
Logs and Bet ween Logs Wi t hi n a Lot . . . . . . . . 1-5
St at i st i cal Di st r i but i on of St r engt h Wi t hi n
aL og . . . . . . . . . . . . . . . . . . . . . . 1-6
Def i ni t i on of Mi ni mumSt r engt h and St r engt h
Di st r i but i on Among Logs . . . . . . . . . . . . . 1-7
1.4.4. Fat i gue Behavi or . . . . . . . . . . . . . . . . . 1-8
1.5. I r r adi at i on Pr ogr am . . . . . . . . . . . . . . . . . . . 1-9
1.5.1. Di mensi onal Changes . . . . . . . . . . . . . . . 1-9
1.5.2. Tensi l e St r engt h and El ast i c Modul us . . . . . . . 1-9
1.5.3. Fat i gue Behavi or . . . . . . . . . . . . . . . . . 1-10
1.5.4. Ther mal Expansi vi t y . . . . . . . . . . . . . . . 1-10
1. 5. 5. Thermal Conductivity . . . . . . . . . . . . . . . 1-10
1.5.6. I r r adi at i on- I nduced Cr eep . . . . . . . . . . . . 1-11
1.6. Oxi dat i on Pr ogr am. . . . . . . . . . . . . . . . . . . . . 1-12
1.6.1. Oxi dat i on Rat e of H-451 Gr aphi t e . . . . . . . . . 1-12
1.6.2. Ef f ect of Oxi dat i on on Tensi l e St r engt h and
El ast i c Modul us . . . . . . . . . . . . . . . . . 1-12
1.4.1.
1.4.2.
1.4.3.
2 . I NTRODUCTI ON . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
3 . CONCEPT AND NEED FOR A NEAR- I SOTROPI C FUEL ELEMENT GRAPHI TE . . 3-1
4 . DEVELOPMENT PROGRAMAT GLCC . . . . . . . . . . . . . . . . . . 4-1
4.1. Fi l l er Cokes . . . . . . . . . . . . . . . . . . . . . . . 4-1
4.2. Pr ocessi ng . . . . . . . . . . . . . . . . . . . . . . . . 4-4
V
4. 3. Prototype and Preproducti on Development . . . . . . . . . .
4. 4. Conclusions . . . . . . . . . . . . . . . . . . . . . . . .
REFERENCE . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5 . CHARACTERI ZATI ON PROGRAM . . . . . . . . . . . . . . . . . . . .
5. 1. I ntroducti on . . . . . . . . . . . . . . . . . . . . . . .
5. 2. Di stri buti on of Properti es Within I ndi vi dual Logs and
Between Logs Within a Lot
5. 2. 1. Sampling . . . . . . . . . . . . . . . . . . . . .
5. 2. 2. Bulk Densi ty . . . . . . . . . . . . . . . . . . .
5. 2. 3. Mechanical Properti es . . . . . . . . . . . . . . .
5. 2. 4. Thermal Properti es . . . . . . . . . . . . . . . .
5. 2. 5. I mpuri ty Content . . . . . . . . . . . . . . . . .
5. 2. 6. Concl usi ons . . . . . . . . . . . . . . . . . . . .
5. 3. Stati sti cal Di stri buti on of Strength Within a Log . . . . .
5 . 3 . 1 . Sampling . . . . . . . . . . . . . . . . . . . . . .
5. 3. 2. Concl usi ons . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . .
5. 4. Def i ni ti on of Minimum Strength and Strength Di stri buti on
Among Logs . . . . . . . . . . . . . . . . . . . . . . . .
5. 4. 1. Sampling . . . . . . . . . . . . . . . . . . . . .
5. 4. 2. Experi mental Resul ts . . . . . . . . . . . . . . .
5. 4. 3. Appl i cati on of Resul ts to Acceptance Testi ng . . .
5. 4. 4. Concl usi ons . . . . . . . . . . . . . . . . . . . .
5. 5. Fati gue Behavior . . . . . . . . . . . . . . . . . . . . .
5. 5. 1. Sampling . . . . . . . . . . . . . . . . . . . . .
5. 5. 2. Experi mental Procedure . . . . . . . . . . . . . .
5. 5. 3. Experi mental Resul ts . . . . . . . . . . . . . . . .
5. 5. 4. Concl usi ons . . . . . . . . . . . . . . . . . . . .
REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . .
6 . I RRADI ATI ON PROGRAM . . . . . . . . . . . . . . . . . . . . . . .
6. 1. I ntroducti on . . . . . . . . . . . . . . . . . . . . . . .
6. 2. Sampling . . . . . . . . . . . . . . . . . . . . . . . . .
6. 3. Dimensional Changes . . . . . . . . . . . . . . . . . . . .
6. 3. 1. 873 to 1673 K ( 600" to 1400C) . . . . . . . . . .
6. 3. 2. 573 to 873 K (300" to 600C) . . . . . . . . . . .
4-4
4-6
4-6
5-1
5-1
5-1
5-1
5-2
5-2
5-4
5-6
5-14
5-15
5-16
5-16
5-17
5-17
5-18
5-20
5-26
5-27
5-28
5-28
5-28
5-31
5-31
6-1
6-1
6-3
6-3
6-3
6-7
vi
6.4. Tensi l e St rengt h. El ast i c Modul us. and St r ai n at Fr act ur e . . 6-9
6.4.1. 823 to 1623 K (550' t o 1350C) . . . . . . . . . . . 6-9
6.4.2. 627 to 873 K (350" to 600C) . . . . . . . . . . . . 6-10
6.4.3. Bet ween- Log and Wi t hi n- Log Var i at i ons i n
St r engt h I ncr ease . . . . . . . . . . . . . . . . . . 6-11
6.5. Fat i gue Behavi or . . . . . . . . . . . . . . . . . . . . . . 6-13
6.5.1. Sampl i ng and Pr ocedur es . . . . . . . . . . . . . . . 6-13
6.5.2. Exper i ment al Resul t s and Di scussi on . . . . . . . . . 6-13
6.6.1. 823 to 1623 K (550" to 1350C) . . . . . . . . . . . 6-15
6.6. Ther mal Expansi vi t y . . . . . . . . . . . . . . . . . . . . . 6-15
6.6.2. 623 to 823 K (350" to 550C) . . . . . . . . . . . . 6-17
6.7. Ther mal Conduct i vi t y . . . . . . . . . . . . . . . . . . . . 6-17
6.7.1. 923 to 1623 K (650" t o 1350C) . . . . . . . . . . . 6-17
6.7.2. 523 to 923 K (250" to 650C) . . . . . . . . . . . . 6-19
6.7.3. Ef f ect of Change i n Temper at ur e . . . . . . . . . . . 6-20
6.8. I r r adi at i on- I nduced Cr eep . . . . . . . . . . . . . . . . . . 6-20
6.8.1. Concl usi ons . . . . . . . . . . . . . . . . . . . . . 6-21
REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21
7 . OXI DATI ON PROGRAM . . . . . . . . . . . . . . . . . . . . . . . . 7-1
7.1. Oxi dat i on Rat e of H-451 Gr aphi t e . . . . . . . . . . . . . . 7-1
7.1.1. React i on Rat e Theor y . . . . . . . . . . . . . . . . 7-1
7.1.2. Exper i ment al Pr ocedur e and Sampl i ng . . . . . . . . 7-3
7.1.3. Det er mi nat i on of React i on Rat e Const ant s . . . . . . 7-4
7. 1. 4. Application of Rate Constants . . . . . . . . . . . 7-6
Ef f ect of St eamOxi dat i on on Tensi l e St r engt h and
El ast i c Modul us . . . . . . . . . . . . . . . . . . . . . . 7-8
7.2.1. Exper i ment al Pr ocedur e and Sampl i ng . . . . . . . . 7-8
7.2.2. Exper i ment al Resul t s . . . . . . . . . . . . . . . . 7-9
7.2.
REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22
8 . ACKNOWLEDGMENTS . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
APPENDI X A: SAMPLI NG DI AGRAMS . . . . . . . . . . . . . . . . . . . . A- 1
APPENDI X B: RESULTS OBTAI NED DURI NG ASSESSMENT PROGRAM . . . . . . . B-1
FI GURES
1 . 1 . Compar i son of di mensi onal changes for H- 451 and H- 327 gr aphi t es:
(a) axi al . (b) r adi al . . . . . . . . . . . . . . . . . . . . . 1-4
vi i
6-1.
6-2.
6-3.
6-4.
7-1.
7-2.
7-3.
7-4.
7-5.
7-6.
7-7.
7-8.
7-9.
A-1.
A-2.
A-3.
A-4.
A-5.
H-451 gr aphi t e i r r adi at i on dat a . . . . . . . . . . . . . . . . 6-2
I r r adi at i on- i nduced di mensi onal change i n H-451 gr aphi t e
( desi gn curves): (a) axi al di r ect i on, (b) r adi al di r ect i on . . 6-5
Di mensi onal changes i n H-451 gr aphi t e i r r adi at ed wi t h
Fat i gue st r ess l i mi t s f or sur vi val of H-451 gr aphi t e t o
105 cycl es, nor mal i zed to t he uni r r adi at ed t ensi l e st r engt h,
ver sus t he f ast neut r on f l uence at an i r r adi at i on t emper at ur e
of 1173 to 1263 K (900" t o 990C) . . . . . . . . . . . . . . . 6-16
Compar i son of r at e const ant s as a f unct i on of PH 0 ( f rom
Ref . 7-2). . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7
Tensi l e st r engt h ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quar t er - l engt h axi al edge and cent er speci mens)
Tensi l e st r engt h ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quar t er - l engt h axi al speci mens) oxi di zed at
Tensi l e st r engt h ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quarter-length axial center specimens) . . . . . . . . 7-16
Tensi l e st r engt h ver sus bur nof f for H-451 gr aphi t e (l og
6484-34, quar t er - l engt h r adi al speci mens) oxi di zed at
Tensi l e st r engt h ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quar t er - l engt h r adi al speci mens) oxi di zed at
El ast i c modul us ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quar t er - l engt h axi al cent er speci mens) . . . . . . . . 7-19
El ast i c modul us ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quar t er - l engt h axi al speci mens) oxi di zed at
El ast i c modul us ver sus bur nof f f or H-451 gr aphi t e ( l og
6484-34, quar t er - l engt h r adi al edge speci mens) oxi di zed at
1273 K (1000C). . . . . . . . . . . . . . . . . . . . . . . . . 7-21
Sampl i ng di agr amof H-451 f or wi t hi n- l og pr oper t y
measur ement s: sl abs and sect i ons . . . . . . . . . . . . . . . A-3
Sampl i ng di agr amof H-451 f or wi t hi n- l og pr oper t y
measur ement s: cent er sect i on showi ng speci men l ocat i ons . . . . A-4
Sampl i ng di agr amof H-451 f or wi t hi n- l og pr oper t y
measur ement s: edge sect i on showi ng speci men l ocat i ons . . . . . A-5
Or i ent at i on of or t hogonal axes f or def i ni t i on of Poi sson' s
r at i o dat a i n Tabl e B-4 . . . . . . . . . . . . . . . . . . . . A-6
Locat i ons of sl abs ( shaded) f or st at i st i cal st r engt h
t est i ng H-451 gr aphi t e ( l og 5651-90) . . . . . . . . . . . . . . A-7
changes i n t emper at ur e ( f romRef . 6-3) . . . . . . . . . . . . . 6-6
2
oxi di zed at 1073 K (800C) . . . . . . . . . . . . . . . . . . . 7-14
1273K(1000C) . . . . . . . . . . . . . . . . . . . . . . . . 7-15
1073K (800C) . . . . . . . . . . . . . . . . . . . . . . . . . 7-17
1273 K (1000C) . . . . . . . . . . . . . . . . . . . . . . . . 7-18
1273 K (1000C) . . . . . . . . . . . . . . . . . . . . . . . . 7-20
n
vi i i
A- 6. Coring pl an f or center zone of A and B secti ons of sl abs
(see Fi g. A- 5) . . . . . . . . . . . . . . . . . . . . . . . .
A- 7. Coring pl an f or edge zone of A and B secti ons of sl abs
(see Fi g. A- 5) . . . . . . . . . . . . . . . . . . . . . . . .
A- 8 . Sampling diagram of H- 451 l ogs for tensi l e strength. . . . . .
A- 9. Sampling diagram of H- 451 l og sample core (see Fi g. A-8):
axi al specimens . . . . . . . . . . . . . . . . . . . . . . .
A- 10. Sampling diagram of H- 451 l og sl ab (see Fi g. A-8):
radi al specimens . . . . . . . . . . . . . . . . . . . , . .
A- 11. Coring diagram f or uni rradi ated H- 451 f ati gue specimens;
edge zone, from sl ab 2 (see Fi g. A- 5) . . . . . . . , . . . .
A- 12. Sampling diagram f or i rradi ati on specimens: center zone,
from sl ab 3 (see Fi g. A- 1) . . . . . . . . . . . . . . . . . .
A- 13. Sampling diagram f or i rradi ati on specimens: outer zone,
edge secti on from sl ab 3 (see Fi g. A- 1) . . . . . . . . . . .
A- 14. Sampling pl an of graphi te l og showing sl ab desi gnated
f or oxi dati on tests. . . . . . . . . . . . . . . . . . . . . .
A- 15. Sampling pl an of H- 451 showing secti oni ng of a sl ab
A- 16. Sampling diagram of H- 451 graphi te: center secti on of
A- 17. Sampling diagram of H- 451 graphi te: edge secti on of
B- 1. Fati gue test data: i n ai r l og-l og pl ot of normal i zed
from Fi g. A- 14 . . . . . . . , . . . . . . . . . . . . . . . .
sl ab from Fi g. A- 15 . . . . . . . . , . . . . . . . . . . . .
sl ab from Fi g. A- 15 . . . . . . . . . . . . . . . . . . . . .
peak stress versus number of cycl es to f ai l ure wi th
R = - 1; lower x/y tol erance l i mi t s represent l i mi t s above
which x% of al l data would f al l , wi th y% confi dence; axi al
specimens; open ci rcl es represent run-outs (from Ref. 5-10). .
B-2. Const ant l i f e f at i gue di agr am ( Goodman di agr am) f or H- 451
graphi te: axi al di recti on (from Ref, 5-10). . . . . . . . . .
i rradi ati on temperatures 875 K t o 975 K and 1075 K to 1175 K
( 602" to 702C and 802" t o 902C) (from Ref. 6- 3) . , . , . .
i rradi ati on temperatures 1275 K t o 1375 K and 975 K to 1075 K
( 1002" to 1102C and 702" to 802C) (from Ref. 6-3) . . , , .
i rradi ati on temperatures 1175 K to 1275 K (902' to 1002C)
(fromRef. 6-3). . . . . , . . . , . :. . . . . . . . . . . .
B- 3. Dimensional change i n H- 451 graphi te: axi al di recti on;
B- 4. Dimensional change i n H- 451 graphi te: axi al di recti on;
B- 5. Dimensional change i n H- 451 graphi te: axi al di recti on;
A- 8
A- 9
A- 10
A- 11
A- 12
A- 13
A- 14
A- 15
A- 16
A- 17
A- 18
A- 19
B- 22
B- 23
B- 24
B-25
B- 26
' \
i x
B- 6.
B-7.
B-8.
B-9.
B-10.
B-11.
B-12.
B-13.
B-14.
B-15.
B-16.
B-17.
Dimensional change i n H-451 graphi te: axi al di recti on;
i rradi ati on temperatures 1475 K to 1575 K and 1575 K to
1675 K (1202" to 1302C and 1302" to 1402C) (from
Ref . 6- 3) . . . . . . . . . . . . . . . . . . . . . . . . . . . B-27
Dimensional change i n H-451 graphi te: radi al di recti on;
i rradi ati on temperatures 875 K to 975 K and 1475 K to 1575 K
(602' to 702C and 1202" to 1302C) (from Ref. 6-3) . . . . . . B-28
Dimensional change i n H-451 graphi te: radi al . di recti on;
i rradi ati on temperatures 975 K t o 1075 K and 1275 K to
1375 K (702" to 802C and 1002" to 1102C) (f rom
Ref. 6 - 3 ) . . . . . . . . . . . . . . . . . . . . . . . . . . . B-29
Dimensional change i n H-451 graphi te: radi al di recti on;
i rradi ati on temperatures 1175 K to 1275 K (902" to 1002C)
(f romRef .6- 3) . . . . . . . . . . . . . . . . . . . . . . . . B - 3 0
Dimensional change i n H-451 graphi te: radi al di recti on;
i rradi ati on temperatures 1075 K to 1175 K (802" to 902OC
and 1302" to 1402OC) (from Ref. 6-3) . . . . . . . . . . . . . B-31
Dimensional changes i n near-i sotropi c graphi te i rradi ated
at 633 K to 773 K (360" t o 500C) (data from Refs, 6-4
and6- 6). . . . . . . . . . . . . . . . . . . . . . . . . . . . R-32
Dimensional changes i n near-i sotropi c graphi te i rradi ated
at 773 K to 873 K (500" to 600C) (data from Refs. 6-4
and6- 6). . . . . . . . . . . . . . . . . . . . . . . . . . . . B-33
Changes i n tensi l e strength and el asti c modulus of H-451
graphi te as a f uncti on of f ast neutron fl uences.
Error
bars denote 5 one standard devi ati on (from Ref. 6-3). . . . . . B-34
Fracti onal changes i n soni c el asti c modulus of extruded
near-i sotropi c pi tch coke graphi te (Dragon code No. 100)
(from Ref. 5-7) . . . . . . . . . . . . . . . . . . . . . . . . B-35
Change i n the soni c el asti c modulus (E) and strength (S)
of near-i sotropi c graphi te i rradi ated at 623 K to 973 K
at (350" t o 700C) (from Ref. 6-8). . . . . . . . . . . . . . . B-36
Cal cul ated percent i ncreases i n stati c el asti c modulus of
near-i sotropi c graphi tes (sol i d parts of curves correspond
to data i n Refs. 6-6 and 6-8; broken parts are extrapol ated).
. B-37
Fati gue test data i rradi ated to 3.0 x 1025 N/m2 (E > 29 fJ l HTGR
at 1173 K (900C). Log-log pl ot of normal i zed peak stress
versus number of cycl es to f ai l ure, wi th stress rati o,
R =-1. Lower x/y tol erance l i mi t s represent the l i mi t s
above which x% of al l data would f al l , wi th y% confi dence;
axi al specimens; open circles represent run-outs (from
Ref. 5-10). . . . . . . . . . . . . . . . . . . . . . . . . . . B-38
X
B-18. Percent change i n thermal expansi vi ty E295 K to 773 K (22"
to 500C)] of near-i sotropi c graphi tes as a functi on of
f ast neutron fl uence: i rradi ati on temperature 865 K to
1205 K (592" to 932OC) (from Ref. 6-3) . . . . . , . . . . . . B-39
B-19. Percent change i n thermal expansi vi ty [295 K to 773 K (22"
to 500C)] of near i sotropi c graphi tes as a functi on of
f ast neutron fl uence: i rradi ati on temperature 1250 K t o
1705 K (592" to 932C) (from Ref. 6-3) . . . . . . . , , . . . B-40
B-20. Change i n thermal expansi vi ty of near-i sotropi c graphi te
i rradi ated at 350" to 550C (data from Ref. 6-4) . . . . . . . B-41
B-21. Thermal conducti vi ty at the i rradi ati on temperature f or
H-451 and other near-i sotropi c graphi tes as a functi on of
f ast neutron fl uence (from Ref. 6-3) . . . . . . . . . . . . . B-42
near-i sotropi c graphi te (data poi nts from Refs. 6-6 and
6-8; curves from Ref. 6-10). . . . . . . . , . . . . . . . . . B-43
B-22. I rradi ati on-i nduced changes i n thermal resi sti vi ty of
TABLES
1-1. Comparison of H-451 and H-327 properti es . . . . . . . . . . .
4-1. Mi crostructural anal ysi s of cal ci ned cokes used to
manufacture H-451 graphi te . . . . . . . . . . . . . . . . . .
4-2. H-451 lots manufactured by (;LCC ,ind l og di stri buti ons
duri ng development program . . . . . . . . . . . . . . . . . .
4-3. Programs uti l i zi ng H-451 graphi te l ogs . . . . . . . . . . . .
5-1.
l ot 426, l og 6484-34 . . . . . . . . . . . . . . . . . . . . .
5-2. I mpuri ty content: H-451, l ot 426 . . . . . . . . . . . . . .
5-3. Summary of l i thi um anal yses: H-451 . . . . . . . . . . . . .
5-4. I mpuri ty content: H-451 . . . . . . . . . . . . . . . . . . .
5-5. Stati sti cal anal yses of GA and GLCC axi al strength data. . . .
5-6. Stati sti cal anal ysi s of radi al strength data . . . . . . . . .
5-7. Components of vari ance: axi al strength data . . . . . . . . .
5-8. Cri teri a f or assi gni ng l ogs to strength categori es A, B, or
C (axi al data) . . . . . . . . . . . . , . . , . . . . . . . .
5-9. Y i el ds of l ogs i n each strength category (based on axi al
strengths) . . . , . . . . . . . , . . . . . . . , . . . . . .
5-10. Stati sti cal anal yses of f ati gue data f or uni rradi ated H-451
graphi te . . . . , . . . . . . . , . . . . . . . . . . . . . .
Summary of boron equi val ent test data on H-451,
1-3
4-3
4-5
4-7
5-8
5-1 2
5-1 3
5-1 4
5-19
5-20
5-21
5-24
5-25
5-30
xi
n
6- 1. Wi t hi n- l og var i at i on i n i r r adi at i on- i nduced shr i nkage of
Bet ween- l og var i at i ons i n i r r adi at i on- i nduced shr i nkage
of H- 451 gr aphi t e, Lot 426 . . . . . . . . . . . . . . . .
H- 451 gr aphi t e, Lot 426 . . . . . . . . . . . . . . . . . .
6- 2.
6- 3. Bet ween- l og var i at i ons i n i r r adi at i on- i nduced st r engt h
6- 4.
6- 5. Resul t s of st at i st i cal anal ysi s of f at i gue dat a f or H- 451
i ncr ease of H- 451 gr aphi t e, Lot 426 . . . . . . . . . . . .
Wi t hi n- l og var i at i ons i n i r r adi at i on- i nduced st r engt h
i ncr ease of H- 451 gr aphi t e, axi al di r ect i on . . . . . . . .
gr aphi t e i r r adi at ed at 1173 t o 1263 K (900' t o 990C)
6- 6. I ncr ease i n t her mal expansi vi t y of near - i sot r opi c gr aphi t e
7- 1. Exper i ment al l y det er mi ned Langmui r - Hi nshel wood const ant s
7- 2.
7-3. Reduct i on i n ul t i mat e t ensi l e st r engt h and el ast i c modul us
wi t h oxi dat i on . . . . . . . . . . . . . . . . . . . . . .
B- 1. Bul k densi t y: H- 451, Lot 426 . . . . . . . . . . . . . . .
B- 2. Ul t i mat e t ensi l e st r engt h: H- 451, Lot 426 . . . . . . . .
B- 3. El ast i c modul us i n t ensi on: H- 451, Lot 426 . . . . . . . .
B- 4. Poi sson' s r at i o: H- 451, Lot 266 . . . . . . . . . . . . .
B- 5. Fl exur al st r engt h: H- 451, Lot 426 . . . . . . . . . . . .
B- 6. Ul t i mat e compr essi ve st r engt h and el ast i c modul us i n
B- 7. Ther mal expansi vi t y: H- 451, Lot 426 . . . . . . . . . . .
B- 8. Ani sot r opy f act or : H- 451, Lot 426 . . . . . . . . . . . .
B-9. Ther mal conduct i vi t y: H- 451, Lot 426, MLC . . . . . . . .
B- 10. Mean t ensi l e st r engt h of uni r r adi at ed H- 451 gr aphi t e
speci mens used i n f at i gue st udy . . . . . . . . . . . . . .
B- 11. I r r adi at i on condi t i ons and mean t ensi l e st r engt h of
i r r adi at ed H- 451 gr aphi t e used i n f at i gue st udy ( al l
( st r ess r at i o, R =- 1) . . . . . . . . . . . . . . . . . .
i r r adi at ed bet ween 623 and 823 K ( 350" and 550C) . . . . .
f or H- 451 gr aphi t e. . . . . . . . . . . . . . . . . . . . .
Summar y of UTS and el ast i c modul us dat a and compar i son of
popul at i on means of nonoxi di zed and oxi di zed speci mens. . .
compr essi on: H- 451, Lot 478. . . . . . . . . . . . . . . .
speci mens MLC l ocat i on) . . . . . . . . . . . . . . . . . .
B- 12. Summar y of i r r adi at i on- i nduced changes i n t her mal
expansi vi t y of H- 451 gr aphi t e i r r adi at ed i n capsul es
OG- 1, OG- 2, and OG- 3 . . . . . . . . . . . . . . . . . . .
expansi vi t y of H- 429 gr aphi t e i r r adi at ed i n capsul es
OG- 1, OG- 2, and OG- 3 . . . . . . . . . . . . . . . . . . .
B- 13. Summar y of i r r adi at i on- i nduced changes i n t her mal
6- 8 . .
6- 8 . .
. .
. .
6- 1 2
6- 12
6- 14 . .
6- 1 8 . .
7- 4 . .
7-1 1 . .
7-1 2
B- 3
B- 4
B- 5
B- 6
B- 7
. .
. .
. .
. .
. .
. .
B- 8
B- 9
B- 10
B- 11
. .
. .
. .
. .
B- 11 . .
B- 12 . .
B- 13 . .
B- 14 . .
xii
U- 14. Summar y of i r r adi nt i on- i nduced cliniiges I n thermal expansi vl t y
of TS- 1240 gr aphi t e i r r adi at ed i n capsul es OG-2 and OG-3 . . . . B-15
B-15. Summar y of i r r adi at i on- i nduced changes i n t her mal expansi vi t y
of SO818 gr aphi t e i r r adi at ed i n capsul e OG-3 . . . . . . . . . . B-16
B-16. Summar y of f r r adi at i on- i nduced changes i n t her mal conduct i vi t y
of H-451 gr aphi t e i r r adi at ed i n capsul es OG-1, OG-2, and
OG-3 ( al l speci mens f r omMLC of par ent l og) . . . . . . . . . . B-17
B-17. Summar y of i r r adi at i on- i nduced changes i n t her mal conduct i vi t y
of TS- 1240 gr aphi t e i r r adi at ed i n capsul es OG-2 and OG-3
( al l speci mens f r omMLC of par ent l og) . . . . . . . . . . . . . B-18
B-18. Summar y of i r r adi at i on- i nduced changes i n t her mal conduct i vi t y
of SO818 gr aphi t e i r r adi at ed i n capsul e OG-3 ( al l speci mens
f r omMLC of par ent l og). . . . . . . . . . . . . . . . . . . . . B-19
B- 19. Cal cul at ed t her mal conduct i vi t y at i r r adi at i on t emper at ur e
of near - i sot r opi c gr aphi t e i r r adi at ed bet ween 573 and 873 K
B- 20. Al l ocat i on of gr aphi t e sampl es f or oxi dat i on st udi es
( 300" and 600OC) . . . . . . . . . . . . . . . . . . . . . . . . B-20
( number of speci mens) . . . . . . . . . . . . . . . . . . . . . B-21
xi i i
1. SUMMARY ANI) CONCLUSIONS
1. 1. I NTRODUCTI ON
Grade H-451 graphi te, devel oped excl usi vel y by the Great Lakes Carbon
Corporati on (GLCC) f or HTGR f uel el ement bl ocks, has been eval uated exten-
si vel y i n preparati on f or i ts i ntroducti on i nto the hi gh-temperature gas-
cool ed reactor (HTGR). Thi s report summarizes the data on grade H-451 and
data from the l i terature on graphi tes si mi l ar to H-451 that were used as a
basi s f or prepari ng the Graphi te Fuel Element secti on of the Fuel Design Data
Manual (GA-AI 44 29) .
The f i ve major secti ons of thi s report descri be: (1) the concept and
need f or a near-i sotropi c f uel el ement graphi te, (2) the development program
at GLCC, ( 3 ) the characteri zati on program, (4) the i rradi ati on program, and
(5) the oxi dati on program. Appendix A contai ns sampl i ng pl ans f or the pro-
gram, and data obtai ned are presented i n the f i gures and tabl es of Appendix B.
Thi s report i s suppl emental to the Materials Speci f i cati on f or Repl aceabl e
Fuel and Ref l ector Element Graphi tes (Number 900739) and the Graphi te Fuel
Element secti on of the Fuel Design Data Manual (GA-A14429).
1.2. CONCEPT AND NEED FOR A NEAR-ISOTROPIC FUEL ELEMENT GRAPHITE
T he pri mary i ncenti ve f or devel opi ng a near-i sotropi c graphi te to
repl ace needle-coke graphi te grade H-327 f or HTGR f uel el ements was to
improve di mensi onal stabi l i ty, strength, and thermal conducti vi ty and thus
improve performance, saf ety margi ns i n FSV, and f l exi bi l i ty i n desi gn f or
f uture HTGRs.
1- 1
The data i n Tabl e 1-1 show a comparison of properti es between grades
H-451 and H-327 i n the uni rradi ated state and af ter i rradi ati on to end-of-
l i f e HTGR fl uences.
thermal conducti vi ty i n the i rradi ated state. The thermal expansi vi ty of
H-451 i s hi gher than that of H-327 i n the uni rradi ated state, but the
thermal expansi vi ty of H-451 decreases wi th i rradi ati on whereas it remains
unchanged f or H-327.
H-451 but H-327 has a hi gher modulus i n the axi al di recti on. A comparison
of di mensi onal changes i s shown i n Fi g. 1-1. Grade H-451 has a lower ani so-
tropy f actor f or di mensi onal change, and radi al expansi on i s del ayed to
beyond the end-of-l i fe HTGR fl uences at peak HTGR temperatures.
The major improvement i s i n the radi al strength and
Grade H-327 has a lower radi al el asti c modulus than
I n addi ti on to the improved properti es and i rradi ati on behavi or, the
near-i sotropy i n properti es and di mensi onal changes greatl y si mpl i f i es
desi gn cal cul ati ons over the more ani sotropi c needle-coke grade H-327.
1.3. DEVELOPMENT PROGRAM AT GLCC
GLCC developed two si mi l ar near-i sotropi c petrol eum cokes, desi gnated
A and C, from two sources f or producti on of near-i sotropi c graphi tes. The
cokes were examined by metal l ographi c techni ques at GA and judged to have
sati sf actory mi crostructures f or f uel element graphi tes. A prototype grade
H-429 was prepared wi th coke A and submi tted f or earl y i rradi ati on experi -
ments. Cokes A and C were bl ended wi th coke B, a regul ar producti on coke,
to devel op grade H-451. A number of preproducti on l ots were manufactured,
usi ng cokes A through A i n combi nati on wi th cokes B1 through B and
eval uated at GA. Preproducti on l ot 426, manufactured wi th cokes A and B
was chosen f or producti on. Approximately 98 H-451 producti on l ogs were
eval uated f or strength, and about 300 H-451 l ogs have been di spersed f or
vari ous studi es on programs at GA, ORNL, BNL, and the European HTGR programs.
1 3 3
2 3
1-2
I
Y
12.8
12.0
7.9
6.9
A
I
W
11.2
6.4
10.3
4.0
Property
U1 t ima te
t ens i l e strength,
Axial
Radi a1
El asti c
modulus,
Axial
Radial
Thermal conductivity,
Axial
Radial
Thermal expansivity
a x 10
[295 to 1273 K (22' to
6
10OO0C) J
Axial
Radial -
TABLE 1-1
COMPARISON OF H-451 AND H-327 PROPERTIES
Units
MPa
GPa
W/m*K
c-l ( O f ' )
Unirradiated
H-451 1 H-327
I
58 65 I ::
Irradiated (4
1
1073
H-45 1
23.0
21.5
19.7
17.2
39
34
3.4
4 .O
17.5
8.4
20.1
7.8
37
28
1.9
3.6
(a)End-of-life fluence f or HTGR: 8 x
N/m 2 (E > 29 fJ)HTGR
* ":
K ("C)
1273
H-451
21.5
20.2
17.8
15.5
41
37
2.7
3.1
1000)
H-327
16.7
8.1
18.6
7.2
41
29
1.8
3.4
:I
0
-1.0
-
ae
-
2 -2.0
a
-l
w
a
z
0
-I
z
v)
9 -3.0
a
El
5 -4.0
I
0
-5.0
-6.0
H-327
J
6 1 a
I I I
I I I
I
2 3 4 5
0 1
FAST NEUTRON FLUENCE X
(b)
RADIAL)
N/m2 ( E >29 FJ ~HTGR
I
6 7 a
I I I
I I I I
3 4 5
0 1 2
FAST NEUTRON FLUENCE (loz5 N d ) (E >29 FJ)HTGR
Fig. 1-1.
Comparison of dimensional changes f or H-451 and
H-327 graphites: (a) axial, (b) radial.
1-4
n
1.4. CHARACTERI ZATI ON PROGRAM
1.4.1. Di stri buti on of Properti es Wi thi n I ndi vi dual Logs and Between
Logs Wi thi n a Lot
A number of H-451 producti on l ots were eval uated to determi ne the
di stri buti on of properti es wi thi n si ngl e l ogs and between l ogs i n a si ngl e
l ot. Properti es measured were bul k densi ty, mechanical properti es i ncl ud-
i ng strength, el asti c modulus, strai n-at-f racture, and Poi sson's rati o i n
tensi on, f l exural strength, strength and el asti c modulus i n compression,
thermal expansi vi ty, thermal conducti vi ty, and i mpuri ty content. Measure-
ments were made at four l ocati ons wi thi n a l og:
mi dl ength edge (MLE), end center (EC), and end edge (EE) .
mi dl ength center (MLC),
Mean property val ues al ong wi th standard devi ati ons and di stri buti ons
of the val ues wi thi n the l ogs and l ots are gi ven i n Secti on 5. The H-451
l ogs are weakest at thei r mi dl ength center l ocati on. Thi s characteri sti c
makes i t mandatory to sampl e the H-451 graphi te f or acceptance strength
testi ng at or near the mi dl ength center of each l og.
The radi al strength of H-451 i s about 80% greater than that of H-327
(the needle-coke graphi te used to manufacture FSV f uel el ements). The
thermal conducti vi ty i n the radi al di recti on i s al so hi gher than that of
H-327. These benef i ts resul ti ng from the use of near-i sotropi c coke w i l l
improve i n-servi ce saf ety margins i nvol vi ng secondary stresses.
The i mpuri ty content was found to be hi ghest i n the center of the l og;
thus, testi ng f or acceptance shoul d paral l el the procedure outl i ned f or
strength. The i mpuri ty content i s a functi on of the degree of puri f i cati on
i n each graphi ti zati on furnace run duri ng manufacture. Mean ash contents
were found to vary from 25 to 300 ppm depending on the graphi ti zati on
furnace run.
1-5
I n general , i mpuri ti es that catal yze oxi dati on reacti ons, such as i ron,
ti tani um, and vanadium, fol l ow the ash content. Li thi um coul d not be
detected i n H-451 graphi te at the l owest l evel of sensi ti vi ty of the ana-
l yti cal techni ques used (0.005 ppm) .
An anal yti cal techni que was worked out i n col l aborati on among four
l aboratori es, under the gui dance of the ASTM Committee on Nuclear Graphi te,
f or measuring the nonburnable boron equi val ent i mpuri ty content i n H-451
graphi te.
ppm of nonburnable boron equi val ent content i n a sample from a hi ghl y puri -
f i ed l og.
The resul ts of round-robi n tests provi de a val ue of about 0.04
1.4.2. Stati sti cal Di stri buti on of Strength Wi thi n a Log
A log of H-451 graphi te was destructi vel y tested to determi ne the
systemati c vari ati on of strength wi thi n a l og, the rel ati onshi p between
tensi l e and f l exural strength, and the determi nati on of a model appl i cabl e
to H-451 strength di stri buti on. The data were anal yzed usi ng Wei bul l 's
stati sti cal model f or br i ttl e materials.
The H-451 graphi te was found, as i n the earl i er characteri zati on work,
to be stronger i n the axi al di recti on than i n the radi al , and weaker al ong
the central axi s than at the edges. The vari ati on of strength wi thi n a
test zone was l owest f or axi al specimens. Vari ati on i n f l exural strengths
was less than the vari ati on i n tensi l e strengths.
Wi thi n experi mental scatter, the data were equal l y wel l represented by
normal (Gaussi an) di stri buti on or by a di stri buti on predi cted by the Wei bul l
model. The val ue of the Weibull modulus, m, was lower f or tensi l e data than
f or f l exural data. Such a di f f erence i s contrary to predi cti ons based on
the Weibull model. Small specimens averaged 3% and 8% stronger than the
l arger specimens f or axi al and radi al di recti ons, respecti vel y. The
observed "si ze ef f ect" was much lower than expected from the Weibull model,
1-6
which would predi ct di f f erences of 29% and 38% f or axi al and radi al di rect-
i ons, respecti vel y. The mean f l exural strength showed good correl ati on
wi th the mean tensi l e strength of companion specimens (correl ati on coef f i -
ci ent 0.9). Fl exural strength averaged 52% and 55% hi gher than the corre-
sponding tensi l e strength f or axi al and radi al di recti ons, respecti vel y.
These val ues are i n good agreement wi th val ues of 51% axi al and 64% radi al
predi cted by the Weibull model.
While there i s agreement between the experi mental f l exural -to-tensi l e
strength rati os and the rati os predi cted by the Weibull model, the experi -
mental l y deri ved si ze ef f ect and the di f f erence i n Weibull modulus between
tensi l e and f l exural data are i nconsi stent wi th the Weibull model. Thus i t
was concluded that the H-451 graphi te l og tested di d not meet the cri teri a
which would permi t i t to be treated as a Weibull sol i d.
1. 4. 3. Def i ni ti on of Minimum Strength and Strength Di stri buti on Amone. Logs
Tensile strength was measured on ei ght axi al specimens taken from the
mi dl ength center from each of 98 producti on l ogs which were taken from
three producti on l ots. The axi al strengths showed consi derabl e l ot-to-l ot
and l og-to-l og vari ati ons.
Acceptance cri teri a were deri ved f or assi gni ng l ogs to a minimum
strength category based on axi al tensi l e tests, i f each l og i s sampl ed.
A stati sti cal model i ncorporati ng a separate l ot-to-l ot vari ance, log-to-
l og vari ance, and wi thi n-l og vari ance was adopted f or thi s purpose.
Acceptance cri teri a which can be used f or assi gni ng a l ot to strength
category A (minimum strength 10.3 MPa), B (minimum strength 8.3 MPa), or C
(minimum strength 5.5 ma) were deri ved. Cal cul ati ons wer e made f or ei ther
four or ei ght repl i cate specimens per log,, and two al ternati ve def i ni ti ons
of "minimum strength" were consi dered. The f i r st def i ni ti on would requi re
1-7
90% of the material at the mi dl ength center of the l og to exceed the speci -
f i ed minimum strength, wi th 90% confi dence (90/90); the second would requi re
99% of the material to exceed the speci f i ed minimum, wi th 95% confi dence
(99/95).
Appl i cati on of these cri teri a to the axi al test data from the 98 l ogs
provided i nformati on f or acceptance/rej ecti on of the l ogs, f or assi gni ng each
l og to a strength category, and subsequentl y f or assi gni ng each l og to a
speci f i c l ocati on wi thi n the reactor core, i .e., strong l ogs to posi ti ons
of hi gh stress and weak l ogs to posi ti ons of low stress. I t al so Frovided
a cri teri on f or rej ecti ng weak or def ecti ve l ogs duri ng qual i ty testi ng at
a confi dence l evel to be establ i shed by the desi gners.
Anal ysi s of the data, usi ng the acceptance cri teri a, showed that 5 l ogs
w o u l d be rejected f or a 4 - s p e c i me n test a t 90/90 confi dence l evel whereas 18
l ogs would be rej ected f or an 8-specimen test at 99/95 confi dence l evel .
When the anal ysi s was appl i ed to speci f i c l ots the resul ts showed that most
of the rej ected l ogs were i n one weak l ot which had a mean strength si gni -
f i cantl y below the other two.
1.4.4. Fati gue Behavior
Grade H-451 graphi te was tested to determi ne i ts f ati gue l i f e. Fati gue
tests were run over a range from compressi on/tensi on cycl i ng (R val ues -1
and -0.5) and i n tensi on (R val ues 0 and 0.5) .
The H-451 graphi te showed cycl i c f ati gue l i f e curves (S-N curves)
general l y resembl i ng those of metals, but wi th more scatter.
stress cycl i ng (R = - l ) , the homologous stress l i mi t s (maximum appl i ed
f ati gue stress di vi ded by the tensi l e strength) f or 50% specimen survi val
5
to 10 cycl es averaged 0.63 i n the axi al di recti on and 0.74 i n the radi al
di recti on. Corresponding homologous stress l i mi t s f or 99% specimen sur-
vi val (99/95 tol erance l i mi t s ) wer e 0.48 and 0.53. The f ati gue l i f e and
the homologous stress l i mi t s i ncreased as R i ncreased.
For reversed
1-8
.
1.5.2. Tensi l e St r engt h and El ast i c Modul us
1.5. I RRADI ATI ON PROGRAM
1.5.1. Di mensi onal Changes
Di mensi onal changes wer e measur ed f r om873 t o 1623 K (600' t o 1350OC)
i n a ser i es of capsul es i r r adi at ed i n t he t o 9 x N/ m (E > 29 f J )HTGR
ORR. Addi t i onal dat a at 573 to 873 K (300" t o 6OOOC) on gr aphi t es si mi l ar
to H- 451 wer e t aken f romt he l i t er at ur e. The di mensi onal dat a cover t he
t emper at ur e and f l uence r ange of t he HTGR.
2
The di mensi onal changes of H- 451 gr aphi t es at 573 t o 1623 K (300" to
1350OC) f al l wi t hi n an envel ope of 0% and -3% i n t he axi al di r ect i on and
0% and -1.5% i n t he r adi al di r ect i on up t o 9 x 10
whi ch i s about 10% above t he l i f et i me f l uence of t he H-451 gr aphi t e i n
an HTGR.
i r r adi at i on per i od, t he shr i nkage r at e i ncr eased to t hat of t he hi gher
t emper at ur e.
i r r adi at i on per i od, t he shr i nkage r at e al so was r educed, but r emai ned
hi gher t han t he i sot her mal r at e at t he l ower t emper at ur e.
25 2
N/ m (E > 29 f J ) HTGR,
When t he i r r adi at i on t emper at ur e was i ncr eased af t er an i ni t i al
When t he i r r adi at i on t emper at ur e was r educed af t er an i ni t i al
Di f f er ences i n shr i nkage bet ween MLC and MLE speci mens f r omt he same
l og wer e not sat i st i cal l y si gni f i cant , nor wer e t here st at i st i cal l y si gni -
f i cant di f f er ences i n shr i nkage among speci mens t aken f romt he same l ocat i on
i n the l og but f romdi f f er ent l ogs.
Tensi l e st r engt h i ncr eased and el ast i c modul us i ncr eased dur i ng i r r a-
di at i on at 823 t o 1623 K (550" t o 135OOC). Ther e was an i ncr ease i n t he
1-9
standard devi ati on of strength val ues but no change i n the coef f i ci ent of
vari ati on. The i ncrease i n strength i s rel ated to the i ncrease i n el asti c
modulus by
0. 64
0
Within-log vari ati on and l og-to-l og vari ati on of f racti onal strength
i ncrease wer e not si gni f i cant.
1 . 5 . 3 . Fati gue Behavior
n
I rradi ati on i ncreased the homologous stress l i mi t s f or f ati gue endur-
ance of H-451 by about a f actor of 2 when the stresses were normalized by
di vi di ng by the uni rradi ated strength.
1. 5. 4. Thermal Expansi vi ty
I rradi ati on induced an i ncrease of about 20% i n thermal expansi vi ty of
H-451 at 623 to 823 K (350' to 550OC) over the l i f e of the f uel el ement.
The thermal expansi vi ty i ncreased by about 10% at 873 to 973 K (600' to
7OOOC) at low f l uences and returned to the ori gi nal val ues at HTGR end-of-
l i f e. A t 923 to 1673 K (700" to 1400C) the thermal expansi vi ty decreased
20% to 50% over the l i f e of the fuel element.
1 . 5 . 5 . Thermal Conducti vi ty
Changes i n thermal conducti vi ty of H-451 graphi te due to i rradi ati on
were measured at 923 to 1623 K (650O to 135OOC) to HTGR end-of-l i fe
fl uences, and data at 523 to 923 K (250" to 65OOC) were obtai ned from
UKAEA data on graphi tes similar to H-451.
2
rapi dl y at f l uences of 0 to 2 x
Thermal conducti vi ty decreased
and then showed N/m (E > 29 fJ )HTGR
1-10
Ir,
.8
2
onl y a small decrease between 2 and 9 x
I rradi ati on-i nduced reducti on i n thermal conducti vi ty was temperature-
dependent, wi th the l argest reducti on occurri ng at the l owest i rradi ati on
temperatures.
N/m (E > 29 fJ )HTGR.
A method i s descri bed f or cal cul ati ng the i rradi ated thermal conduc-
ti vi ti es at the temperature of i rradi ati on. When the i rradi ati on tempera-
ture was ei ther i ncreased or decreased af ter an i ni ti al peri od, the new
conducti vi ti es assumed the saturati on l evel of the new i rradi ati on tempera-
ture.
1.5.6. I rradi ati on-I nduced Creep
A systemati c program desi gned to measure i rradi ati on-i nduced creep
coef f i ci ents of H-451 graphi te i s i n progress at ORNL, but onl y one capsul e
has been completed to date. Therefore, the creep coef f i ci ents have been
deri ved from the l i terature.
A wide vari ety of graphi tes have been measured i n a vari ety of experi -
ments duri ng the past 20 years.
experi ments at RCN Petten i n the Netherl ands, where a number of graphi te
grades were measured i n a restrai ned shri nkage experi ment; thus, a few
H-451 data poi nts were avai l abl e f or comparison. RCN and J RC Euratom,
Petten, have completed the f i r st phase of an experiment where the creep coef-
f i ci ent of an H-451 specimen was measured i n tensi on. I n thi s experi ment,
A few H-451 specimens were i ncl uded i n
at 1123 K (850"C)l ,
N/m [(E > 29 fJ )HTGR
2
which was taken to about 3.3 x
both the transi ent and steady-state creep coef f i ci ent were measured.
An equati on f or cal cul ati ng the creep strai n i n
deri ved that covers the range 773 to 1473 K (500" to
and creep strai ns up to 2.5% i n
N/m (E > 29 fJ I HTGR
compression.
2
desi gn has been
26
1200OC) up to 10
tensi on and 2% i n
1-1 1
n
1.6. OXI DATI ON PROGRAM
1.6.1 Oxi dati on Rate of H-451 Graphi te
The chemical reacti ons of water vapor wi th H-451 are represented by
the Langmuir-Hinshelwood equati on.
the Langmuir-Hinshelwood equati on f or l ow water concentrati ons (5300 Pa)
and hi gh water concentrati ons (2300 or 13300 Pa)
Rate constants were deri ved to sati sf y
The OXI DE computer code i s used to determi ne the oxi dati on rates f or
reactor servi ce. Rate constants deri ved f or H-451 by the Langmuir-
Hinshelwood equati on are used as i nput f or the OXI DE cal cul ati ons.
water l evel rate constants have been deri ved f or acci dent condi ti ons, where
hi gh moi sture l evel s are possi bl e.
been deri ved and shoul d be used f or normal steady-state reactor operati on,
High
Low water l evel rate constants have
where
1.6.2
water concentrati ons i n the range 10 to 1000 Pa are expected.
Ef f ect of Oxi dati on on Tensile Strength and El asti c Modulus
A l arge number of small specimens taken from a parent log of H- 5
graphi te were oxi di zed to burnof f s up to 20%, and the changes i n tensi l e
strength and el asti c modulus were determi ned.
The tensi l e strength and el asti c modulus of H-451 graphi te were
decreased by an average of 3. 6% i n center axi al specimens when oxi di zed
to burnoffs up to 2.0% at ei ther 1073 K or 1273 K (800' or lOOO'C), and
no si gni f i cant reducti on i n el asti c modulus i n these same specimens was
observed when they were oxi di zed to burnof f s of up to 2.0% at 1273 K
(100O'C). These resul ts are of parti cul ar importance because the maximum
l ocal i zed burnoff i n the HTGR f uel el ement bl ocks has been cal cul ated to
be 1%.
1-12
The rate of reducti on of tensi l e strength and el asti c modulus f or
center axi al specimens i s greater at 1073 K (800C) than at 1273 K (lOOOC).
Thi s concl usi on i s not i mportant f or desi gn because the maximumburnoff of
the f uel element bl ocks i n an HTGR i s cal cul ated to occur at approxi matel y
1273 K (1000C). About 0.1% to 0.2% burnoff is cal cul ated f or f uel el ement
bl ocks operati ng at 1073 K (8OOOC).
I n general , the reducti on rate of el asti c modulus wi th burnoff was
greater than that of ul ti mate tensi l e strength (UTS). The hi gher reducti on
rate of the el asti c modulus i s i mportant i n desi gn because a lower el asti c
modillus decreases the secondary stresses, i .e., thermal stresses resul ti ng
from gradi ents and di f f erenti al i rradi ati on-i nduced strai n. The rate of
reducti on of tensi l e strength and el asti c modulus f or axi al specimens
oxi di zed at 1273 K (lOOOC) i s greater at the edge than at the center of a
l og. Thi s does not impose a l i mi tati on i n desi gn because the tensi l e
strength f or acceptance of a l og f or f uel el ement bl ocks i s always measured
at the center of the l og where i t i s a minimum.
edge of a l og oxi di zed up to 2% burnoff i s never less than the tensi l e
strength at the center at 0 to 2% burnoff. I n general , the reducti on i n
tensi l e strength and el asti c modulus of radi al specimens was hi gher than
that of axi al specimens. The hi gher sei smi c-i nduced stresses i n an HTGR
f uel el ement are i n the radi al di recti on and thi s phenomenon coul d af f ect
desi gn. However, the reducti on i n el asti c modulus of the radi al specimens
was greater than the st rengt h loss, and, thus, the overal l e f f e c t on s e i s m i c
performance shoul d be negl i gi bl e.
The tensi l e strength at the
1-13
2. INTRODUCTION
Grade H-451 near-i sotropi c graphi te is the reference candi date graph-
i te f or repl aceabl e f uel and ref l ector el ements i n HTGRs. Grade H-451
graphi te has been under development at GLCC f or approxi matel y 7 years.
Concurrent wi th GL CC's development program, an i ntensi ve eval uati on program
has been carri ed out on H-451 at GA. The raw material type, formul ati on,
and processi ng have been frozen, and several producti on l ots have been
manufactured and eval uated.
The data generated from the eval uati on programs have been publ i shed i n
a series of GA reports. The purpose of thi s report i s to col l ect, anal yze,
and sort the data from the GA reports, i ncl udi ng data on graphi tes similar
to H-451 from other U. S . or European programs and the open l i terature, and
to present the total avai l abl e data set on H-451 graphi te f or use i n pre-
pari ng the H-451 secti on of the Fuel Design Data Manual (GA-A14429), which i s
requi red f or desi gn and saf ety anal ysi s of HTGRs. The fol l owi ng topi cs are
di scussed:
Concept and Need f or a Near-I sotropi c Fuel Element Graphi te
Secti on 3 expl ai ns the l ogi c and need f or devel opi ng a near-i sotropi c
graphi te i n the U. S. f or HTGR f uel elements.
Development Program at GLCC
Secti on 4 descri bes the scope of the H-451 development program at
GLCC .
2- 1
Char act er i zat i on Pr ogr am
I n Sect i on 5, t he char act er i zat i on pr ogr ami s descr i bed. An ext ensi ve
char act er i zat i on pr ogr amwas r equi r ed t o (1) conf i r mt hat a sui t abl e
mat er i al was avai l abl e f or use i n t he cor e of HTGRs and (2) pr ovi de a
dat a set on pr oper t i es, pur i t y, and f at i gue. The char act er i zat i on
pr ogr amwas desi gned t o eval uat e t he var i ous devel opment pr oduct s f r om
t he GLCC pr ogr amand sel ect a f or mul at i on and pr ocess f or pr oduct i on.
The qual i t y of t he sel ect ed gr ade was est abl i shed by det er mi ni ng t he
pr oper t i es and di st r i but i on of pr oper t i es r epr esent at i ve of t he grade.
A mat er i al s speci f i cat i on has been wr i t t en t hat def i nes r equi r ement s
f or f uel el ement gr aphi t e i n HTGRs and i t wi l l be appl i ed t o ensur e
t hat f ut ur e H- 451 pr oduct i on meet s t he qual i t y r equi r ed.
Irradiation Program
Sect i on 6 di scusses t he i r r adi at i on pr ogr am, whi ch was desi gned to
pr ovi de t he mean and di st r i but i on of pr oper t i es of H- 451 t hat ar e
r epr esent at i ve of t he mat er i al i n t he f ast neut r on f l ux pr esent dur -
i ng t he ser vi ce l i f e of t he f uel el ement s.
di r ect l y to desi gn t he f uel el ement s and t o cal cul at e t he t her mal and
st r ess gr adi ent s t hat occur i n t he f uel el ement gr aphi t e dur i ng i t s
l i f e i n t he r eact or core. Test s on t he f i l l er cokes have been i ncl uded
i n t he mat er i al s speci f i cat i on t o ai d i n st andar di zi ng t he qual i t y of
t he r awmat er i al and ensur e t hat f ut ur e H- 451 pr oduct i on wi l l exhi bi t
t he same i r r adi at i on behavi or as t hat of t he pr epr oduct i on l ogs used
t o obt ai n t he i r r adi at i on dat a set present ed her e.
These dat a ar e used
Oxi dat i on Pr oer am
The oxi dat i on pr ogr ami s di scussed i n Sect i on 7.
el ement bl ocks may be exposed t o st eamoxi dat i on dur i ng t hei r l i f e i n
t he r eact or ; t her ef or e, i t i s necessar y to det er mi ne t he ef f ect of
oxi dat i on on t hei r propert i es.
The H- 451 f uel
The oxi dat i on pr ogr amwas desi gned t o
2-2
determi ne the rate of oxi dati on i n H O-He mi xtures and the ef f ect of
oxi dati on burnoff on mechanical properti es, pri mari l y strength and
el asti c modulus. The oxi dati on data are requi red f or desi gn and
saf ety anal ysi s.
2
Two documents are cl osel y rel ated to thi s report.
Speci f i cati on f or Repl aceabl e Fuel and Refl ector Element Graphi tes
(Number 900739), which contai ns r aw material, processi ng, and property
l i mi t s that must be met by the manufacturer to qual i f y H-451 f or
acceptance and subsequent use i n HTGRs.
speci f i cati on i s to prevent the i ncl usi on of def ecti ve or out-of-
speci f i cati on l ogs i n the manufacture of f uel el ements or repl aceabl e
ref l ectors. The speci f i cati on al so requi res testi ng to ensure uni-
formi ty i n r aw materials from batch to batch over a l ong peri od, thus
ensuri ng properti es and i rradi ati on behavi or consi stent wi th those of
the materials uti l i zed i n the current eval uati on programs.
One i s the Materials
The obj ecti ve of the materials
The other document to be used wi th thi s report i s the H-451 graphi te secti on
of the Fuel Design Data Manual (GA-A14429), which contai ns H-451 property
data deri ved from thi s report, other domesti c and European graphi te programs,
and the open l i terature. The material i n the Fuel Design Data Manual i s
presented i n a form sui tabl e f or use f or the desi gn and safety anal yses of
HTGR f uel elements.
2-3
3. CONCEPT AND NEED FOR A NEAR-I SOTROPI C
FUEL ELEMENT GRAPHITE
The primary i ncenti ve f or devel opi ng a near-i sotropi c graphi te i n the
U.S. f or HTGR f uel el ements was to improve the di mensi onal stabi l i ty and
strength over the conventi onal HTGR needle-coke graphi te (grade H-327).
The development of H-451 was aimed at provi di ng more f l exi bi l i ty i n desi gn,
better saf ety margins f or stresses, and stretch capabi l i ty f or f uture
desi gns. The i sotropy i mparted to the graphi ti zed l ogs by the use of near-
i sotropi c petrol eum coke was aimed at minimizing the di mensi onal contracti on
and del ayi ng the subsequent expansi on to fl uences wel l beyond the servi ce
l i f e i n an HTGR. An addi ti onal goal of the program was to i ncrease the
thermal conducti vi ty of the graphi te, especi al l y i n the radi al di recti on
which i s paral l el to the thi ckness of the thi n l i gaments that separate the
f uel and the cool ant i n the f uel el ement bl ocks.
3- 1
4. DEVELOPMENT PROGRAM AT GLCC
Based on the i ncenti ves descri bed i n Secti on 3 , the development of a
near-i sotropi c graphi te was i ni ti ated i n 1969. To minimize the impact of
development costs and to keep the pri ce of the new product competi ti ve, a
deci si on was taken j oi ntl y by GA and GLCC to uti l i ze commercially avai l abl e
materials wi th conventi onal extrusi on and processi ng as i n the manufacture
of H-327, whi l e at the same t i me emphasizing improved i sotropy i n the f i l l er
coke structure. Thus, the development work and f uture producti on coul d be
accomplished employing exi sti ng raw materials, equipment, and pl ants.
The structure of Gi l socoke was used as a gui de i n procuri ng a new
petroleum-based, speci al , near-i sotropi c coke f or the GLCC development
program. Gi l socoke was used i n Europe to manufacture graphi tes f or the
UK Advanced Graphi te Reactors.
shown sati sf actory i rradi ati on behavi or. However, Gi l socoke i s a si ngl e-
source raw materi al that i s no l onger commercially avai l abl e. Also, Gi l so-
coke presented di f f i cul ti es when used to f abri cate l arge-di ameter l ogs,
i mparti ng a hi gh degree of hardness to the graphi ti zed products.
Graphi tes manufactured wi th Gi l socoke have
4.1. FILLER COKES
GLCC procured a speci al batch of near-i sotropi c coke and desi gnated
i t coke A Subsequent batches from suppl i er A were procured and are
1'
desi gnated A and A
3' 2
A commercial coke that i s used routi nel y i n the producti on of other
commercial graphi te arti cl es i n GLCC pl ants was al so consi dered f or blend-
i ng wi th Coke A. Thi s coke i s a speci al type of sponge coke and has a
structure that i s less i sotropi c than coke A, but i t i s not a needl e coke.
4-1
1
The second coke, desi gnated B 1 , was consi dered f or bl endi ng wi th coke A
to improve the manufacturi ng characteri sti cs and the mi crostructure of the
f i nal product.
A second speci al near-i sotropi c coke was procured from a second
suppl i er.
type feedstock, the ai m bei ng to establ i sh a coke similar to coke A but
from a di f f erent suppl i er.
prototype l ogs duri ng l ater stages of the development program.
Thi s coke, desi gnated C, was produced from the same generi c
Thi s coke was used al ong wi th coke B to make
1
The mi crostructures of the cal ci ned cokes descri bed above were classi-
f i ed at GA usi ng metal l ographi c techni ques descri bed by White and Pri ce
(Ref. 4- 1) .
i n grade H-429 and the earl y prototype H-451 l ogs, consi sted of onl y 65% of
the desi rabl e heterogeneous f i ne i sotropi c (HFI) material, whereas cokes
The resul ts are gi ven i n Tabl e 4-1. Coke A I , which was used
A2 and A consi sted of 90% or more of the HFI material. Coke C i s compar-
3 1
abl e to cokes A and A i n mi crostructure. Coke B i s cl assi f i ed as a
regul ar or sponge coke; the anal ysi s shows a range of consti tuents from
HFI to coarse f i brous (CF) consti tuents. None of the cokes used i n H-451
development and subsequent producti on l ogs contai ned f i ne f i brous (FF)
consti tuents, and they contai n onl y small amounts of CF material. However,
there i s some degree of ani sotropy i n the f i nal graphi ti zed product due to
the s mal l content of ori ented consti tuents i n the f i l l er cokes.
2 3 1
Cokes that have near-perf ect i sotropy were not consi dered because they
i mpart hi gh thermal expansi vi ty t o the graphi ti zed product and are even more
di f f i cul t to process i nto l arge-di ameter l ogs wi th conventi onal equipment.
Needl e-l i ke consti tuents, on the other hand, i mpart low strength and ani so-
tropi c di mensi onal changes duri ng servi ce i n a fast neutron environment.
Thus, the near i sotropi c petrol eum cokes used i n H-451 appear to be optimum
f or HTGR f uel el ement graphi tes.
4- 2
TABLE 4-1
MICROSTRUCTURAL ANALYSIS OF CALCI NED COKES
USED TO MANUFACTURE H-451 GRAPHITE
Coke
No.
536 1-60
5361-61
5361-65
(4
Percent of Consti tuent
Coke
De si gna t i on HFI FI C I CF FF
65 0 15 20 0
95 0 5 0 0
97 0 3 0 0
A 1
A2
A3
52
90
B 1
c1
5361-62
5361-67
("'Descri pti ons from Ref. 4-1 :
HFI =heterogeneous f i ne i sotropi c
FI = f i ne i sotropi c
C I = coarse i sotropi c
CF =coarse f i brous
FF = f i ne f i brous
7 12 29 0
0 4 6 0
4- 3
4.2. PROCESSING
Details of the manufacturi ng processes of H-451 are propri etary to
GLCC.
i n l ength usi ng conventi onal graphi te manufacturi ng processes common to the
manufacture of el ectri c steel furnace el ectrodes. The cal ci ned coke i s
crushed and si zed and a speci f i c formul ati on sel ected consi sti ng of mul ti -
si zed f racti ons of the coke parti cl es, wi th coal tar pi tch as the bi nder.
Thi s formul ati on of cal ci ned cokes and coal tar pi tch is mixed thoroughl y
i n the range 393 to 453 K (120" to 180"C), extruded i nto green logs, and
baked sl owl y to about 1073 K (800C) to carboni ze the bi nder pi tch. The
baked l ogs are then impregnated wi t h petrol eum pi tch and the l ogs heated
to 2973 K (2700C) or above to graphi ti ze the structure.
l ogs i s improved by conducti ng the graphi ti zati on process i n the presence
of chl ori ne gas. The resul tant product i s a hi gh puri ty, near-i sotropi c,
medium-grained nucl ear graphi te sui tabl e f or use i n an HTGR core.
I n general , H-451 i s produced as l ogs 432 mm i n di ameter by 864 mm
The puri ty of the
.
4.3. PROTOTYPE AND PREPRODUCTION DEVELOPMENT
Grade H-429 was formul ated wi th Coke A and extruded i n the GLCC pi l ot
1
pl ant as a 52-mm-diameter log.
di ati on testi ng by Ch duri ng 1970-1972.
H-429, GLCC manufactured a number of f ul l - si ze experi mental grades.
H-451 ( l ot 266), i ni ti al l y f abri cated wi th coke A1, was sel ected j oi ntl y
by GA and GLCC as the most promi si ng material f or f urther development.
chronology of the development program i s gi ven i n Tabl e 4-2.
preproducti on development, l ots 408, 424, and 426 were f abri cated usi ng a
bl end of ei ther cokes A2 and B1 or A3 and B
a bl end of cokes C1 and B
rated i nto GA's characteri zati on and i rradi ati on programs.
Grade H-429 was committed to earl y irra-
Concurrent wi th the i rradi ati on of
Grade
A
I n subsequent
Two l ots were produced usi ng
Logs from l ots 266, 408, and 426 were i ncorpo-
2'
3'
I n 1975, the formul ati on and processi ng methods of l ot 426 were j oi ntl y
sel ected by GLCC and GA as models f or the i ni ti al producti on of 350 l ogs of
4-4
4
-
5

n
H-451 f or possi bl e use i n FSV as rel oad el ements. Producti on l ots 472, 474,
476, 4 7 8 , and 482 were produced f or the Fort St. Vrai n rel oad segments usi ng
a bl end of coke A and B and the same formul ati on and processi ng as f or
preproducti on l ot 426. Ni nety-ei ght l ogs from producti on l ots 472, 4 7 8 , and
482 were sampled at the mi dl ength center (MLC) of each l og, and tensi l e
strength was measured on ei ght axi al and four radi al specimens from each.
3 1
During the development program a number of the l ogs from each l ot were
The programs di stri buted to eval uati on programs wi thi n and external to GA.
uti l i zi ng H-451 graphi te are gi ven i n Tabl e 4-3. The use of H-451 prepro-
ducti on l ogs f or experi ments i nvol vi ng f uel development, oxi dati on, recycl e,
FSV f uel test el ements, l arge-scal e mechani cal testi ng, forei gn programs,
ORNL programs, and BNL programs occurred concurrentl y wi th the GLCC develop-
ment program and the characteri zati on and i rradi ati on programs at GA. Thus,
s e l e c t i o n of material f or each program depended on the availability of l ogs
at the t i me of thei r need; i.e., eval uati on di d not wai t unti l the develop-
ment program was complete.
4. 4. CONCLUSIONS
GLCC developed propri etary sources of near-i sotropi c cokes f or use i n
devel opi ng grade H-451 as a candi date f or advanced HTGR f uel el ements.
Grade H-451 was developed usi ng conventi onal graphi te processi ng and a
bl end of a near-i sotropi c coke and a speci al sponge coke.
producti on l ots and one producti on batch were manufactured f or eval uati on
by GA and other reactor programs i n the U. S. and Europe.
A number of pre-
REFERENCE
4-1. White, J . L , , and R. J . Pri ce, The Formation of Mesophase Micro-
structures During the Pyrol ysi s of Sel ected Coker Feedstocks,
Carbon 12, - 321 (1974).
4-6
TABLE 4- 3
PROGRAMS UTI L I ZI NG H-45 1 GRAPHITE LOGS
Program
Characteri zati on
I rradi ati on
Fuel el ement development
Oxida t i on studi es
Recycle f uel element
studi es
Large-scal e mechanical
tests
ORNL programs
BNL program
Forei gn programs: KFA,
CEA, RCN Petten, and
Dragon
Use or Measurements
Measurement of physi cal , mechani cal , and
chemical properti es on s mal l specimens cut
from f ul l - si ze l ogs.
wi thi n l ogs, from l og-to-l og wi thi n l ots, and
from l ot-to-l ot were i nvesti gated. Fati gue
characteri sti cs were determi ned.
Same as above except fewer specimens measured
due to l i mi ted resources and hi gh cost of
i rradi ati on experi ments.
Ful l -si ze machined bl ocks used to determi ne
characteri sti cs of H-451 graphi te and i ts i nter-
acti on wi th f uel sti cks duri ng carboni zati on-
i n-pl ace (CIP) experi ments.
Measurement of reacti on rates of H-451 i n
He-H20 mi xtures.
of H20 and H2 concentrati on, fl ow rate, and
temperature. Studi es of the ef f ect of oxi da-
ti on on strength reducti on.
Ful l -si ze machined bl ocks used to determi ne
ef f ect of material on crushi ng, burni ng, and
f uel separati on.
Use of f ul l - si ze or scal ed machined bl ocks
f or sei smi c testi ng. I ntermedi ate-si ze
specimens used f or dowel pi n, thermal stress,
and mi scel l aneous mechani cal tests.
Oxi dati on, i rradi ati on creep, and f uel recycl e
t e s t s .
Oxi dati on tests.
Oxi dati on and i rradi ati on tests i ncl udi ng
creep, i n-reactor thermal stress tests, f ul l -
si ze machined el ements f or strength proof
testi ng, and machining tests.
Vari ati ons of properti es
Parametri c studi es of ef f ect
4- 7
5. CHARACTERIZATION PROGRAM
5.1. I NTRODUCTI ON
Characteri zati on of grade H-451 i ncl udes determi nati on of : (1) di s-
tri buti on of properti es wi thi n i ndi vi dual l ogs and between l ogs wi thi n a
l ot, (2) stati sti cal di stri buti on of strength wi thi n a l og, ( 3) strength
di stri buti on among l ogs, and ( 4 ) f ati gue behavi or.
5.2. DISTRIBUTION OF PROPERTIES WI THI N I NDI VI DUAL LOGS AND BETWEEN
LOGS WI THI N A LOT
5.2.1 . Sampling
Sampling diagrams are shown i n Appendix A. Properti es were measured
on specimens taken paral l el to the extrusi on di recti on (axi al )* and per-
pendi cul ar to the extrusi on di recti on (radi al )*. I n the experi ments to
determi ne property di stri buti ons wi thi n a l og, the l ogs were sampled at
four di f f erent l ocati ons wi thi n each l og: mi dl ength center (MLC), end
center (EC), mi dl ength edge (MLE), and end edge (EE). Properti es measured
on l ogs i n the uni rradi ated state wer e ( 1) bulk densi ty, (2) tensi l e prop-
erti es, i ncl udi ng strength, el asti c modulus, strai n at f racture, and
Poi sson's rati o i n tensi on, ( 3) f l exural strength, ( 4 ) strength and el asti c
modulus i n compression, (5) thermal expansi vi ty, (6) thermal conducti vi ty,
and (7) i mpuri ty content.
*
The terms axi al and radi al are used throughout thi s report to desi gnate
specimens whose l ongi tudi nal axi s (axi s al ong which measurement was made)
was paral l el to the l ongi tudi nal axi s of the parent l og and paral l el to
the radi us of the parent l og, respecti vel y.
5-1
5.2.2. Bulk Densi ty
The bul k densi ty of graphi te is defi ned as the weight of the l og
di vi ded by the bul k volume (outer dimensions of the l og).
ti on, the bul k densi ty was determined on the tensi l e strength specimens
pri or to thei r use i n strength tests.
on whole as-graphi ti zed logs at the GLCC producti on pl ant.
acceptance w i l l be based on whole l og densi ti es measured at GLCC.
For characteri za-
Densi ty measurements were al so made
Producti on
The densi ti es of f our l ogs from preproducti on l ot 426 are presented i n
The data i ncl ude measured and cal cul ated Appendix B, Table B-1 (Ref. 5-1).
whole l og densi ty val ues.
val ues from the center and edge specimens.
whole l ogs i n the manufacturer's pl ant were about 0.01 Mg/m3 hi gher than
those measured at GA on small specimens l ocated throughout the l og.
was a s mal l but significant increase in dens i t y from the center to the edge
of some l ogs. However, several l ogs had no gradi ent. The densi ty was, i n
general , l owest at the MLC posi ti on and i ncreased sl i ghtl y near the edges
and ends of the l ogs. Again a few excepti ons were observed.
i n densi ty f or H-451, l ot 426, ranged from 1.695 to 1.753 Mg/m ,
The l atter were obtai ned by averagi pg the mean
The bul k densi ti es measured on
There
The vari ati on
3
The mean of the small-specimen measurements agrees wel l wi th that of
3
measurements by GLCC on whole l ogs.
l ogs from l ot 426 was 1.73 5 0.01 Mg/m .
val ues were obtai ned on 98 l ogs from producti on l ots 472, 478, and 482.
The mean bul k densi ty of these l ogs was 1.74 ? 0.025 Mg/m .
The mean bul k densi t y f or the four
Addi ti onal whole l og densi ty
3
5.2.3. Mechanical Proper ti es
The mechanical properti es measured were ul ti mate tensi l e strength,
el asti c modulus i n tensi on, strai n at f racture i n tensi on, Poi sson's rati o
i n tensi on, ul ti mate f l exural strength, ul ti mate compressive strength,
el asti c modulus i n compression, and f ati gue behavi or.
5-2
5.2.3.1. Tensi l e Strength, El asti c Modulus, and Strai n at Fracture. The
ul ti mate tensi l e strength data f or preproducti on l ot 426 are summarized i n
Appendix B, Table B-2 (Ref. 5-1). The tensi l e strength of H-451 i s hi ghest
i n the axi al di recti on, l owest at MLC f or axi al and radi al di recti ons, and
i ncreases from the center to the edge. The mean tensi l e strength of H-451,
l ot 426, ranged from 13.65 f 1.60 MPa at MLC to 19.00 _+ 1.85 MPa at MLE i n
the axi al di recti on and from 10.75 ? 2.10 MPa at MLC to 15.22 _+ 2.25 MF' a at
EE i n the radi al di recti on.
The observed pattern of l owest axi al or radi al strength at the MLC of
each l og makes i t mandatory to test each l og as near the MLC as possi bl e
duri ng acceptance/rej ecti on testi ng, as requi red by Speci f i cati on 900739
(wi thi n sl ab 3, secti on AC/BC; see Appendix A, Fi g. A-1). Thi s ensures
that each l og i s tested at i ts weakest l ocati on. Testi ng specimens of ei ther
axi al or radi al di recti on i s acceptabl e. Vari ati ons i n tensi l e strength were
observed from l ot to l ot at the same l ocati on i n each l og (see Secti on 5.4).
Data on el asti c modulus measured i n tensi on f or preproducti on l ot 426
are gi ven i n Appendix B, Tabl e B-3 (Ref. 5-1). The el asti c modulus followed
the same pattern wi thi n l ogs as the tensi l e strength.
H-451, l ot 426, ranged from 7. 93 GPa at MLC to 8.82 GPa at MLE i n the axi al
di recti on and from 6.89 GPa at MLC to 7.45 GPa at EE i n the radi al di recti on.
The mean modulus of
The strai n at f racture f or H-451 was i n the range 0.25 to 0. 35% (Ref.
5-1). The strai n at f racture was l owest f or both axi al and radi al specimens
at the MLC of al l logs and i ncreased from the center to the edges. A
systemati c vari ati on i n the strai n at f racture from l og to l og or l ot to
l ot was not observed i n H-451.
5.2.3.2. Poi sson's Rati o. Poi sson's rati o data are summarized i n Appendix
B, Tabl e B-4 (Ref. 5-1). Poi sson's rati o val ues, v are i denti f i ed i n
standard tensor notati on accordi ng to the orthogonal axes (Ref. 5-2) wi thi n
i j '
a l og (see Appendix A, Fi g. A-4). Poi sson's rati o was measured on H-451 i n
the axi al and radi al di recti ons at several l ocati ons wi thi n a l og.
5-3
Poi sson's rati o decreased wi th i ncreasi ng stress duri ng i ni ti al l oadi ng
and reached a constant val ue, i ndependent of stress, af ter two or three l oad-
i ngs. or u2) to MLX
specimens, v = v = 0.110 ? 0.009 and v = w = 0.108 2 0.008. When
stresses were appl i ed i n the axi al di recti on (a ) to MLC specimens, v =
- 3 31
v = 0.127 ? 0.013. When stresses were appl i ed i n the axi al di recti on (u )
to MLE specimens, u
When stresses were appl i ed i n a radi al di recti on (a
1
- - - -
-
13 23 12 21
3
-
32
= 0.121 _+ 0.005 and J = 0.114 _+ 0.006. When stresses
32 31
-
were appl i ed i n the axi al di recti on (a ) to EE specimens, v = 0.110 ? 0.010
- 3 32
and v =0.117 _+ 0.006.
31
5.2.3.3. Fl exural Strength. The f l exural strength data f or H-451 l ot 426
are summarized i n Appendix B, Tabl e B-5 (Ref. 5-3). The f l exural strength
ranged from 20.2 to 25.3 MPa i n the axi al di recti on and from 17.4 to 21.7
MPa i n the radi al di recti on.
5.2.3.4. Compressive Strength and El asti c Modulus. Data on the compressi ve
strength and el asti c modulus are summarized i n Appendix B, Tabl e B-6. The
mean ul ti mate compressi ve strength measured on a l og from producti on l ot
478 was 47 MPa i n the axi al and radi al di recti ons.
was 2.5 MPa and the l og-to-l og vari ati on was 1.5 MPa. El asti c modulus i n
compression averaged 7.6 MPa.
The wi thi n-l og vari ati on
5.2.4. Thermal Properti es
5.2.4.1. Thermal Expansi vi ty and Ani sotropy Factor. Thermal expansi vi ty
data are summarized i n Appendix B, Tabl e B-7 (Ref. 5-1). The mean thermal
expansi vi ty between 300 and 773 K (27' and 50OoC) of H-451, l ot 426,
ranged from 3.9 to 4.1 x 10 K ( ' C- ' ) i n the axi al di recti on and 4.5 to
4.6 x 10 K ("C-l) i n the radi al di recti on. There was no si gni f i cant
vari ati on of thermal expansi vi ty as a functi on of specimen l ocati on wi thi n
the l ogs of l ot 426.
-6 -1
-6 -1
5-4
The ani sotropy f actor i s defi ned as
a(radi s1)
cr(axia1)
ani sotropy f actor (AF) =
where a(radi a1) is the thermal expansi vi ty i n the radi al di recti on and
cc(axia1) i s the thermal expansi vi ty i n the axi al di recti on.
data are shown i n Appendix B, Tabl e B-8 (Ref. 5-1, 5-3). The mean ani sot-
ropy f actor f or the l ogs i n l ot 426 i s 1.15.
The ani sotropy
5.2.4.2. Thermal Conducti vi ty. Data on thermal conducti vi ty are summarized
i n Appendix B, Tabl e B-9 (Ref. 5-1). The mean thermal conducti vi ty at the
MLC of l ogs from l ot 426 was 65 f 4 W/m*K i n the axi al di recti on and 63 +_ 4
W/m*K i n the radi al di recti on at 1073 K (8OOOC).
5.2.3.3. Speci f i c Heat. The speci f i c heat of H-451 graphi te is gi ven by
the equati on (Ref. 5-4)
1 -1
= (0.54212 - 2.42667 x T - 9.02725 x 10 T
cP
- 4.34493 x l o4 T- +1.59309 x l o7 T-3
9 -4
- 1.43688 x 10 T ) x 4186
C = s peci f i c heat at constant pressure (J/kg-K),
P
T = temperature (K ).
where
5-5
5.2.5. I mpuri ty Content
5.2.5.1 . Neutron-Absorbing I mpuri ti es. Two types of neupron-absorbing
i mpuri ty el ements, burnabl e* and nonburnable*, are of importance to the
neutroni c desi gn and operati on of HTGRs.
burnabl e poi son el ements i s expressed i n boron equi val ents:
The i mpuri ty content of the non-
'xAB
Ax5B
BE (boron equi val ent) =- (5-2)
where CS = ef f ecti ve neutron capture cross secti on of i mpuri ty
X
el ement x,
boron,
-
u = ef f ecti ve neutron capture cross secti on of natural
Ax =atomic weight of impurity element x,
AB = atomi c wei ght of natural boron.
B
The boron equi val ent val ues f or each el ement are then mul ti pl i ed by thei r
respecti ve concentrati ons i n the graphi te, and the products are summed to
obtai n the boron equi val ent l evel , i n parts per mi l l i on, f or the graphi te:
Y E C = BEG
i
x x
where BE =
c =
X
X
boron equi val ent of i mpuri ty element x,
boron equi val ent concentrati on of al l i mpuri ty
el ements i n graphi te.
(5-3)
*
Nonburnable i mpuri ty el ements are those that remain i n some proporti on to
thei r ori gi nal content at the end-of-l i fe f or the f uel el ement bl ock,
whereas the burnabl e i mpuri ti es are compl etel y transmuted to other
i sotopes.
5-6
The neutroni c desi gners of HTGRs requi re knowledge of the nonburnable
i mpuri ti es l i sted i n Tabl e 5-1, column 8. Those defi ned as burnabl e poi sons
are: boron, cadmium, europium, gadolinium, samarium, and l i thi um; the
bal ance are defi ned as nonburnabl e. I t i s desi rabl e to keep the total non-
burnabl e i mpuri ty content below 0.5 ppm. However, i t i s a formi dabl e and
expensi ve task to perform chemical anal yses f or al l requi red nonburnable
el ements and obtai n the sensi ti vi ty requi red to detect the el ements at a
l evel sati sf yi ng the requi rement of 0.5 ppm. A recommended practi ce f or
determi ni ng BE i nvol vi ng low-temperature ashi ng of the graphi te and subse-
quent anal ysi s of the ash by emi ssi on spectroscopy i s under development by
ASTM Committee C5:05, "Nuclear Appl i cati ons," a subcommittee of C-5,
"I ndustri al Carbon and Graphi te." A round-robin specimen of H-451 taken
from l og 6484-34 of l ot 426 was prepared by GA and anal yzed by AirCo Speer,
OWL, BNL, and GA, who have representati ves on Committee C5:05. The resul ts
of the round-robin tests are presented i n Tabl e 5-1, columns 4 through 7,
wi th the permi ssi on of the organi zati ons l i sted above.
4
The agreement among the four l aboratori es was excel l ent. The GA data
(column 7) wer e obtai ned by emi ssi on spectroscopy on the ash of a 0.100-kg
sampl e. The ash was prepared at about 473 to 523 K (200" to 25OOC) over a
258-hr peri od. Low-temperature ashi ng prevents the evaporati on of vol ati l e
i mpuri ti es, thus improving the accuracy of the data. The val ues f or each
element represent, i n most cases, the lower l i mi t of detecti on and, i n some
cases, the actual val ue of the i mpuri ty el ement. Thus, the cal cul ated boron
equi val ent concentrati on represents an upper l i mi t of detecti on; i .e., the
boron equi val ent concentrati on, i n most cases, i s less than the val ue shown.
An attempt was made to sel ect and el i mi nate el ements that have ei ther
(1) a low boron equi val ent f actor (equal to or less than O.OOOl), or (2) a
hi gh probabi l i ty of' occurri ng at i nsi gni f i cant concentrati ons.
Using the GA data (Table 5-1, column 7), a boron equi val ent of 0.131
ppm was obtai ned f or nonburnable el ements. Thi s excl udes chl ori ne, which
i s i ncl uded i n column 8 but not i n column 7 because no data were avai l abl e.
5-7
TABLE 5-1
SIMNARY OF BORON EQUIVALWT TEST DATA ON H-451, LOT 426, LOG 6484-34
4 5
column
6 7 8
-
2
-
Symbol
Al
Sb
A
AS
Ba
Be
B i
B
Br
cd
ca
C
Ce
CS
cl
cr
Co
cu
Dy
EK
Eu
F
Gd
Ga
Ge
Au
Hf
He
Ho
H
I n
I
Ir
Fe
KK
La
Pb
L i
Lu
m
Mn
Hg
Ma
Nd
Ne
N i
Nb
N
OS
0
Pd
P
-
9 10 1 1 14 13
Elements
DI Boron
ul val ent
al ysescd)
1
12
Elements
di th Boron
Equivalent
< 0.0001
3
Boron
equivalent
Factor
Clements NO'
Recomendei
:or Analyse:
by ASTH
Comi tted
C5:05
Analyses
)r Purposes
Other
Than Boron
l ui val ent(c)
X
Equivalent Boron
( ped
Elements
Requested
+or Analyses(b
l e n t N T
equestedyb) I I1 I11 Element
Aluminum
Anti wny
Argon
Arseni c
Barium
Beryl l i um
Bismuth
Bomn
Bromine
cadmium
Calcium
Carbon
Cerium
cesium
Chl ori ne
Chromium
Cobal t
Dysprosiun
Erbium
Europium
Fl uori ne
Gadoliniun
Gallium
Germanium
Cold
Hafnium
Helium
Holmium
Hydrogen
Indium
I odi ne
I ri di um
I ron
Krypton
Lanthanum
Lead
Lithium
Luteti um
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Neon
Ni ckel
Niobium
Ni trogen
Osmium
Pal l adi um
Phosphorus
Copper
Omen
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
0.000036
0.0001 2
0.000025
0.000000016
0.000000016
0.18
0.02565
0.00006
0.0000005
0.038
0.00015
0.0001 4
0.000030
0.0000
0.00014
0.0023
0.0079
0.0029
0.000044
0.0004 1
0.0012
0.0000057
0.000000018
0.00051
0.00024
0.000003
0.0001 2
0.000034
0.00029
0.00014
0.00001 6
NA
NA
0.0001
0.0001 2
0.0062
--
--
0.00042
0.00001 6
0.000026
1 .woo
0.855
0.00020
0.0001
0.0127
0.0136
0.00086
0.0114
0.00099
0.1048
0.0692
0.459
1.57
--
--
-
--
-
-_
0.0475
0.0222
0.135
--
--
--
--
0.00068
0.00114
0.000001
0.171
0.048
0.00005
0.0041
0.0014
0.00573
0.00114
0.00088
0.002
0.000004
0.0001
--
-
-
-
--
0.3
-
--
--
0.02
0.005
0.01
0.2
0.03
0.2
0.2
--
--
-
--
0.2
0.02
0.07
0.05
0.02
0.01
0.01
0.01
0.02
0.05
0.02
--
--
--
I
--
-
--
4.0
0.01
0.07
0.005
0.1
0.1
0.06
0.03
0.2
_-
-
-
--
--
-
--
-
-
--
0.45
0.45
0.45
0.045
0.045
0.45
4.5
0.45
--
--
--
-
--
-
--
0.14
0.45
0.14
4.5
4.5
4.5
4.5
0.045
0.45
4.5
--
-
--
--
L
-
--
--
2.2
4.5
0.45
0.45
4.5
0.045
0.045
0.045
4.5
0.14
0.045
-
--
--
-_
--
-
--
--
0.2
-
--
-
0.009
-
--
0.05
0.007
0.2
--
--
-
0.02
0.2
0.04
0.001
0.018
0.004
0.002
0.007
-
-
--
-
-
0.004
0.018
0.007
-_
--
--
--
2.6
--
-
0.014
0.007
0.001
0.07
0.07
0.002
--
-
--
0.2
--
--
0.004
0.001
--
--
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
TABLE 5-1 (Continued)
1
Element
Pl ati num
Potassium
Praseodyni u
Protacti ni u
Radium
Redon
Rhenium
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Si l i con
Si l ver
Sodium
stronti um
Sul f ur
Tantalum
Tel l uri um
Terbium
Thallium
Thorium
Thulium
Ti n
Titanium
Tungsten
Uranium
Vanadium
Xenon
Y tterbium
Y t t r i um
Zinc
2
Symbol
Pt
K
P I
Pa
Ra
Rn
Re
Rh
Rb
Ru
Sm
SC
Se
si
Ag
Na
Sr
s
Ta
Te
Tb
TS
Th
Tm
Sn
T i
W
U
V
Xe
Yb
Y
Zn
3
Boron
Equi val ent
Factor
-_
0.00081
0.00156
-_
-
-
-
-
0.00033
0.941
0.0074
0.000085
0.0322
0.00034
0.000836
0.00029
0.0159
0.0137
0.0004 3
0.0487
0.00029
0.0018
0.00857
0.00147
0.00715
0.00027
0.0001
0.053
--
-
--
I
--
-
__
4 5 6 7
Round Robin Test
Dataca) ( p p d
Laboratori es
I Ill
-
:0.001
:0.017
-
-
--
-
:0.001
:O.W)4
:O .004
:o.002
:0.007
L-
I
26.0
0.028
0.10
0.006
:O .007
-
--
--
0.2
:0.004
0.07
:0.004
:0.004
0.001
-
--
--
--
_-
0.070
0.070
_-
-
IV
<0.012
<0.030
C0.050
--
--
__
--
<0.024
<0.120
<O .050
<0.002
3.0
0.001
0.90
<0.012
<0.120
<O .060
<0.050
0.060
<O .005
0.060
0.180
<0.120
<0.060
0.018
<0.002
C0.003
t0.060
0.060
--
--
--
--
-
-_
Colurrm
8
Elements
Requested
>r Analyses (b)
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
a)Work done by ASTM Anal yti cal Task Force; C5:05 Nuclear Graphi te Committee.
(b)Elements requested by neutroni c desi gners.
(C)Neasured f or purpose of control l i ng oxi dati on. but included i n BE cal cul ati on.
(d)Elements not l i sted i n columns 10. 11, and 12.
(e)NZ measured on l og 6884-34 = 45 ppm
Note: Ash content of anal yti cal specimen used for thi s experiment - 60 ppm.
9
:lement N
.eques tedx)
X
X
X
X
X
X
X
X
X
X
X
X
X
x
10
Analyses
or Purposes
Other
Than Boron
qui val ent(c:
X
X
C5:05
X
X
X
X
X
X
X
1 1
lements NOT
ecomended
or Analyses
by ASTU
Committee
12
Elements
di th Boron
l qui val ent
< 0.0001
X
X
Elements
for Boron
Squivalent
mal yses(d)
- -
X
X
X
X
X
X
X
X
X
X
14
Boron
Equi val ent
( ppd
~
0.000024
0.000078
0.000040
0.047
0.000075
0.00026
0.000032
0.0031
0.00001
0.00046
0.0019
0.00069
0.000026
0.00024
0.00032
0.0010
0.000026
0.00001 4
0.000016
0.000006
No anal ysi s was done f or phosphorus or ni trogen, but val ues of 1.6 pprn f or
phosphorus (Ref. 5-1) and 45 ppm f or ni trogen (see Tabl e 5-1, footnote e)
were obtai ned on di f f erent specimens and i ncl uded i n the BE cal cul ati on. A
BE val ue of 0.238 ppm was obtai ned f or burnabl e el ements (boron, calcium,
europium, gal l i um, l i thi um, and samarium). The onl y element that contri buted
si gni f i cantl y to the nonburnable BE val ue was cadmium, whereas f or the
burnabl e BE val ue boron and samarium wer e the bi g contri butors. I t was
assumed that chl ori ne (BE f actor = 0.0136) di d not contri bute greatl y to the
total BE.
By el i mi nati ng el ements i n Tabl e 5-1, column 9 (not requested by the
neutroni c desi gners), column 10 (to be determi ned f or purposes of checki ng
on oxi dati on resi stance), column 11 (not recommended f or anal yses by ASTM
C5:05 work due to low probabi l i ty of occurrence), and column 12 (BE f actor
<0.0001), w e arrive at t he r e m a i n i n g l i st of e l e m e n t s i n column 13 which
are requi red. Again usi ng data from Tabl e 5-1, column 7, a BE of 0.093
ppm was cal cul ated f or nonburnabl e el ements and 0.18 ppm f or burnabl e. The
el i mi nati on of cadmium i n accordance wi th the ASTM Committee C5:05 recom-
mendation accounts f or the l arge reducti on i n nonburnable BE. I f cadmium
i s i ncl uded i n column 13, the val ue becomes 0.128 ppm, i n excel l ent agree-
ment wi th the val ue of 0.131 when al l el ements are i ncl uded.
The nonburnabl e BE concentrati on i s wel l below the desi red l i mi t of
0.5 ppm f or thi s specimen and i t made l i ttl e di f f erence whether i t was cal-
cul ated usi ng i mpuri ty data f or el ements i n column 8 or column 13.
val ue cal cul ated from the round-robin data si gni f i cantl y i ncreases the
sensi ti vi ty of anal ysi s and gi ves an upper l i mi t of 0.131 ppm on the
nonburnable BE i n comparison wi th an upper l i mi t val ue of 0.9486 ppm
reported i n Ref. 5-1 and 0.238 ppm f or the round-robin data versus 3.2922
ppm from Ref. 5-1 f or burnabl e BEs.
The BE
I t shoul d be noted that the resul ts reported on the boron equi val ent
i mpuri ty content were obtai ned on a preproducti on l og of hi gh puri ty (ash
content = 60 pprn). I mpuri ty content w i l l be di stri buted among l ogs wi thi n
5-3 0
a producti on batch, the puri ty depending on the degree of puri f i cati on with-
i n each graphi ti zati on furnace l ot. The di stri buti on of i mpuri ty content i s
di scussed f urther i n Secti on 5. 2. 5. 2.
l ot 426, i s of hi gh puri ty and would easi l y qual i f y as a f uel element i n the
core of an HTGR.
Based on thi s experi ment, log 6848- 34,
5. 2. 5. 2. Ash, I mpuri ti es Affecti ng Oxi dati on Rate, and Lithium. The total
ash content, i mpuri ti es that catal yze oxi dati on reacti ons, and l i thi um are
i mportant f or desi gn and saf ety anal yses. The data f or H-451 graphi te, l ot
426, are summarized i n Tabl es 5- 2, 5- 3, and 5-4.
I mpuri ty content f or four l ogs of l ot 426 are shown i n Table 5- 2. The
ash content f or these l ogs averaged 45 ppm and ranged from <25 to 89 ppm
wi th s mal l vari ati ons wi thi n the l og (Ref. 5- 1) . Elements known to catal yze
oxi dati on reacti ons, such as i ron, vanadium, ti tani um, aluminum, si l i con,
and cal ci um, ranged from 0.5 to 22 ppm. Sul f ur content was about 1 ppm.
The di stri buti on of these el ements was uniform wi thi n each l og and paral -
l el ed the di stri buti on of the ash. Li thi um (see Table 5- 3) was not detected
usi ng the most sensi ti ve methods avai l abl e. The l i thi um content was wel l
below 1 ppm and may be below 0. 005 ppm.
As mentioned previ ousl y, the puri ty of the l ogs i s a f uncti on of the
degree of puri f i cati on imparted i n each graphi ti zati on furnace.
ash content f or a number of the preproducti on l ots as a f uncti on of thei r
graphi ti zati on run are gi ven i n Table 5-4. The mean ash content i n furnace
runs 6399-C and 6003-C was 23 and 50 ppm, respecti vel y, whereas i t was 255
Data on
ppm i n run 5698-C.
3 l ots; l ot 426 l ogs contai ned coke A, and l ots 438 and 440 l ogs contai ned
coke C; however, al l l ogs were low i n ash. Producti on l ots 472, 478 and
482 were rel ati vel y hi gh i n ash content.
di f f erent and less ef f i ci ent puri f i cati on f aci l i ty than the preproducti on
l ots.
Graphi ti zati on furnace run 6399-C contai ned l ogs from
These l ogswere graphi ti zed i n a
Si nce the data presented here show that the manufacturi ng process i s
5-1 3
bl
I
ir
Mg Pb
~ 0 . 5 6.0
~0.6 <10.3
2.0 < 6.0
~0 . 5 < 6.0
to
x o . of
Repl i cates
8
8
8
8
Log No. I As h
GA
(b 1
GLCC GLCC
C 1 . 0
~ 2 . 1
c1.0
ql . 0
<1.3
6484-40
6484-4 1
Mean lot ( 4
1
C2.0 4.0 <20 213.8 <i o
<2.1 11.3 ~ 2 7 . 5 36.3 <11. 3
<1.0 C 1. 0 c20.0 c10.0 C10.0
C1.0 < 1.0 C 2 0 . 0 <10.0 c10.0
c 1 . 5 < 4 . 3 c21.9 c21. 3 <10.3
6484-33
6484-34
logs)
92 34
198 24
-
GA
55
84
<25
<25
89
41
<45
42
13
TABLE 5-2
IMPURITY CONTENT: H-451, LOT 426' " )
I
-
B
3. 0
4. 8
~0.8
~ 1 . 4
~ 2 . 5
Fe
4 . 0
C 7 . 4
<1 .o
<1 .o
~3 . 2
Va
<0. 5
~ 0 . 5
~ 0 . 5
<O. 5
<0. 5
(a)From Ref . 5 - 1 .
(b)Measured by GLCC; 1 specimen per l og.
Mean Value (MLC, MLE, EC, EE) (pprn)
<0.9 I ,: 7. 1 j 32
,
TABLE 5-3
SUMMARY OF L I THI UM ANALYSES : H-45 1 (a)
GA Log No./(GL CC Log
No./GLCC L ot No.)
565 1-861
521408
6484-331
921426
64 84 - 34 1
198/ 426
6484- 40/
1551426
6484-41 /
1841426
No. of
K e p 1 i c a t es
4
1
1
8
2
2
8
1
1
1
1
1
1
1
8
1
1
3
1
(a)From Ref. 5- 1.
( b) A l l speci mens have this val ue.
C o nt ent (ppm)
<O .07
<o .02
<1 .o
(b 1
<O. 005
0. 074
<O .005
<0. 01
<0.01
5-3 3
Q
-
Ash (ppm)
CLCC Graphi ti zati on GLCC Lot ._
Furnace Run No. No. X U
TABLE 5-4
IMPURITY CONTENT : H-451
(a)
No. Logs Tested
1272 472(b) 304
478(b)
5698-C
6399-C
6003-C
6399-C
6399-C
258
426
426
4 26
4 38
440
23
50
21
26
n
4 38
6.5
75
9.1
13
45
31
51
25
23
98
(a)One specimen tested per l og.
(b)Lots 472, 478, and 482 val ues averaged together.
capabl e of producing materi al wi th extremel y low i mpuri ty content, i t i s
the f uncti on of the materi al speci f i cati on to mai ntai n the i mpuri ty content
requi red f or reactor desi gn and saf ety analyses i n f uture producti on.
5.2.6. Concl usi ons
3
The bul k densi ty averaged 1.74 2 0.02 Mg/m f or producti on logs. The
mechani cal properti es exhi bi ted near-i sotropi c characteri sti cs wi th the
l owest strength val ues at the MLC of the l ogs.
Thermal expansi vi ty val ues were i ntermedi ate between needle-coke
graphi tes and hi gh-strength i sotropi c graphi tes.
was 1.15. The i ntermedi ate thermal expansi vi ty and the ani sotropy f actor
The ani sotropy f actor
5-1 4
resul t from the structure of the f i l l er coke used. The near-i sotropi c cokes
improve the thermal conducti vi ty i n the radi al di recti on (major di recti on of
heat flow i n reactor servi ce) over needle-coke grnphi tes.
The i mpuri ty content of l ogs from each graphi ti zati on l ot depends on
the thoroughness of puri f i cati on duri ng the graphi ti zati on process. The ash
content can range from <50 to 300 ppm, depending on the degree of puri f i ca-
ti on.
0.131 ppm and the burnabl e boron equi val ent val ue 0.238 ppm.
The nonburnable boron equi val ent val ue of a hi ghl y puri f i ed l og was
5.3. STATISTICAL DISTRIBUTION OF STRENGTH WI THI N A LOG
A detai l ed knowledge of the stati sti cal di stri buti on of tensi l e and
f l exural strength wi thi n an H-451 l og was obtai ned by destructi vel y testi ng
a complete l og (Ref. 5-5). Factors sought were (1) the systemati c vari ati on
of strength wi th ori entati on and l ocati on throughout a l og, (2) f or a gi ven
ori entati on and l ocati on, the stati sti cal di stri buti on of strengths, the
mean, standard devi ati on, and the coef f i ci ent of vari ati on which characteri ze
the specimen popul ati on, ( 3) the rel ati on between f l exural strength and
tensi l e strength, and ( 4 ) the val i di ty of the Weibull stati sti cal theory
(Ref. 5-61, i ncl udi ng the dependence of strength on specimen si ze and the
Weibull modulus, i f appl i cabl e. The Weibull theory, i n which the strength
of a br i ttl e sol i d i s assumed to be control l ed by fl aws, has potenti al uses
i n the engi neeri ng desi gn of l oad-beari ng structures made f r om bri ttl e
materials because i t rel ates the probabi l i ty of f ai l ure to the volume of
material under l oad, the stress gradi ent, and mul ti axi al stress states. I t
can be combined wi th f i ni te element stress anal ysi s to predi ct the prob-
abi l i ty of f ai l ure as a functi on of posi ti on i n components under complex
stress states. Previ ous studi es of the strength of H-327 graphi te (Ref.
5-7) and near-i sotropi c Gilsocoke-based graphi tes (Ref. 5-8) showed that
whi l e the rati os rel ati ng the strength of f l exural specimens and i nternal l y
pressuri zed tubes to the tensi l e strength were correctl y predi cted by the
Weibull model, the dependence of strength on specimen volume was over-
esti mated.
5-35
n
5.3.1 . Sampling
Sampling diagrams are shown i n Appendix A, Fi gs. A- 5, A-6, and A-7.
A l og from preproducti on l ot 408, log 5651-90, was wed.
of two si zes and f l exural specimens were taken i n both axi al and radi al
di recti ons from l ocati ons coveri ng most of the l og.
mens were tested to f ai l ure.
'I 'ensilc specimens
More than 2000 speci -
5.3.2. Concl usi ons
Complete data sets are reported i n Ref. 5-5. The fol l owi ng paragraphs
summarize the resul ts.
Axial tensi l e specimens averaged 19% stronger than radi al specimens,
and axi al f l exural specimens averaged 13% stronger than radial specimens.
Axi al specimens taken near the edge of the l og averaged 16% and f l exural
specimens 7% stronger than those taken near the center.
vari ati on f or axi al tensi l e strengths from the same zone i n the parent l og
averaged 11.2%, compared wi th 14.7% f or radi al tensi l e strengths.
the coef f i ci ent of vari ati on averaged 7.9% and 9.0% i n the axi al and radi al
di recti ons, respecti vel y.
The coef f i ci ent of
I n f l exure,
Wi thi n experi mental scatter, the data were equal l y wel l represented by
a normal (Gaussi an) di stri buti on or by a di stri buti on predi cted by the
Wei bul l model. The val ue of the Wei bul l modulus m was lower f or tensi l e
tests (mean val ues of 10.7 f or axi al specimens and 8.1 f or radi al speci -
mens) than f or f l exural tests (mean val ues of 15.8 f or axi al specimens and
13. 6 f or radi al speci mens).
based on the Wei bul l model.
mm and 724 mm ) were tested.
stronger than the l arge specimens f or the axi al and radi al di recti ons,
respecti vel y.
the Weibull model, which predi cted di f f erences of 28% and 38% f or the axi al
and radi al di recti ons, respecti vel y.
Such a di f f erence is contrary to predi cti ons
Tensi l e specimens of two si zes (volumes 9847,
The small specimens averaged 3% and 8%
3 3
The observed si ze ef f ect was much lower than expected from
n
5-3 6
The mean f l exural strength showed good correl ati on wi th the mean ten-
si l e strength of companion specimens (correl ati on coef f i ci ent 0.9). Flex-
ural strength averaged 52% and 55% hi gher than the correspondi ng tensi l e
strengths f or the axi al and radi al di recti ons, respecti vel y. These val ues
are i n good agreement wi th val ues of 51% axi al and 64% radi al predi cted by
the Wei bul l model. While there i s agreement between the experi mental
fl exure-to-tensi l e strength rati os and the rati os predi cted by the Wei bul l
model, the experi mental l y deri ved si ze ef f ect and the di f f erence i n Weibull
modulus between tensi l e and bend data are i nconsi stent wi th the Wei bul l
model. Thus, the H-451 graphi te l og tested does not meet the cri teri a which
would permi t i t to be treated as a Weibull sol i d.
When consi deri ng the minimum strength of H-451 l ogs f or acceptance/
rej ecti on tests, the data i n Ref. 5-5 confi rmthe resul ts from Ref. 5-1 that
the l ogs are weakest at the mi dl ength center (MLC). Thus, testi ng speci -
mens from the MLC zone consti tutes the most conservati ve cri teri on f or
el i mi nati ng weak or def ecti ve l ogs.
5.4. DEFINITION OF MI NI MUM STRENGTH AND STRENGTH DISTRIBUTION AMONG LOGS
Ni nety-ei ght f ul l - si ze (432 mm di ameter by 813 mm l ong) producti on
l ogs were manufactured, usi ng the same formul ati on, raw materials, and pro-
cedures as preproducti on l ot 426.
producti on order f orpossi bl euse as FSV rel oad el ements. The 354-log order
was manufactured i n 6 extrusi on l ots, taken through the baki ng process and
stored at GLCC.
tensi l e strength testi ng, and to ORNL and BNL f or experi mental purposes.
The 98 l ogs were taken from three of the producti on extrusi on l ots (472,
478, and 482). A l l l ogs were graphi ti zed i n furnace run number 1272.
The 98 l ogs were a porti on of a 354-log
The 98 l ogs were graphi ti zed and di stri buted to GA f or
5.4.1. Sampling
The l ogs were sampled for tensi l e testi ng by GLCC at thei r Morgantown
The sampl i ng di a-
pl ant i n accordance wi th a sampl i ng pl an devi sed by GA.
gram is gi ven i n Appendix A, Fi gs. A-8, A-9, and A-10. A rod 16 mm i n
5-1 7
di ameter by 356 mm l ong was cored from the center and a 25-mm sl ab was taken
from one end of each l og.
shown i n Fi g. A-9.
mi dl ength center (MLC) of each l og as possi bl e (wi thi n 51 mm of the center;
see Fig. A-8) whi l e preservi ng the l ogs f or subsequent machining i nto f uel
element bl ocks. Axi al test specimens 6. 35 mm i n di ameter by 23 mm l ong
were machined from the axi al core, as shown i n Fi g. A-9,and radi al specimens
of the same si ze were machined from the end sl ab, as shown i n Fig. A-10. A
si ngl e tensi l e test specimen ( 12. 8 mm i n di ameter by 76. 2 mm l ong) was taken
from each center core, as shown i n Fi g. A-8, f or measurement by GLCC.
A 102-mm core was taken f or axi al specimens, as
The GA axi al strength specimens were taken as cl ose to the
U l t i mat e tensi l e strength was measured on ei ght axi al specimens and
f our radi al specimens from each l og at GA, and one axi al specimen was meas-
ured from each l og at GLCC.
5.4.2. Experi mental Resul ts
I ndi vi dual strength val ues f or each l og and the mean val ues grouped by
extrusi on l ot are reported i n Ref. 5-9. The average strengths and standard
devi ati ons f or axi al specimens tested by GA and GLCC from each extrusi on
l ot are gi ven i n Tabl e 5-5. The grand mean of 12. 7 MPa f or GA data com-
pares wi th 13. 3 MPa f or GLCC's si ngl e specimens.
Correl ati on between the values f or GLCC's si ngl e specimen and the GA
average val ues was poor (Ref. 5-9). The di f f erence may ref l ect both the
spati al separati on of the sampling zones and the i nherent randomness of the
si ngl e specimen measured by GLCC. Stati sti cal tests showed no si gni f i cant
di f f erence i n mean val ues between A and B specimens (l ocated cl osest to the
l og center) and the C and D specimens; theref ore, they can be treated as
coming from the same popul ati on.
The di f f erences i n average strength (GA data) between the three ex-
trusi on l ots, as shown i n Tabl e 5-5, were stati sti cal l y hi ghl y si gni f i cant.
The small di f f erences i n standard devi ati on between the di f f erent extrusi on
l ots were not stati sti cal l y si gni f i cant.
5-1 8
TABLE 5-5
STATISTICAL ANALYSES OF GA AND GLCC AXI AL STRENGTH DATA
No. of
Specimens
Tested by:
Average Tensi l e Strength and
Standard Devi ati on ( ma)
GLCC
14
56
28
98
-
S
12.3
13.6
1 1 . 1
12.7 3.0
Lot No.
472
478
482
A 1 1
. * 13.8
GA
1 1 1
4 39
2 24
7 74
I
There was no correl ati on between strength and the posi ti on of the l og
wi thi n the graphi ti zati on furnace. The di f f erences between the average
strengthsof l ots 4 7 2 , 4 7 8 , and 482 were accounted f or by GLCC as di f f erences
i n processi ng duri ng extrusi on.
The average radi al strengths and standard devi ati ons f or each extrusi on
l ot are gi ven i n Tabl e 5-6. The grand mean was 15.8 MPa. The di f f erence i n
strength between l ots 472 and 478 was not stati sti cal l y si gni f i cant, but
l ot 482 was si gni f i cantl y weaker than the other two l ots.
the axi al strengths, the di f f erences i n standard devi ati ons were stati s-
ti cal l y si gni f i cant, wi th l ot 482 showing more vari abi l i ty than the other
two l ots.
vari abi l i ty and the within-log (specimen-to-specimen) variability.
I n contrast to
Thi s was attri butabl e to an i ncrease i n both the l og-to-l og
There was no stati sti cal l y si gni f i cant correl ati on between the radi al
strength and the axi al strength of the same l ogs (correl ati on coef f i ci ent
0. 11) .
specimens at the end-center posi ti on compared wi th the axi al speci mens at
the mi dl ength-center posi ti on are not unusual and have been observed i n
preproducti onl ogs (Refs. 5-1, 5-5). The di f f erences between the three l ots
show that material extruded i n di f f erent l ots can vary consi derabl y i n
The hi gher strength and reduced standard devi ati on of the radi al
strength properti es af ter baki ng i mpregnati on and graphi ti zati on.
5-39
Av c r il g C'
S t rcng t h
CLCC
Extrris i on No. o I-
Lot No. Spec i mms 'I'cistcd (Wa)
-___I- --.-___---I_
4 72 56 16.4
478 224 16.3
482 112 14.5
A 1 1 39 2 15.8
5.4.3. Appl i cati on of Resul ts to Acceptance Testi ng
Standard
Dev i ii t i on
(ma)
1.4
1.8
2.7
2.2
The strength of axi al midlength-center specimens was both l ower and
more scattered than the strength of radi al end-center specimens.
between extrusi on l ots and vari ati ons between l ogs wi thi n the same l ot both
contri bute to the scatter. The log-to-log vari ati ons appears to be too
great to al l ow qual i f i cati on of enti re l ots. Therefore, acceptance tests
i ntended to ensure minimum strength requi rements shoul d be based on axi al
mi dl ength-center specimens and each l og shoul d be tested.
Vari ati ons
5.4.3.1. Stati sti cal . Model. Acceptance cri teri a assume the fol l owi ng sta-
ti sti cal model (Ref. 5- 9) :
x
= p +ai +B , +Ei j
i j J
(5-9)
where x
p is the grand mean strength, ai is the vari ati on systemati c to the ith l ot,
6. is the vari ati on systemati c to the j th l og from thi s l ot, and E
i s an axi al strength measurement from the jth l og i n the ith l ot,
i j
is the
1 i j
-
random vari ati on (i n themi dl ength-center sampling zone) wi thi n thi s l og. It
was f urther assumed that a, 6, and E are normally and i ndependentl y di stri b-
- -
2
WL'
and u respecti vel y.
2
U
2
l ot' l og'
uted wi th means of zero and vari ances of u
The l atter three quanti ti es are, i n order, the vari ances attri butabl e to
n
5-20
l ot-to-l ot vari ati ons, log-to-log vari ati ons, and wi thi n-l og vari ati ons. I t
i s i mpl i ci t i n the model that the l og-to-l og vari ance i s the same f or al l
extrusi on l ots and the wi thi n-l og vari ance is the same f or al l l ogs.
Val ues f or the three components of vari ance were cal cul ated from the
test data by the anal ysi s-of-vari ance method. The cal cul ati ons confirmed
that both l ot-to-l ot and l og-to-l og vari ati ons were stati sti cal l y hi ghl y
2 2
WL
and 0 are shown in Tabl e 5- 7; the si gni f i cant. The val ues f or u 2 a
l ot l og
correspondi ng standard devi ati ons are al so i ncl uded.
The l argest contri butor to the spread i n the axi al strength measure-
ments i s the log-to-log vari ati on among l ogs from the same extrusi on l ot
(see Tabl e 5-7), whereas the wi thi n-l og vari ance [2.67 ( ma) ] is low enough
f or log-by-log acceptance tests based on a few specimens per l og to be
practi cabl e.
2
5. 4. 3. 2. Acceptance Cri teri a. The purpose of acceptance testi ng i s to
ensure that materi al from the weakest l ocati on (mi dl ength center) of the
l ogs meets the minimum strength requi rement Smin. Because of the vari abi l i ty
COMPONENTS
Source of Vari ati on
Lot- to-l o t
Log-to-log
Within-log (resi dual )
TABLE 5-7
OF VARI ANCE: AXI AL STRENGTH DATA
Var i anc e Devi ati on
5-2 3
i n graphi te strengths, a stati sti cal def i ni ti on of minimum strength is
requi red. The fol l owi ng two al ternati ve def i ni ti ons were consi dered:
90/90: A t l east 90% of the material at the mi dl ength center of the l og
equal s or exceeds a speci f i ed minimum strength, wi th 90%
confi dence.
90/95: A t l east 99% of the material at the mi dl ength center of the l og
equal s or exceeds a speci f i ed minimum strength, wi th 95%
confi dence.
An acceptance testi ng procedure which meets the needs can be deri ved
from the stati sti cal model of Eq. 5-9, i f i t i s assumed that the present
estimate of the wi thi n-l og variance [2.67 ( ma) ] i s exact and w i l l remain
unchanged i n f uture producti on runs. I t is assumed that n repl i cate speci -
mens from the mi dl ength center of a l og are tested and thei r average, x, i s
used to estimate the mean l og strength, p +ai +6 .
requi rement S
2
-
The mi ni mum strength
j
w i l l be met i f x meets the fol l owi ng cri teri on:
min
- 1.282
JT
WL
x 2 Smin +1.282 uWL +-
where a 90/90 def i ni ti on of minimum strength i s used, or
- 1 645
x 2 Smin +2.326 am +
(5-loa)
(5-lob)
where a 99/95,def i ni ti on of minimum strength i s used. The numeri cal f actors
i n Eq. 5-10 come from tabul ated val ues f or the standard normal di stri buti on.
5-22
Because di f f erent components i n the HTGR core experi ence di f f erent
stress l evel s, i t is desi rabl e to devi se an acceptance test that sorts the
lrigs accordi ng to thei r strength. Therefore, the fol l owi ng strength cate-
gori es were consi dered:
Category A: minimum strength 10.3 MPa
Category B: minimum strength 8.3 MPa
Category C: minimum strength 5.5 MF' a
The val ue which must exceed f or a l og to be assi gned to category A, B, or
C can be cal cul ated from Eq. 5-10. Values are shown i n Tabl e 5-8 f or f our
and ei ght repl i cate tests per l og, and f or 90/90 and 99/95 def i ni ti ons of
minimum strength.
The cri teri a l i sted i n Tabl e 5-8 were appl i ed to each of the 98 l ogs.
For the case requi ri ng f our repl i cate tests, the f our speci mens cl osest to
the l og center (subscri pts A and B; see Fi gs. A-8 and A-9b) were used. The
assi gned category f or each l og is gi ven i n Ref. 5-9 f or a four- or ei ght-
specimen sampling pl an, and f or a 90/90 or 99/95 def i ni ti on of minimum
strength.
5.4.3.3. Y i el ds of Logs by Category. A summary of the numbers of l ogs as-
si gned to each category under four- and eight-specimen sampling pl ans, apply-
i ng either a 90/ 90 or 99/95 def i ni ti on of minimum strength, i s gi ven i n
Tabl e 5-9. Resul ts are presented f or each extrusi on l ot.
Using a 90/90 def i ni ti on of minimum strength and an eight-specimen
sampling pl an, onl y two l ogs would be rej ected as f ai l i ng to qual i f y f or
strength category C, and al most hal f the l ogs would qual i f y f or category A.
I f a 99/95 def i ni ti on were used, 18 l ogs would be rej ected and about 20% of
the remai nder would qual i f y f or category A.
repl acement segment of an HTGR core would requi re about 25% of the accepted
l ogs to qual i f y f or category A and 70% to qual i f y f or A or B. I f a 99/95
A typi cal order of l ogs f or a
5-23
No. of
Tests per
Log
TABLE 5-8
CRI TERI A FOR ASSIGNING LOGS TO STRENGTH
CATEWRIES A, B, OR C (AXIAL DATA)
Def i ni ti on of
Minimum
Strength Smin
90/90 (b)
99/95(c)
90/90(b)
99/95(c)
S trengtva)
Category
A
B
C
A
B
C
A
B
C
A
B
C
Value Which Average
Measured Strength 2
Must Exceed
(MPa)
13.5
11.4
8.7
15.5
13.4
10.7
13.2
11.1
8.3
15.1
13.0
10.3
(a)Categori es correspond to the fol l owi ng minimum strengths:
A: 10.3 MPa
B: 8.3 MFa
C: 5.5 MPa
(b)At l east 90% of material at mi dl ength center exceeds speci f i ed
minimum strength, wi th 90% confi dence.
(')At l east 99% of materi al at mi dl ength center exceeds speci f i ed
minimum strength, wi th 95% confi dence.
5-24
No. of
Tests per
Log
4
8
TABLE 5-9
YIELDS OF LOGS I N EACH STRENGTH
CATEGORY (BASED ON AXI AL STRENGTHS)
Def i ni ti on
of Minimum
Strength
min
S
90 / 90 ( a )
99/95(b)
90/90 (a)
99/95 (b)
Extrusi on
Lot
472
4 78
482
A 1 1
472
4 78
4 82
A1 1
4 72
4 78
4 82
A 1 1
4 72
4 78
482
A l l
A
6
27
6
39
1
12
1
14
6
29
7
42
2
14
1
17
No. of Logs Assigned to
Strength Categor
B
-
3
22
6
31
5
16
5
26
3
22
6
31
4
20
6
30
-
C
4
6
13
23
3
26
7
36
4
5
14
23
4
20
9
33
Reject
1
1
3
5
5
2
15
22
1
0
1
2
4
2
12
18
1 To tal
14
5 6
28
98
14
56
28
98
14
56
28
98
14
56
28
98
(a)At l east 90% of material at mi dl ength center exceeds speci f i ed
minimum strength, wi th 90% confi dence.
(b)At l east 99% of material at mi dl ength center exceeds speci f i ed
minimum strength, wi th 95% confi dence.
5-25
minimum strength def i ni ti on were adopted i n place of the 90190 def i ni ti on,
the yi el ds i n the hi gher categori es would f nl 1 j ust short of these requi re-
ments, based on the qual i ty of the 98 l ogs consi dered i n thi s experi ment.
The ef f ect on the yi el ds of reduci ng the number of tests per l og from
ei ght to four i s smal l . The number of rej ects would i ncrease from two to
f i ve under a 90/90 strength def i ni ti on, and rej ects would be i ncreased from
18 to 22 under a 99/95 strength def i ni ti on. There would be some overal l
downgrading because more borderl i ne l ogs would be moved down i n categorythan
would be moved up.
The better qual i ty of extrusi on l ot 478, i ndi cated by i ts hi gher
average strength i n Tabl e 5-4, i s ref l ected i n the yi el ds l i sted i n Tabl e5-9.
Even usi ng a 99/95 def i ni ti on of minimum strength, onl y two of the 56 l ogsi n
l ot 478 would be rej ected and 25% would meet category A requi rements.
5.4.4. Concl usi ons
The axi al strengths (average val ue 12.7 MPa) from the MLC showed con-
si derabl e l ot-to-l ot and l og-to-l og vari ati ons, whi l e the radi al strengths
(average val ue 15.8 ma) from the EC were more uni form. There were no
stati sti cal l y si gni f i cant correl ati ons between axi al strength and radi al
strength i n the same l og, or between strength and the posi ti on of the l og
i n the graphi ti zi ng furnace.
Acceptance cri teri a f or assi gni ng l ogs to a minimum strength category
can be based on axi al tensi l e tests, i f each l og i s tested. A stati sti cal
model i ncorporati ng a separate l ot-to-l ot vari ance, l og-to-l og vari ance, and
wi thi n-l og vari ance can be adopted f or thi s purpose.
Acceptance cri teri a which coul d be used f or assi gni ng a l og to strength
category A (minimum strength 10.3 ma) , B (minimum strength 8.3 ma) , or
C (minimum strength 5.5 MPa) were deri ved. Cal cul ati ons were made f orei ther
four or ei ght repl i cate specimens per l og and two al ternati ve def i ni ti ons of
5-26
/ \
minimum strength were consi dered. The f i r st def i ni ti on would requi re 90%
of the material at the mi dl ength center of the l og to exceed the speci f i ed
minimum strength, wi th 90% confi dence (90/90); the second would requi re 99%
of the material to exceed the speci f i ed minimum, wi th 95% confi dence (99/95).
When these cri teri a were appl i ed to the axi al test data from the 98 l ogs,
two l ogs would f ai l to qual i f y f or category C, whi l e al most hal f of the l ogs
would qual i f y f or category A i f a 90/90 def i ni ti on of minimum strength and
ei ght specimens per l og were used.
strength would i ncrease the number of l ogs rej ected to 18. Decreasi ng the
number of tests per l og from ei ght to four would cause a s mal l reducti on i n
the yi el ds.
Use of a 99/95 def i ni ti on of minimum
Using a 99/95 def i ni ti on of minimum strength, onl y two of the 56 l ogs
i n the l ot of hi ghest average strength (478) would be rej ected and about 25%
would qual i f y f or category A.
40% f or l ogs from the other two lots.
Thi s compares wi th a rej ecti on rate of about
These resul ts provi de the i nformati on requi red to wr i t e an acceptance
speci f i cati on f or strength of a l og by measuring the tensi l e strength on
specimens taken at the MLC. The number of l ogs and specimens tested and
the confi dence requi red depend on the confi dence requi red i n desi gn.
5.5. FATIGUE BEHAVI OR
The graphi te f uel el ement bl ocks are subj ect to cycl i c stresses from
power cycl i ng, operati ng vi brati ons, and possi bl y seismic shaki ng. Design
of the components requi res a knowledge of the cycl i c f ati gue behavi or of
graphi te under l oadi ng cycl es wi th di f f erent rati os of minimum stress to
maximum stress (R val ue). The i nherent scatter i n mechani cal properti es
of graphi tes requi res that suf f i ci ent tests be made f or stati sti cal anal ysi s.
Uni axi al f ati gue tests were performed on H-451 graphi te wi th R val ues rang-
i ng from -1 to 0.5 (Ref. 5-10).
5-27
5.5.1. Sampling
Specimens f or uni rradi ated f ati gue testi ng of H-451 were taken i n the
axi al and radi al di recti ons a quarter of the way al ong the l ength of the
l og used f or wi thi n-l og strength testi ng (see Fi g. A-5 i n Appendix A)between
25 and 100 mm from the edge (see Fi g. A-11 i n Appendix A). For a gi ven
seri es of tests, specimens were taken from l ocati ons spread uni forml y over
the sampling zone to prevent bi as from l ocal i nhomogenei ti es i n strength.
Cyl i ndri cal specimens 12.7 mm i n di ameter by 25. 4 mm l ong were used.
5.5.2. Experi mental Procedure
The f i r st test series consi sted of 30 to 35 control tensi l e tests of
radi al and axi al specimens on standard f ati gue specimens mounted i n the
f ati gue machine. These tests establ i shed the mean tensi l e strengths of the
control specimens (see Appendix B, Tabl e B-10). Fati gue tests wer e run usi ng
R val ues of - 1, -0.5, 0, and 0.5. Forty to f i f ty specimens were i ncl uded i n
each series of tests. From seven to ten specimens were cycl ed at each of
f i ve maximum stress l evel s rangi ng from 0.6 to 1.0 times the mean tensi l e
strength. The stress l evel s were sel ected to avoi d an excessi ve number of
run-outs beyond 100,000 cycl es. Axial and radi al specimens were measured.
5.5.3. ExDerimental Resul ts
A typi cal S-N curve, taken from Ref. 5-10, i n which the l ogari thm of
the maximum stress S i s pl otted agai nst the l ogari thm of the number of
cycl es at f ai l ure N i s shown i n Appendix B, Fi g. B-1, f or axi al specimens
wi th an R val ue of -1. The stresses are normal i zed by di vi di ng by the mean
tensi l e strength. The tensi l e data and f i r st cycl e f ai l ures are pl otted at
N = 0.25, and run-outs (specimens which survi ved 100,000 cycl es wi thout
f ai l ure) are shown as open ci rcl es at N = 100,000.
5-28
The S-N curves have the same form as those of many metals, except that
the scatter band i s wi der. The data do not extend to hi gh enough val ues of
N to confi rm the exi stence of an absol ute endurance l i mi t .
The usual practi ce of anal yzi ng f ati gue data has been to deduce the N
val ue correspondi ng to a parti cul ar f ai l ure probabi l i ty from the di spersi on
of l og (N) val ues at a gi ven stress setti ng, assuming a Weibull or Gaussian
di stri buti on. Thi s procedure has several di sadvantages when appl i ed to
graphi te; i n parti cul ar, i t provi des no i nformati on on low f ai l ure probabi l -
i ti es i n the hi gh cycl e regime. The anal yti cal problem was approached i n
Ref. 5-10 by i nverti ng the usual practi ce and assuming that f or a constant
l i f e the f ai l ure stresses fol l ow a speci f i c di stri buti on (Ref. 5-11). The
fol l owi ng stati sti cal model was assumed (Ref. 5-10):
(5-11)
where u i s the peak tensi l e stress, S i s the mean tensi l e strength, crand
/3 are constants, and E i s a random vari abl e di stri buted normal l y wi th a mean
of zero and a standard devi ati on s. Data i n Ref. 5-10 were anal yzed accord-
i ng to the model of Eq . 5-11, i ncl udi ng the tensi l e tests at N = 0.25 but
excl udi ng the specimens which ran out beyond l o5 cycl es.
strai ght l i ne through the data and the x/ y lower tol erance l i mi t s (represent-
i ng the l i mi t s above which at l east x% of al l observati ons would f al l , wi t h
y% confi dence) were cal cul ated f or the x/y combi nati ons 90/90, 95/95, and
99/95 and are i ncl uded i n Appendix B, Fi g. B-1. The data support a l i near
rel ati on between l og (a ) and l og (N) assumed i n Eq. 5-11. Resul ts of
the stati sti cal anal yses are summarized i n Tabl e 5-10.
max
The l east-squares
max
For desi gn, i t i s conveni ent to pl ot f ati gue resul ts on a constant
l i f e f ati gue diagram (Goodman di agram), which relates f ati gue l i f e to the
fol l owi ng i nterdependent l oadi ng cycle parameters: maximum stress, minimum
stress, stress ampl i tude, and mean stress. The data i n Appendix B, Fi g. B-2,
provi de an example of a Goodman diagram, taken from Ref. 5-10, rel ati ng the
5-29
n

I
u

I

r
r
,

a
J

a
l

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T
-

a
m

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d

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G

a
J

.
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k

0

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r
o
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c
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)
o
l
n
m

C
O
b
\
o
9
c
n
C
O
b
b

0
0
0
0
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0
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a
3
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b
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5
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3
0

2 3 4 5
l oadi ng cycl e parameters f or 50% survi val to 10 , 10 , 10 , and 10 cycl es
i n axi al specimens of H-451 graphi te.
When normal i zed by di vi di ng by the mean tensi l e strength, the homologous
stress l i mi t s f or radi al specimens were somewhat greater than those f or axi al
specimens under si mi l ar condi ti ons (Tabl e 5-10).
Under reversed stress cycl i ng (R = - l ), the homologous stress l i mi t s
f or survi val of axi al specimens to l o5 cycl es averaged 0.63 f or 50% survi val
and 0. 48 f or 99% survi val (99/95 tol erance l i mi t) , i n good agreement wi th
L ei chter and Robinson's resul ts (Ref. 5-11). The homologous stress l i mi t s
f or radi al specimens averaged 0. 74 f or 50% survi val and 0.53 f or 99% survi val .
5. 5. 4. Concl usi ons
H-451 graphi te showed cycl i c f ati gue l i f e curves (S-N curves) general l y
resembl i ng those of metals, but wi th more scatter. For reversed stress
cycl i ng (R =- l ) , the homologous stressl i mi ts (maximum appl i ed f ati gue
stress di vi ded by the tensi l e strength) f or 50% specimen survi val to 10
cycl es averaged 0.63 i n the axi al di recti on and 0. 74 i n the radi al di recti on.
Corresponding homologous stress l i mi t s f or 99% specimen survi val (99/95
tol erance l i mi ts) were 0. 48 and 0.53. The f ati gue l i f e and the homologous
stress l i mi t s i ncreased as R i ncreased.
5
REFERENCES
5-1. J ohnson, W. R., and G. B. Engl e, "Properti es of Uni rradi ated Fuel
Element Graphi tes H-451 and TS-1240," ERDA Report GA-A13752, General
Atomic Company, J anuary 31, 1976.
Nye, J . F., Physi cal Properti es of Crystal s, Oxford Uni versi ty Press,
London, pp. 1-8, 1967.
5-2.
5-3. Engl e, G. B., and W. R. J ohnson, "Properti es of Uni rradi ated Fuel
Element Graphi tes H-451 and S0818," ERDA Report GA-A14068, General
Atomic Company, October 8, 1976.
5-31
n
5-4.
5-5.
5-6.
5-7.
5-8.
5-9.
5-10.
5-1 1.
Butland, A. T. D., and R. J . Maddison, "The Speci f i c Heat of Graphi te:
An Eval uati on of Measurements," J . Nucl. Mater. 49, (1973-74).
Pri ce, R. J ., "Stati sti cal Study of the Strength of Near-I sotropi c
Graphi te," ERDA Report GA-A13955, General Atomic Company, May 24, 1976.
Wei bul l , W. , "A Stati sti cal Theory f or the Strength of Materials,"
Hand. I ng. V et . Akad., Proceedi ngs, Royal Swedish I nsti tute f or
Engi neeri ng Research, Stockholm, Nr . 151, 1939.
Pri ce, R. J ., and H. R. W. Cobb, "Appl i cati on of Weibull Stati sti cal
Theory to the Strength of Reactor Graphi te," Proceedi ngs, Conference
on Continuum Aspects of Graphi te Design (CONF-701105), USAEC Techni-
cal I nformati on Center, 1972, p. 547.
Brockl ehurst, J . E., and M. I. Darby, "Concerning the Fracture of
Graphi te Under Di f f erent T est Condi ti ons," Mater. Sci . En&. 16, 91
(1974).
Engle, G. B., and R. J . Pri ce, "Strength Testi ng of Producti on Grade
H-451 Graphi te; L ots 472, 478 and 482," ERDA Report GA-A14269, General
Atomic Company, March 1977.
Pri ce, R. J ., "Cycl i c Fati gue of Near-I sotropi c Graphi te: I nfl uence
of Stress Cycle and Neutron I rradi ati on," DOE Report GA-A14588,
General Atomic Company, December 1977.
L ei chter, H. L ., and Robinson, E., "Fati gue Behavior of a High-
Densi ty Graphi te and General Design Correl ati on," J . Am. Ceram. SOC.
3, 197 (1970).
,
n
5-32
6. I RRADI ATI ON PROGRAM
6.1 . I NTRODUCTI ON
The properti es of H-451 graphi te duri ng i rradi ati on under HTGR condi-
ti ons of fl uence and temperature are requi red f or desi gn and saf ety anal yses.
I rradi ati on behavi oral studi es of H-451 graphi te began wi th the i rradi a-
ti on of grade H-429 i n a series of BNWL capsul es i n the ETR.
specimens were l ater transf erred to GA's OG capsul e series and i rradi ati on
conti nued i n the ORR. I rradi ati on of H-451 was i ni ti ated i n the OG capsul e
series. Capsul es OG-1, -2, and -3 were i rradi ated at 823 to 1623 K (550' to
135OOC) to a peak fl uence of 9 x
6-3). By operati ng the three capsul es i n series i t was possi bl e to obtai n
complete data sets over the fl uence and temperature range of the HTGR. The
capsul es were i rradi ated over a peri od of approxi matel y 5 years, and speci -
mens from the GLCC development program were i nserted i nto the program as they
became avai l abl e. Specimens from H-451 l ots 266, 408, and 426 were i rradi -
ated al ong wi th grade H-429.
The H-429
(Refs. 6-1, 6-2,
N/m (E > 29 fJ )HTGR
2
Dimensional changes and changes i n tensi l e strength, el asti c modulus
and strai n at f racture, f ati gue behavi or, thermal expansi vi ty, thermal con-
ducti vi ty, and i rradi ati on creep wer e determi ned. Within-log and between-l og
vari ati ons i n di mensi onal changes and properti es were determi ned. Some of
the specimens were i nterchanged wi thi n the capsul es on subsequent i rradi ati ons
to provi de data on the ef f ect on di mensi onal changes of i ncreasi ng and
decreasi ng the temperature duri ng i rradi ati on.
Fi gure 6-1 shows the fl uences and temperatures of the HTGR covered by
the i rradi ati on data. I n some i nstances the i rradi ati on data exceed the
temperature and fl uence range of the reactor.
Capsul e desi gn and constructi on detai l s are gi ven i n Refs. 6-1, 6-2,
and 6-3. The i rradi ati on data presented are excl usi vel y or H-451 except
f or changes i n thermal expansi vi ty and conducti vi ty, where data from grades
6-3
ENVELOPE FOR FIRST RELOAD SEGMENT.4 YEAR FUEL,
3000 MWM REACTOR
ESTIMATED CURVE
10 \ /FOR LEA0 PLANT
8 -
6 -
4 -
2 -
0 -
/
/
/
/
I
I
DIMENSIONS
AN0 THERMAL
EXPANSIVITY
a
W
+
I
- I 1
c
u
: 10
Y
N
S 8
=
z
L n N
THERMAL
CONDUCTIVITY
6
I
w
0
z w
3
U
- I 4
z
0
a
I - 2
a Y
z
z o
a
lo t I
4
:i 2
/' LOT266
[I
TENSILE STRENGTH
AND ELASTIC
MODULUS
- K 673 873 1073 1273 1413 1673
"C 400 600 800 1000 1200 1400
TEMPERATURE ("C)
t
Fi g. 6-1. H-451 graphite irradiation data
6-2
Q
TS-1240 manufactured by Union Carbi de Corporati on and grade SO818 by AirCo
Speer Di vi si on of A i r Reduction Corporati on were i ncl uded. These grades
wer e al so manufactured f or use as f uel el ement graphi tes i n HTGRs and are
si mi l ar to grade H-451. The TS-1240 and SO818 specimens were i rradi ated i n
the same cruci bl es wi th the H-451 speci mens.
6.2. SAMPLING
Diagrams of the sampling procedures f or i rradi ati on testi ng are gi ven
i n Appendix A, Fi gs. A-1, A-12, and A-13. The specimens were taken from
sl abs which were removed from the same l ogs as those used f or the characteri -
zati on studi es.
secti on of the l og and from the same specimen popul ati on as those used f or
i rradi ati on.
Uni rradi ated control specimens were taken from the same
6.3. DIMENSIONAL CHANGES
Dimensional change data are reported as percent strai n [ ( a - l l o)/k0 x
1001, where R i s the posti rradi ati on l ength and Ro i s the ori gi nal
(uni rradi ated) l ength.
6.3.1. 873 to 1673 K (600' to 14OO0C)
6.3.1.1. I sothermal Dimensional Changes. I n capsul e OG-3, the thi rd i n the
OG capsul e series, 219 axi al and 170 radi al di mensi onal change specimens of
H-451 graphi te wer e i rradi ated. Many of these specimens wer e previ ousl y
i rradi ated i n capsul es OG-I and -2 (Refs. 6-1, 6-2); thus, the total f ast
f l uence of some of these H-451 specimens exceeded the l i f eti me f l uence f or
HTGR f uel el ement bl ocks.
Specimens were i rradi ated at average temperatures rangi ng from 887 to
1673 K (600' to 1400'C) to total f ast neutron fl uences of 1.6 to 9.2 x 10 25
n/m (E > 29 fJ I HTGR. The data are shown i n Appendix B, Fi g. B-3 through
2
6-3
B-10. The cl osed symbols i n the f i gures represent i rradi ati on data from
previ ous OG series capsul es, whereas the open symbols represent the data
from capsul e 0 6 3 .
Q
Radi al H-451 specimens were i rradi ated to f l uences suf f i ci ent to show
turnaround i n di mensi onal change and, i n two specimens, a small net radi al
expansion. The earl i est change i n l i near di mensi onal change to net expan-
si on occurred i n H-451 graphi te i rradi ated at approxi matel y 1273 K (lOOOC) .
Radi al specimens appear to go to net expansi on when exposed to approxi matel y
9 x N/m (E > 29 fJ )HTGR neutron fl uence. Higher i rradi ati on tempera-
tures create a greater i ni ti al contracti on which del ays crossover to net
expansi on unti l a f ast fl uence of greater than 9 x
2
2
N/m (E > 29 fJ )HTGR.
These data and rel ated ef f ects were i ncorporated i nto the desi gn curves
fol l owi ng the procedures outlined i n R e f . 6-2. I sothermal secti ons through
the desi gn surf ace are shown i n Fi g. 6-2.
6 . 3 . 1 . 2 .
Af ter i rradi ati on i n capsul e O G l , two sets of f our axi al and f our radi al
specimens were i nterchanged between two cruci bl es f or the next two i rradi a-
ti on i ncrements.
948 K (675OC) and 1323 K (1O5O0C), respecti vel y.
presented i n Fig. 6-3; i sothermal curves are i ncl uded i n the f i gure. When
the i rradi ati on temperature of the axi al specimens was i ncreased, the shri nk-
age rate i ncreased to that of specimens i rradi ated i sothermal l y at the
hi gher temperature.
thei r i rradi ati on temperature was reduced, but remained hi gher than that of
specimens i sothermal l y i rradi ated at the lower temperature to the same
fl uence.
correspond to the lower temperature i sothermal curve extrapol ated to the
hi gher strai n of the stepped-down specimens. The data poi nts f or radi al
specimens are too cl osel y cl ustered to draw f i rm concl usi ons, but the trends
appear si mi l ar to those of the axi al specimens.
Ef f ect of Changing I rradi ati on Temperature on Dimensional Changes.
The mean operati ng temperatures of the cruci bl es wer e
The di mensi onal changes are
The shri nkage rate of axial specimens decreased when
The shape of the curves suggests that the new shri nkage rate may
6- 4
- 2t
-3 t
-4 t
I 1 I I I 1 I I I I
0 1 2 3 4 5 6 7 8 3 10
FAST NEUTRON FLUENCE N/m2) (E >29 FJ)HTGR
(b) AXIAL
1
1225 K (952OC) \
/ ' A
0
- 1
I I
-
-2 I I I
I I I I I I
0 1 2 3 4 5 6 7 8 9 10
FAST NEUTRON FLUENCE N/m2) (E >29 FJ)HTGR
Fig. 6- 2. I rradi ati on-i nduced di mensi onal change
i n H-451 graphi te (desi gn curves):
(a) axi al di recti on, (b) radi al di recti on
6-5
- 1
2
-
$ -2
a
W
a
z
I
u
J
z
v)
z
W
0
a
a
'1
z
-3
0
-1
AXIAL
h ISOTHERMAL
e- 948 - 1323 K
-b - 1323 - 948 K
(675'- 1050'C)
(1050' -675' C)
1338 K
- 1068'C)
1338 K
- 1068'C)
RAOIAL
2 4 6 8 10
FAST NEUTRON FLUENCE (1025 N I ~ ) (E >29 FJ)HTGR
0711 I
Fig. 6-3. Dimensional changes i n H-451 graphite irradiated
with changes i n temperature (from Ref.6-3)
6-6
6.3.1.3.
Several groups of H-451 specimens were made up from three di f f erent l ogs from
the same l ot.
i ncl uded. Four or f i ve repl i cates wer e used f or each l ot and l ocati on.
Between-Log and Within-Log Vari ati ons i n Dimensional Change.
I n some cases, specimens from the MLC and MLE i n thei l og were
Af ter posti rradi ati on l ength measurements, the data were anal yzed by the
anal ysi s-of-vari ance method to fi nd whether the between-log and wi thi n-l og
vari ati ons were stati sti cal l y si gni f i cant.
anal yses of vari ance are gi ven i n Tabl es 6-1 and 6-2.
nei ther the between-log nor the wi thi n-l og vari ati ons were si gni f i cant at
the 95% confi dence l evel .
specimens were not stati sti cal l y si gni f i cant f or H-451 graphi te.
Summaries of the resul ts of the
For H-451 graphi te,
Di fferences i n shri nkage between MLC and MLE
6.3.2. 573 to 873 K (300' to 60OoC)
Only a few data poi nts are avai l abl e on H-451 graphi te below 827 K
(600'C) from the OG capsul e series. Therefore, the main body of data f or
low-temperature i rradi ati on di mensi onal changes has been taken from UKAEA
resul ts (Ref. 6-4) on a near-i sotropi c graphi te (code No. PI ) i rradi ated
i n the Dounreay Fast Reacter (DFR) at temperatures between 633 and 873 K
(360' and 600OC).
paper (Ref. 6-5). The UKAEA graphi te was manufactured wi th near-i sotropi c
-6
coke and had a thermal expansi vi ty at 293 to 393 K (20' to 120'C) of 3 x 10
K ("C-') paral l el to extrusi on (axi al ) and 4.1 x 10 K ("C ) perpendi c-
ul ar to extrusi on (radi al ). Therefore, i ts di mensi onal change behavi or i s
expected to be s i mi l a r to that of H-451.
The UKAEA resul ts were col l ected and anal yzed i n a revi ew
-1 -6 -1 -1
The data poi nts from Ref. 6-4 are gi ven i n Appendix B, Fi gs. B-11 and
B-12. The f i gures al so i ncl ude Dragon data on extruded near-i sotropi c
graphi tts (graphi te reference numbers 100 and 120 from Ref. 6-6). A few GA
data poi nts on H-451 graphi te are al so i ncl uded. Agreement between the
three sets of data is good.
0
No i rradi ati on data below 360' to 400 C have been reported f or near-i so-
tropi c graphi tes. However, resul ts f or PGA (needle-coke) graphi te i rradi ated
i n DI DO and PLUTO at 573, 623, and 723 K (300, 350, and 450'C) are avai l abl e
6-7
TABLE 6-1
WI THI N-LOG VARI ATI ON I N I RRADI ATI ON-I NDUCED SHRINKAGE OF H-451 GRAPHITE, LOT 426
Ori entati on Cruci bl e
Edge of
Logs
0.75
0.18
0.30
1210 (9 37)
l l l O(837)
1200 (927)
Si gni f i cant at 95%
Confidence Level?
No
No
No
Mean Shri nkage (%)
Fast
Is Vari ati on
~
Axi al
Radi al
Radi al
Center of
Neutron
Fl uence x 10-25
[N/m2 (E > 29 fJ )HTCRl
6
8
3
2.68 I 0.71
Log 6484-34 Log 6L84-41
2.01 1 0.18
Si gni f i cant at 95%
Confidence Level?
2.83 1 0.36
Axi al
Radi al
Radi al
Radi al
Radi al
6 1 ZlO(937)
1 910 (637)
8 11 lO(837)
3 1200 (9 27)
6 1270(997)
TABLE 6-2
BETWEEN-LOG VARIATIONS I N I RRADI ATI ON-I NDUCED SHRINKAGE OF H-451 GRAPHITE, LOT 426
2.68
1.84
2.01
2.83
2.68
Mean Shri nkage (%)
Fast
1 Temp. I Fl uence x
I rrad. Neutron
0.71
0.18
0.17
0.28
0.79
Ori entati on I Cruci bl e 1
K ('C)
I [~/ m2 (E > 29 ~J )HTGR] I Log 6484-33
0.79
0.16
0.20
0.36
0.82
0.69
0.14
0.19
0.36
0.79
I Is Vari ati on
No
No
No
No
No
.o *
(Ref. 6 - 7 ) . The probabl e behavi or of near-i sotropi c graphi te at 573 K
( 300 C ) can be predi cted from t he P(: A d n t n by cal cul ati ng the vol umetri c
shri nkage rates at 573 and 723 K (300" and 450 C ) and assuming that the rati o
between the rates at these two temperatures i s the same f or near-i sotropi c
graphi te and PGA. Thi s procedure was appl i ed to the near-i sotropi c 723 K
( 450 C) experi mental data i n Fi gs. B-11 and B-12. The cal cul ated 573 K
(300' C) vol umetri c shri nkages were then converted to l i near shri nkage by
assuming that the rati o of axi al to radi al shri nkage i s the same at 573 K
(300OC) as at 723 K (45OOC).
0
0
6. 4. TENSI LE STRENGTH, ELASTIC MODULUS, AND STRAIN AT FRACTURE
6 . 4 . 1 . 823 to 1623 K (550' to 135OOC)
Approximately 500 tensi l e tests measured at ambient temperature were
conducted on H-451 graphi te specimens from l ots 2 6 6 , 408, and 426 i rradi ated
at several di f f erent fl uences and temperatures i n capsul es OG-1, - 2 , and - 3.
The percent i ncreases i n tensi l e strength and el asti c modulus (ref er-
enced to uni rradi ated control specimens from the same l ocati on i n the same
l og) are pl otted as functi ons of f ast neutron fl uence i n Fi g. B-13. For
H-451 graphi te, the data f or al l ori entati ons, l ocati ons, and l ots f al l i n
the same scatter bands.
The stati sti cal spread i n strength val ues i s an i mportant parameter i n
the mechani cal desi gn of graphi te structures. I rradi ati on causes a si gnf i -
cant i ncrease i n the standard devi ati on. However, the coef f i ci ent of varia-
ti on (standard devi ati on di vi ded by the mean) i s unaffected by i rradi ati on.
The esti mated coef f i ci ent of vari ati on showed no def i ni te trend wi th irra-
di ati on.
Design curves presentl y used f or the i rradi ati on-i nduced i ncrease i n
el asti c modulus (Ref. 6- 2) are based on Dragon proj ect data (Ref. 6- 6) f or
change i n soni c el asti c modulus of a near-i sotropi c pi tch coke graphi te.
The Dragon data cover a wide range of temperatures and fl uences (see Fi g.
6-9
B- 14) .
Dragon curves. The desi gn curves as shown i n Fi g. B-13 from Ref . 6-2 w i l l
The GA data on H-451 graphi te are i n excel l ent agreement wi th the
conti nue to be used.
A desi gn method f or accounti ng f or the i rradi ati on-i nduced strength
increase. uti l i zi ng al l the avai l abl e data i s recommended (Ref. 6- 3) . The
i ncrease i n strength S i s assumed to be rel ated to the i rradi ati on-i nduced
i ncrease i n el asti c modulus E as fol l ows:
s/so = ,
where the exponent k depends on the graphi te grade.
0. 64 f or axi al and radi al specimens was obtai ned from the current H-451 data.
This k val ue i s ref l ected i n the desi gn curves f or the strength data pl otted
i n Fi g. B- 13.
An average k val ue of
6. 4. 2. 627 to 873 K (350' to 600'C)
Measurements of changes i n el asti c modulus (by a soni c method) and
strength (tensi l e and bri ttl e- ri ng tests) were obtai ned on near-i sotropi c
graphi te i rradi ated i n the DFR under the UKAEA program (Refs. 6- 4, 6-8).
Resul ts from Ref . 6-8 f or material i rradi ated at 623 to 713 K (350' to 44OOC)
are shown i n Appendix B , Fi g. B-15. The f racti onal i ncrease i n strength
equal s the square root of the f racti onal i ncrease i n the el asti c modulus,
i ndi cati ng that the strai n energy to f ai l ure remains constant.
(Ref. 6- 4) show that thi s rel ati on hol ds to about 3 x N/m
(E ' 29 fJ )HTGR (2 x
somewhat at hi gher fl uences.
Later data
2
2
N/m NDE), but the strength may decrease
Dragon has reported (Ref. 6- 6) changes i n the soni c el asti c modulus of
near-i sotropi c graphi tes i rradi ated at 673 and 873 K (400' and 600OC) to
( 3 to 4 x NDE). The fl uences of 4.5 to 6 x N/m (E > 29 fJ l HTGR
Dragon data are shown i n Appendix B , Fig. B-14. The 673 K (40OOC) i ncreases
are consi stent wi th the hi gher fl uence data al so shown i n Fig. B-14. Design
curves f or the stati c el asti c modulus have been deri ved from the Dragon data
2
6-30
n
(Ref. 6- 6) usi ng a mul ti pl e of 0. 8 to convert dynamic modulus to stati c
modulus (uni rradi ated graphi te) and a mul ti pl e of 0. 6 to convert fl uence
( E > 29 f.J ) to fl uence (NDE) (Ref. 6 - 3 ) . For i rradi ated graphi te, the soni c
and stati c el asti c moduli were assumed qual . Curves f or temperatures other
than 673 and 873 K (400' and 600'C) were obtai ned by i nterpol ati on.
cal cul ated desi gn curves are shown i n Appendix B, Fi g. B-16. For the low-
temperature data, the i ncrease i n strength was assumed equal to the square
root of the i ncrease i n modulus (Ref. 6- 5) :
The
However, Eq. 6-1 was used i n the desi gn data manual (GA-A14428; see Secti on
2 ) f or the temperature range 623 to 1673 K (350' to 1400' C).
6. 4. 3. Between-Log and Within-Log Vari ati ons i n Strength I ncrease
Three groups of tensi l e specimens of H-451 graphi te were made up from
three di f f erent l ogs from lot 426, and three groups contai ned specimens from
both the MLC and the MLE. Five or more repl i cate specimens were used from
each l og and l ocati on. The i rradi ati on-i nduced percent strength i ncreases
(referenced to control specimens from the same l og and l ocati on) were
anal yzed by the anal ysi s-of-vari ance method. I ndi vi dual strength val ues are
gi ven i n Ref . 6- 3. The resul ts of the comparison are summarized i n Tabl es
6-3 and 6-4. Among one group of specimens, those from one l og showed a
si gni f i cantl y smaller i ncrease than those from the other two l ogs, but thi s
was not the case f or the other two groups (see Tabl e 6- 3) .
si gni f i cant di f f erences i n the strength i ncreases between specimens from the
center of the l og and specimens from the edge of the l og (see Tabl e 6- 4) .
There were no
6-1 1
TABLE 6-3
BETWEEN-LOG VARIATIONS I N I RRADI ATI ON-I NDUCED STRENGTH INCREASE OF H-4 51 GRAPHITE,
~~
Ori entati on
Radial
Radial
Axial
LOT 426
Fast Neutron Mean Strength I ncrease (%)
-25
I rrad.
Fluence x 10
Temp,
Cruci bl e No. K ("C) [ N h 2 (E > 29 fJ >HTGF] Log 6484-33 Log 6484-34 Log 6484-41
8 1 1 l O( 837) 2.01 28 32 39
6 1 210( 937) 2.68 41 56 48
3 1200 ( 9 27) 2. 83 57 35 60
Cruci bl e No.
1
8
6
QI
1 L
N
I rrad. Fast Mean Strength I ncrease (%) Is Vari ati on
K ("C) [ N/ m2 (E > 29 fJ )HTGR] Center of Logs Edge of Logs Confidence Level?
940( 667) 4.6 33 4 3 No
1150( 877) 4.1 31 44 No
1210( 937) 2.7 50 46 No
Si gni f i cant at 95%
-25
Temp, Neutron Fluence x 10 Lot
No.
4 08
408
4 26
-
Is Vari ati on
Si gni f i cant at 95%
Confidence Level?
No
Yes
No
i
6.5. FATI GUE BEHAVIOR
6.5.1. Sampling and Procedures
The experi mental procedures descri bed f or uni rradi ated specimens i n
Secti on 5. 4. 2 were al so used to test i rradi ated specimens. Specimens were
taken from the same regi ons as those f or i rradi ated tensi l e strength testi ng.
Three groups of H-451 specimens were i rradi ated i n graphi te cruci bl es i n
capsul es OG-1, -2, and -3 (Refs. 6-1, 6-2, 6-3). The specimens were i rradi -
ated at 1173 to 1273 K (900' to 1000C) to di f f erent neutron fl uence expo-
sures. Ten specimens out of each group were tensi l e- tested i n the f ati gue
machine to establ i sh the mean tensi l e strength. The val ues are l i sted i n
Appendix B y Tabl e B-11, together wi th the strengths of uni rradi ated companion
specimens from the same l ocati on i n the l og and the i rradi ati on condi ti ons.
A l l groups showed the expected i ncrease i n strength af ter i rradi ati on. The
remai nder of the specimens i n each group were used f or tensi on-compressi on
f ati gue tests (R =- 1).
l evel s unti l they f ai l ed or reached 100,000 cycl es wi thout f ai l ure.
Ei ght specimens were cycl ed at each of four stress
6.5.2. Experi mental Resul ts and Di scussi on
A homologous stress S-N curve (anal ogous to the curve f or uni rradi ated
specimens i n Fi g. B-1) f or axi al specimens of H-451 graphi te i rradi ated to
at 1173 K (900C) i s shown i n Appendix B, 3.0 x lo2' N/m (E > 29 fJ >HTGR
Fi g. B-17. Comparison between the resul ts i n Fi g. B-17 and the uni rradi ated
resul ts (Fi g. B-1) shows that the homologous stress l i mi t s f or f ati gue
endurance are i ncreased by neutron i rradi ati on. The resul ts of stati sti cal
anal yses of the S-N curves f or al l the i rradi ated H-451 specimens are gi ven
i n Tabl e 6-5. The homologous stress l i mi t s f or survi val to IO5 cycl es are
substanti al l y hi gher than f or uni rradi ated H-451 tested wi th R = -1 (Tabl e
6-5), at least f or the axi al specimens. The homologous stress 99/95 lower
tol erance l i mi t i s lower at hi gher f l uences as the resul t of i ncreased data
scatter, but i t remai ns above the uni rradi ated l evel . The i ncreased scatter
may be caused by sl i ght warpage i n the hi ghl y i rradi ated specimens, which
i nterf eres wi th accurate uni axi al al i gnment i n the test ri g.
2
6-13
TABLE 6-5
RESULTS OF STATISTICAL ANALYSIS OF FATIGUE DATA FOR H-451 GRAPHITE IRRADIATED AT
1173 to 1263 K (900' to 990'C) (STRESS RATIO, R = -1)
Standard
Devi ati on
s(a)
0.046
0.044
0.056
0
Homologous Stress L i mi t max/S
f or Survi val to 105 cycl es (a)
99/95 Lower
50% Probabi l i ty Tol erance L i mi t
0.93 0.66
0.74 0.54
0.81 0.51
(a)Based on the model of Eq. 5-11.
Ori entati on
rn Axi al
I
1l
.b Rad i al
Axi al
I ntercept of
Least Sq a es
Li ne a 'tat
Fast Neutron
Fl uence N/ m2)
(HTGR)
3 .O
5.7
8.5
- -
-0.010
-0.020
-0.033
Sl ope of
Least Squares
L i ne ~( a )
-0.004
-0.022
-0.012
I f the f ati gue stress l i mi t s are normal i zed by di vi di ng by the uni rra-
di ated tensi l e strength i nstead of tlie i rradi ated tensi l e strength, the
l i mi t s i ncrease by more than a f actor of two duri ng i rradi ati on. The stress
l i mi t s f or 50% survi val to 10 cycl cs and the 99/95 l ower tol erance l i mi t s
normal i zed to the uni rradi ated strength are pl otted agai nst neutron fl uence
i n Fi g. 6-4.
5
6.6. THERMAL EXPANSI VI TY
6.6.1. 823 to 1623 K (550' to 135OOC)
Thermal expansi vi ty measurements were made on H-451 graphi te (10~s 266
and 426) and H-429 (Refs. 6-1, 6-2, 6-3). A l l except H-451 ( l ot 426) had
been i rradi ated i n previ ous capsul es. Data on grades TS-1240 and SO818 are
i ncl uded (see Secti on 6.1). Measurements were made between room temperature
and up to 100 K ("C) below the i rradi ati on temperature.
The accumul ated data on near-i sotropi c graphi tes H-451, H-429,
TS-1240, and SO818 from capsul es OG-1, -2, and -3 are summarized i n Appendix
B, Tabl es B-12 through B-15. The f racti onal change i n thermal expansi vi ty
is pl otted as a functi on of f ast neutron fl uence i n Appendix B, Fi gs. B-18
and B-19. A t the l owest i rradi ati on temperatures [865 to 1045 K (592'to
772"C)I the thermal expansi vi ty fi rst i ncreases by 5% to 10% and then
sl owl y decreases. A t hi gher i rradi ati on temperatures, the thermal expansi -
vi ty decreases by as much as 50% of i ts prei rradi ati on val ue, wi th the
decrease most marked at the hi ghest i rradi ati on temperatures. Data from
al l the near-i sotropi c graphi tes f al l i nto the same band regardl ess of
ori entati on and l og l ocati on, wi th the excepti on of H-429, f or which i rradi a-
ti on-i nduced changes i n thermal expansi vi ty are somewhat l ower than the
others.
For conveni ence i n desi gn cal cul ati ons, the data f or i rradi ati on-i nduced
f racti onal changes i n thermal expansi vi ty, (ai - a ) / a o , of the H-451 and
other near-i sotropi c graphi tes were f i t to the fol l owi ng pol ynomi al (Ref.
0
6-9) :
6-15
16 c
1 0
0 8
0 6
1 4
1 2
0 8
A AXI AL , 50" SURVI VAL
0
0 RADI AL , 50 SURVI VAL
0
AXI AL . 99 95 LOWER TOLERANCE L I MI T
RADI AL , 99' 95 LOWER TOLERANCE L I MI T
0 RADI AL , 50 I SURVI VAL
0 RADI AL , 93/ 95 LOWER TOLERANCE L I MI T
H-451 GRAPHI TE
I RRAOI ATED AT 1173 1263K
REVERSED STRESS CYCLE I R =- 1 )
FAST NEUTRON FLUENCE 11025N:m2) (E >29 f J ) HTGR
5
Fi g. 6- 4. Fati gue stress l i mi t s f or survi val of H-451 graphi te to 10
normalized to the uni rradi ated tensi l e strength, versus the f ast
neutron f l uence at an i rradi ati on temperature of 1173 to 1263 K
cycl es,
(900" to 990C)
I
d3
-7 2
(ai - ao)/ao = (0.27830 - 4.2734 x
T +1.7815 x 10 T ) @
(6-4)
-2 2 -3 @3
-2.0664 x 10 @ +1.3601 x 10
where T i s the i rradi ati on temperature ( " C) and @ i s the neutron fl uence
(lo2' N/ m2 ( E > 29 fJ)HTcR]. Curves cal cul ated from the equati on are
i ncl uded i n Appendix B, Figs. B-18 and 11-19. The standard devi ati on of data
point-s from the desi gn curves i s 0.063.
6.6.2. 623 to 823 K (350' to 55OoC)
The thermal expansi vi ty data of near-i sotropi c graphi te samples i rradi ated
i n the DFR (Ref. 6-4) are reproduced i n Appendix B, Fi g. B-20. No i rradi a-
ti on temperature ef f ect i s apparent f or the temperature range 623 to 823 K
(350' to 5 5 OOC. )
The rati o of posti rradi ati on thermal expansi vi ty to prei rradi ati on
expansi vi ty taken from Fi g. B-20 i s tabul ated as a functi on of f ast fl uence
i n Tabl e 6-6.
at temperatures between 573 and 873 K (300' and 600') are deri ved from the
f actors i n Tabl e 6-6.
The thermal expansi vi ty of near-i sotropi c graphi te i rradi ated
6.7. THERMAL CONDUCTIVITY
6.7.1. 923 to 1623 K (650" to 1350C)
Thermal di f f usi vi ty measurements were made on di scs of H-451 ( l ots 266
and 426) graphi te i rradi ated at three temperatures [(925, 1220, and 1615 K
(652", 947" , and 1342OC)I (Ref. 6-3). The H-451 specimens from l ot 266
had been previ ousl y i rradi ated i n earlier OG capsul es (Refs. 6-1, 6-2). The
measurements were made by the heat-pul se method and the thermal di f f usi vi ty
val ue was converted to the thermal conducti vi ty by mul ti pl yi ng by the den-
si ty and heat capaci ty.
temperature and 1073 K (800), except for the specimens i rradi ated at 925 K
Readings were taken every 100 K (OC) between ambient
(652OC), when the upper measurement temperature was l i mi ted to 773 K (500 0 C)
to avoi d the possi bi l i ty of anneal i ng.
6-1 7
TABLE 6-6
INCREASE I N THERMAL EXPANSIVITY OF NEAR-ISOTROPIC GRAPHITE
IRRADIATED BETWEEN 623 AND 823 K (350' AND 55OOC)
' Fast Fl uence
[1025N/m2 (E > 29 fJ )HTGR]
0
5
6
7
8
9
10
11
12
13
14
15
Rati o of Posti rradi ati on Expansi vi ty
to Prei rradi ati on Expansi vi ty al a,
1.00
1.09
1.13
1.15
1.18
1.19
1.20
1.21
1.22
1.21
1.20
1.20
1.19
1.18
1.18
1.17
6-1 8
llie accumulated data on near-i sotropi c graphi tes H-451, TS-1240, and
SO818 from capsul es OG-1, -2, and -3 are summarized i n Appendix B, Tabl es
B-16, B-17, and B-18. The conducti vi ty at the i rradi ati on temperature i s
pl otted as a functi on of f ast neutron fl uence i n Fi g. B-21. I rradi ati on
rapi dl y reduces the thermal conducti vi ty to a saturati on l evel which
i ncreases wi th i ncreasi ng i rradi ati on temperature. The thermal conducti vi ty
of al l the near-i sotropi c graphi tes tested f al l s i nto the same band af ter
i rradi ati on, even though some di f f erences exi sted i n thei r prei rradi ati on
conducti vi ti es. The i rradi ated val ues are i n excel l ent agreement wi th the
desi gn equati ons currentl y i n use (Ref. 6-2).
6.7.2. 523 to 923 K (250' to 650'C)
The thermal conducti vi ty ( at room temperature) of near-i sotropi c
graphi tes i rradi ated i n the DFR was measured by the UKAEA (Ref. 6-8).
Changes i n thermal resi sti vi ty f or the grade (code-numbered PI , paral l el
to extrusi on) are gi ven i n Ref. 6-8 and are repl otted i n Appendix B, Fi g.
B-22. Higher fl uence resul ts are contai ned i n Ref. 6-4. A few data
poi nts at 807 to 923 K (435" to 650C) on near-i sotropi c pi tch-coke
graphi tes were reported by Dragon i n Ref. 6-6 and these poi nts are al so
i ncl uded i n Fi g. B-22.
The experi mental data on near-i sotropi c graphi tes do not extend down to
573 K ( 3 OOOC) and are not suf f i ci ent to show the shape of the curve at low
fl uences. However, a consi derabl e amount of thermal conducti vi ty data on
PGA graphi te i rradi ated between 523 and 923 K (250' and 650'C) i s avai l abl e
from the AGR program (Refs. 6-10, 6-11). Curves taken from Ref. 6-10 showing
the f racti onal change i n thermal resi sti vi ty of PGA graphi te are i ncl uded i n
Appendix B, Fi g. B-22. The sol i d carves correspond to experi mental data, and
the dashed curves are extrapol ati ons. The data poi nts f or near-i sotropi c
graphi te are i n good agreement wi th the PGA curves.
To obtai n val ues usef ul f or desi gn, the f racti onal changes i n thermal
resi sti vi ty gi ven by the smoo'th curves i n Fi g. B-22 wer e appl i ed to the
measured room temperature conducti vi ty of H-451 graphi te, i nterpol ati ng
6-1 9
between the curves f or cal cul ati ons at i ntermedi ate temperatures. The con-
ducti vi ty at the i rradi ati on temperature was cal cul ated by assuming that f or
gi ven i rradi ati on condi ti ons, i rradi ati on adds the same increment to the
thermal resi sti vi ty at al l measurement temperatures (Ref. 6-12). The resul ts
of the cal cul ati ons are gi ven i n Appendix B, Tabl e B-19.
6.7.3. Ef f ect of Change i n Temperature
Two radi al specimens of H-451 graphi te which had been i rradi ated previ-
ousl y i n capsul e OG-1 at 1623 K (135OOC) were rei rradi ated i n OG-3 at 923 K
(65OoC), and two specimens formerl y i rradi ated at 873 K (6OOOC) were reirra-
di ated at 1613 K (1342OC). I n both cases the new conducti vi ti es were equal
to the saturati on l evel f or the new i rradi ati on temperature. Thi s behavi or
i s consi stent wi th the currentl y used desi gn model f or the conducti vi ty of
graphi te subj ected to a changi ng i rradi ati on temperature.
6.8. I RRADI ATI ON-I NDUCED CREEP
Two programs are currentl y under way on H-451: (1) compressi ve creep
experi ments at ORNL and (2) a tensi l e creep experiment at RCN and J RC Euratom,
Petten. Creep coef f i ci ents f or desi gn have been taken froi., an anal ysi s of
restrai ned shri nkage experi ments conducted at RCN, Petten, on H-451 graphi te
and a si mi l i ar molded grade (AGL grade SMI-24) (Ref. 6-13). I rradi ati on
creep i n H-451 graphi te may be represented by the equati on:
- 24
E = 4.16 x u [l - exp (-5 x 10 y)]exp(1.27 x 10-3T)
cr
t 6.2 x u y exp(7.48 x 10-4T)
where E: i s the total creep strai n (uni tl ess),
cr
u i s the appl i ed stress, MPa,
y
T i s the temperature i n K .
2
is the f ast neutron fl uence, N/ m
(E > 29 fJ )HTGR,
n
6-20
The equati on appl i es between 773 and 147'3 K (500" and 12OOOC) to a fl uence of
f or tensi l e strai ns l ess than 2.5% or compressive N/ m (E > 29 fJ )HTGR
2
strai ns less than 2%.
6.8.1 . Concl usi ons
Several i nvesti gators have establ i shed that the form of the f ast-
neutron-irradiation-induced creep curve f or graphi tes consi sts of a peri od of
transi ent creep, which rapi dl y saturates, followed by steady-state creep,
where the creep strai n i ncreases l i nearl y wi th f l uence. The onl y possi bl e
excepti on appears to be Gray's resul ts (Refs. 6-34, 6-15) f or compressive
creep i n i sotropi c graphi tes at 1073 K (800 C) where the creep rate slowed
down at f l uences above 6 to 7 x
si ve creep strai n exceeded 2%. Another possi bl e i ndi cati on of reduced creep
rates at hi gh f l uences may be i nf erred from the LJKAEA restrai ned shri nkage
resul ts on i sotropi c graphi tes i rradi ated i n the DFR.
0
when the compres-
N/m (E > 29 fJ )HTGR
2
REFERENCES
6-1. Pri ce, R. J ., and L. A. Beavan, "Fi nal Report on Graphi te I rradi ati on
T est OG-1," USAEC Report GA-A13089, General Atomic Company, August 1,
1974.
6-2. Pri ce, R, J ., and L. A. Beavan, "Fi nal Report on Graphi te I rradi ati on
T e s t OG-2," ERDA Report GA-A13556, General Atomic Company, December 15,
1975.
6-3. Pri ce, R. J ., and L. A. Beavan, "Fi nal Report on Graphi te I rradi ati on
T est OG-3," ERDA Report GA-Al4211, General A tomi c Company, J anuary
1977.
6-4. Kel l y, B. T., et al ., "Studi es of I rradi ati on Damage i n Carbons and
Graphi tes Appropri ate to MK I1 Gas-Cooled Reactors (AGRs) and the
MK 111Gas-Cooled Reactors (HTGRs)," Proceedi nns, Fourth UN I nt.
Conf. on Peaceful Uses of Atomic Energy, Geneva, 1971, v. 10, I AEA,
Vienna, 1972, p. 399.
6-2 1
6- 5.
6- 6.
6- 7.
6- 8.
6- 9.
Pr i ce, R. J . , "Pr oper t y Changes i n Near I sot r opi c Gr aphi t es I r r adi at ed
a t 300C to 600C: A Li t er at ur e Sur vey, " ERDA Repor t GA- A13478,
Gener al At omi c Company, J une 13, 1975.
Ever et t , M. R. , et al . , "I r r adi at i on Per f or mance and Sel ect i on of
Gr aphi t es f or HTGRs, " Dr agon Repor t DP- Repor t - 877, Apr i l 1974. .
Kel l y, B. T. , et al . , "Di mensi onal Changes i n Pol ycr yst al l i ne Gr aphi t e
Under Fast - Neut r on I r r adi at i on, " Phi l . Tr ans. Roy. SOC. London,
Ser. A, 260, 51 (1966).
Net t l ey, P. T. , et al . , "I r r adi at i on Exper i ment wi t h I sot r opi c
Gr aphi t e, " Pr oceedi ngs, Symposi umon Advanced and Hi gh Temper at ur e
Gas- Cool ed React or s, J Gl i ch, Oct ober 21- 25, 1968, I EAA, Vi enna, 1969,
p. 603.
Pr i ce, R. J . , "Cycl i c Fat i gue of Near - I sot r opi c Gr aphi t e: I nf l uence
of St r ess Cycl e and Neut r on I r r adi at i on, " DOE Repor t GA- A14588,
Gener al At omi c Company, December 1977.
6- 10. Mar t i n, W. H. , and A. M. Pr i ce, "Det er mi nat i on of Dose and Temper a-
t ure of Gr aphi t e I r r adi at i on Exper i ment s i n t he Dounr eay Fast
React or , " J . Nucl . Ener gy 2 l , 359 (1967).
6- 11. Br i dge, H. , et al . , "Ef f ect of Hi gh- Fl ux Fast - Neut r on I r r adi at i on on
t he Physi cal Pr oper t i es of Gr aphi t e, " Car bon 2, 83 (1964).
6- 12. Pr i ce, R. J . , "Ther mal Conduct i vi t y of Neut r on I r r adi at ed React or
Gr aphi t es, " USAEC Repor t GA- A13157, Gener al At omi c Company, Oct ober
1974.
6- 13. Ver i nga, H. J . , and R. Bl ackst one, "Radi at i on Cr eep i n React or
Gr aphi t es f or React or Appl i cat i ons, " Car bon - 14, 279 (1976).
6- 14. Gr ay, W. J . , "Const ant St r ess I r r adi at i on Cr eep Exper i ment s on
Gr aphi t e, " Pr oceedi ngs of t he Car bon - 72 Symposi um, Baden- Baden,
J une 1972.
6- 15. Gr ay, W. J . , "Techni cal Act i vi t i es Quar t er l y Pr ogr ess Repor t , AEC
React or Devel opment and Technol ogy Pr ogr ams, J an, - Mar . , 1971, "
n
USAEC Repor t BNWL- 1522- 2, Paci f i c Nor t hwest Labor at or y, 1971, p. 8.1.
n
6- 22
7. OXI DATI ON PROGRAM
Two t ypes of wat er l eaks ar e i mpor t ant i n det er mi ni ng t he ef f ect of
st eamoxi dat i on on t he f uel el ement : (1) hi gh wat er concent r at i ons, up to
1000 kPa (10 atm), whi ch may occur i n t he event of a l ar ge st eaml eak, and
(2) l owwat er concent r at i ons, up t o 50 Pa ( 500 uat m) , whi chcoul d occur dur -
i ng nor mal oper at i on.
above on t he i nt egr i t y of t he f uel el ement gr aphi t e over t he cor e l i f e of
t he f uel el ement s, i t i s necessar y to det er mi ne ( 1) oxi dat i on r at es of H- 451
i n st eam- hel i ummi xt ur es as a f unct i on of H 0 and H concent r at i on, r eact i on
t emper at ur e, degr ee of bur nof f , and sampl e conf i gur at i on, and (2) cl xi nges in
st r engt h and el ast i c modul us due to oxi dat i on bur nof f s.
To assess t he ef f ect s of wat er i ngr ess as descr i bed
2 2
7.1. OXI DATI ON RATE OF H- 451 GRAPHI TE
7.1 .l . React i on Rat e Theor y
React i on r at e t heory f or st eam- gr aphi t e r eact i ons i s di scussed i n de-
t ai l i n Ref s. 7-1 and 7-2. The ext ent of t he r eact i on of wat er vapor wi t h
the H- 451 graphi te i n an HTGR is cal cul at ed (predi cted) ut i l i z i ng computer
codes OXI DE- 3 ( Ref . 7- 3) and GOP ( Ref . 7-4) wi t h appr opr i at e i nput of r eac-
t i on r at e dat a.
The r eact i on of wat er vapor wi t h gr aphi t e i s cont r ol l ed by chemi cal
i nt er act i ons and mass t r anspor t of t he gaseous const i t uent s wi t hi n t he por es
of t he graphi t e. Low concent r at i ons of wat er vapor , up to 50 Pa ( 500 patm)
wat er vapor and hi gh concent r at i ons, up t o 1000 Pa (10 at m) ar e di scussed.
7- 1
Controversy sti l l exi sts over the mechanisms i nvol ved i n the reacti on of
water vapor wi th graphi te, but there i s general agreement that the chemical
reacti ons can be represented by the Langmuir-Hinshelwood equati on:
R =
+ pn H2 + K3PH*0
pH20 and are
K2, and K where K 1,
parti al pressures of water vapor and hydrogen, respecti vel y, F corrects the
are rate constants, n i s a constant,
H2
3
b
- rate f or the ef f ect of burnoff, and F corrects the rate f or the ef f ect of
catal yti c reacti ons due to f i ssi on product i mpuri ti es i ntroduced i nto the
graphi te by i rradi ati on.
quanti f i ed i n H-451 graphi te; theref ore, catal yti c ef f ects cannot be consi dered.
C
The ef f ects of catal yti c i mpuri ti es have not been
The oxi dati on of graphi te by water vapor consi sts of three di sti nct
processes* (Refs. 7-5, 7- 6, 7-7): ( 1) sorpti on of water mol ecul es on acti ve
carbon si tes, ( 2) chemical reacti on of the sorbed water to form H and CO,
and ( 3) i nhi bi ti on of water sorpti on by competi ti ve sorpti on of H mol ecul es.
Process (1) can be expressed by
2
2
where C
rate constants or the forward and reverse reacti ons. Following process 7-2,
sorbed water reacts wi th the sol i d phase to form carbon monoxide and
hydrogen as expressed by
and C(H20) denote f ree and occupi ed si tes and i and j are reacti on

J 3
C(H20) -f CO +H2 +aCf
*
Transport consi derati ons are negl ected i n thi s treatment.
7- 2
(7-3)
n
where a i s an i nteger havi ng val ues from 0 to 2. I f a > 1 (observed i n the
earl i er stages of oxi dati on), the number of reacti on si tes i ncreases as the
reacti on proceeds, l eadi ng to i ncreased reacti on rates. I f a < 1 (observed
onl y duri ng the f i nal stages of the oxi dati on process), the graphi te becomes
less reacti ve as the reacti on proceeds. Thus, the reacti on rate i s af f ected
by burnoff (i .e., the extent of oxi dati on).
Hydrogen mol ecul es compete wi th water vapor mol ecul es f or the avai l abl e
si tes (Refs. 7- 5, 7-6). Thus, i ncl uded i n the denominator of Eq. 7-1 i s a
t er m which ref l ects the rates of adsorpti on of hydrogen on graphi te (process
7- 3) as expressed by
2
i
J 2
These three processes form the basi s f or the Langmuir-Hinshelwood equati on:
I >
j , +j 3'~20
i1
rate =
i
1 +- 2 n +
j 2 ' H ~
j , +j 3 ' ~ ~ 0
(7-5)
I f j ,, the rate of evaporati on of wat er mol ecul es from the surface, i s negl i -
K1 = i K = i /j and K = i ,/j 3. gi bl e,
1' 2 2 2' 3
7.1.2. Experi mental Procedure and Samding.
I nstantaneous reacti on rates are measured by specimen wei ght-l oss deter-
mi nati ons usi ng automati c recordi ng mi crobal ances (Ref. 7-1).
Specimens were taken from near the center of a l og of preproducti on
H-451 graphi te. The densi ty of the specimens ranged from 1.69 to 1.70 Mg/m .
The total metal l i c i mpuri ty content of the graphi te was l ess than 200 ppm
and i ron ranged from < 1 to 6 ppm.
3
7-3
K2, and K are obtai ned w
1' 3
Values of the constant n and rate constants K
from the sl opes of i sothermal pl ots of Llic reacti on rate data deri ved from
Eq . 7-1. Because al l three rate constants i ncrease wi th burnoff, val ues of
the constants were corrected to a constant burnoff of 1%.
7.1.3. Determi nati on of Reacti on Rate Constants
__
Values were determi ned f or reacti on rate constants: (1) burnoff f actor
Fb, ( 2) hydrogen exponent n, and (3) K 1, K 2, and K3.
these constants from experi mental data are gi ven i n Refs. 7-1 and 7-2.
Recommended val ues are l i sted i n Tabl e 7-1.
The determi nati ons of
7.1.3.1.
of rel ati ve reacti on rate versus percent burnoff, where the rate data are
normal i zed to uni ty at 1% burnof f (Ref. 7-1).
Burnoff Factor Fb. The burnoff f actor Fb i s determined from pl ots
TABLE 7-1
EXPERIMENTALLY DETERMINED LANGMUIR-H N HELWOOD
CONSTANTS FOR H-451 GRAPHITE by
Constant
-1 -1
K sec Pa
1
-0.75
K, Pa
L
-1
K3 Pa
Hydrogen
exponent n
Parti al Pressure Water (Pa)
Low $300
21 8 exp (-253500/RT)
1940 exp(-131900/RT)
1.02 exp(-47030/RT)
0.75
(a)Langmuir Hinshelwood equati on:
- 1
K1 'H,O
High 2 300 s 3300
0.11 exp(-195400/RT)
8.2 x exp(119700/RT)
1.3 x lo-' exp(131400/RT)
0.75
L
rate (sec ') =
0.75
+ K3PH,0
1 + K P
2 H,
L L
7-4
The i ncrease i n reacti on rate wi th burnoff is more rapi d at lower tempera-
tures. For example, at 5% burnoff, F i s 4 , 2.6, and 2.5 f or 1093, 1173,
b
and 1253 K , (820, 900, and 980C) respecti vel y.
I n the reactor, because of hi gh helium pressures, burnoff i s l argel y
surf ace ori ented, and the F t er m i s l i kel y to be qui te di f f erent from that
found i n these l aboratory experi ments.
b
7.1.3.2. Hydrogen Exponent n. The determi ned val ue of n i s 0.695 f: 0.18
(Ref. 7-l ), and thi s val ue is i n accord wi th n = 0.75 currentl y used i n the
OXIDE-3 code (Ref. 7-3).
7.1.3.3.
from the sl ope of the pl ot of 1/ R versus l/PH o, where R i s the rate of
reacti on and P i s the parti al pressure of water. I t i s essenti al that
the parti al pressure of hydrogen (P
H,
Rate Constants Kl LK2, and K3. The rate constant K, i s deri ved
2
H2
) be negl i gi bl e when compared wi th
L
i n order to obtai n a val i d val ue f or K Therefore, was ei ther ex-
'H20 1'
cl uded or hel d near zero duri ng the experi ments.
2
deri ved from experi ments carri ed out under these condi ti ons are reported i n
Ref. 7-2 f or three temperatures [1093, 1173, and 1253 K (820, 900, and
980C)].
disk-shaped sampl es 31.8 mm i n di ameter by 1.57 mm thi ck. Previ ous work
(Ref. 7-1) showed samples of these dimensions to exhi bi t minimal mass trans-
port control of the reacti ons.
Pl ots of 1/ R versus l /PH
The pl ots i n Ref. 7-2 summarize the data on reacti on rates usi ng
A l east-squares f i t (POLFIT) was used to generate the stati sti cal data
requi red to cal cul ate the vari ances of sl ope and i ntercept. An apparent
acti vati on energy was cal cul ated usi ng POLFIT wi th each data poi nt wei ghted
by i ts vari ance usi ng the methods gi ven previ ousl y i n Ref. 7-1.
The rate constant K is deri ved from the sl ope of a pl ot of 1/ R versus
2
theref ore, K can be determi ned usi ng
2
. The sl ope i s equal to K /K P
2 1 H20;
known val ues of K and n. The val ue of n (see above) was determi ned to be
1
7 -5
0.695 ? 0.18. A si mi l ar val ue f or n was used f or deri vi ng the constants
used herei n. Another assumpti on used i n determi ni ng K2 by thi s method i s
that errors associ ated wi th K are negl i gi bl e. As a precauti on, propaga-
ti onal error theory was employed to examine the contri buti ons of errors i n
K to the vari ance of K
1
2' 1
The experi mental data used to obtai n the requi red sl opes are gi ven i n
Ref. 7-2.
the 50-Pa water vapor i sobar.
exponenti al f actor were esti mated from the Arrheni us rel ati on (Ref. 7-2).
A composite of data from several experi ments was used to devel op
The apparent acti vati on energy and pre-
Establ i shment of equi l i bri um f or the competi ti ve reacti on
i s sl ow, parti cul arl y at low temperatures, and, consequentl y, data at
temperatures below 1123 K (85OoC> are l i mi ted. When addi ti onal data are
col l ected, val ues of K2 can be determi ned at temperatures of i nterest down
to about 1000 K (727OC).
The i ntercept val ues from pl ots of 1/ R versus 1/ P = 0 wer e used to
H2
determi ne K By rearrangi ng the Langmuir-Hinshelwood equati on, the i nter-
cept val ue of the above rel ati on can be equated to K /K However, K i s
al so dependent on the errors associ ated wi th K
f or cal cul ati ng K
3'
1 3' 3
The expressi on recommended
1'
over the parti al pressures examined i s gi ven i n Ref. 7-2.
3
7.1.4. ADvl i cati on of Rate Constants
A pl ot of l og rate versus l og P which compares both sets of deri ved
H2
constants f or H-451, al ong wi th the constants presentl y used i n the OXI DE
code, i s shown i n Fi g. 7-1. The OXI DE code constants were deri ved from a
composite of data from other graphi tes (Ref. 7-l) , pri mari l y measured at
low water concentrati ons; theref ore, the OXI DE code constants cl osel y match
the ti-451 constants deri ved herei n f or P l ess than 300 Pa. An addi ti onal
"2O
7-6
I
"' c
v
I
v
I I 1 1
I I 1 I 1 I 1 I I I I ~r
T =1173 K (900OC)
pH2 =51 Pa
/'
/'
/-
I I I I t I I 1 1
I I 1 I t
-
10.000 100,000 100 1000
10
P H ~ O (Pa)
Fi g. 7-1. Comparison of rate constants as a functi on
of P (from Ref. 7-2)
H2
problem wi th the OXI DE code lias been i ts predi cti ons of a near-zero-order
rel ati on at parti al pressures of water that are too l ow (see Fi g. 7-1).
use of H-451 constants deri ved f or hi gh water vapor w i l l improve the rel i a-
bi l i ty of the OXI DE code.
trati ons i n the range of 1 to 1000 kPa are possi bl e, the hi gh-water-l evel
H-451 rate constants shoul d be used. For normal steady-state reactor opera-
ti on, where water concentrati ons i n the range 10 to 1000 Pa are expected,
the low-water-level H-451 constants shoul d be used.
The
For acci dent condi ti ons, where moi sture concen-
7.2. EFFECT OF STEAM OXl DATI ON ON TENSILE STRENGTH AND ELASTIC MODULUS
The f uel element bl ocks are subj ect to mechanical stresses i ncl udi ng
compressi ve, due to the wei ght of the core components, and tensi l e, due to
i rradi ati on-i nduced strai ns and thermal gradi ent ef f ects.
bl ocks may have to wi thstand addi ti onal stresses resul ti ng f r om s ei s mi c
events. The f uel el ement bl ocks are requi red to wi thstand these i n-servi ce
stresses and retai n thei r structural i ntegri ty. Thus, a knowledge of the
ef f ect of oxi dati on on thc strength and el asti c modulus is requi red.
The f uel el ement
7.2.1. Experi mental Procedure and Sampling
The experi mental work (Ref. 7-8) consi sted of oxi di zi ng l arge numbers
of small test specimens uni forml y and i sothermal l y at 1073 and 1273 K (800'
and 1000C) i n steam-helium mi xtures, and subsequentl y measuring the strength
and el asti c modulus of the oxi di zed specimens. The strength and el asti c
modulus val ues of the oxi di zed specimens were compared wi th val ues of non-
oxi di zed control specimens, taken from the same popul ati on of specimens
used f or oxi dati on, to determi ne changes due to oxi dati on burnof f .
I n an ef f ort to obtai n data on material of hi ghest and l owest strength,
specimens were sel ected from quarter-l ength center (QLC) and quarter-l ength
edge (QLE) posi ti ons of GA l og 6 3 8 4 - 3 4 . Axial and radi al specimens were
sel ected iis i ndi cated i n Appendix A, Fi gs. A-14 through A-17.
7- 8
Groups o f sampl es were randomized and al l ocated for oxi dati on accordi ng
to Appendix B, Tabl e B-19.
After oxi dati on, approxi matel y 0.6 mm was removed from each end of each
oxi di zed specimen and each specimen cut i n hal f to provi de two specimens
6.34 mm i n di ameter by approxi matel y 2.3 mm i n l ength.
Oxi dati on specimens were 634 mm i n l ength.
The apparatus used f or the oxi dati on measurements i s descri bed i n
Ref 7-8.
taneousl y i n each experi ment.
hydrogen, and the bal ance hel i um was used f or oxi di zi ng the specimens.
Several of the cyl i ndri cal graphi te specimens were oxi di zed simul-
A gas mi xture composed of 3% water vapor, 5%
To determi ne the extent of oxi dati on, the oxi dati on process was i nter-
rupted peri odi cal l y and the sampl es were cool ed and weighed to 20.1 mg. The
percent burnoff was cal cul ated from changes i n specimen wei ght.
I t was anti ci pated that use of smal l -di ameter sampl es i n a hydrogen-
ri ch gas mi xture would ensure rel ati vel y uni form oxi dati on throughout the
bul k of the sampl es.
determi ni ng radi al densi ty prof i l es on a number of nonoxi di zed and oxi di zed
Uni formi ty of oxi dati on burnoff was confirmed by
specimens. Techniques f or measuring tensi l e strength and el asti c modulus
are reported i n Ref. 7-9.
7.2.2. Experi mental Resul ts
Complete data sets of ul ti mate tensi l e strength, el asti c modulus, and
strai n at f racture are tabul ated i n Ref. 7-8.
7.2.2.1. Oxidation-I nduced Bulk Densi ty Prof i l es. Bulk densi ty prof i l es
for nonoxi di zed control specimens of H-451 and f or three oxi di zed specimens
arc givcw i n K c T . 7-8. There is l arge scatter i n the data, which i s due to
cbxpcrinicwtal d i f f i cul ties and the heterogeneous nature of the graphi te.
T l i c oxi d;i ti on prof i l es arc uniform for al l specimens oxi di zed at 1073 K
or 1273 K (800" or 1000C). I t was anti ci pated that some pref erenti al oxi -
dati on on thc outer surf ace of the specimens would occur at 1273 K (1000C);
7-9
that i s, the f i nal densi ty prof i l e al ong the radi us af ter oxi dati on shoul d
Q
i ncrease from the outer edge toward the center. In most cases, oxi dati on
at 1273 K (lOOOC) produced uniform prof i l es. I t i s concluded from the bul k
densi ty prof i l e data that al l UTS specimens were oxi di zed uni forml y across
the radi us.
7.2.2.2. U l t i mat e Tensi l e Strength, El asti c Modulus, and Strai n at Fracture.
The UTS and el asti c modulus val ues f or nonoxi di zed control material were
hi ghest i n the axi al di recti on and i ncreased from the center to the edge of
the l og. The ul ti mate tensi l e strengths and el asti c modulus were i n agree-
ment wi th other data obtai ned on the same l og and other l ogs of H-451
graphi te (Ref. 7-9).
Stati sti cal anal yses were performed on the data to (1) determi ne
w h e t h e r t he di s t r i but i on of UTS w a s Gaussian ( us i ng the chi-square analysis)
(Refs. 7-10, 7-11), (2) compare popul ati on mean val ues of strength and
el asti c modulus f or control and oxi di zed specimens [usi ng a comparison of
popul ati on means (CPM) test] (Ref. 7-12), and ( 3) determi ne the maximum,
minimum, and most probabl e (mean) rates of property change wi th burnoff at
95% confi dence (usi ng the CONFTD computer code, deri ved from a techni que
gi ven i n Ref. 7-12).
The UTS data fol l owed a Gaussian di stri buti on. Confi rmati on of a
Gaussian di stri buti on i s i mportant si nce both the CPM test and the CONFID
computer code assume Gaussi an di stri buti ons,
The resul ts of the CPM and CONFI D anal yses are gi ven i n Tabl es 7-2 and
7-3, respecti vel y. The rates of changes i n UTS and E from the CONFID cal cu-
l ati ons arc presented graphi cal l y in Ref. 7-8, where the most probabl e rate
changes arc shown as l i near regressi on l i nes. A comparison of nonoxidized
and oxi di zed UTS val ues showed that strength decreased wi th oxi dati on. The
popul ati on means of the control and oxi di zed specimens were compared (see
Tabl e 7-2, column 7). No si gni f i cant reducti on i n UTS or modulus ( at 95%
confi dence) was observed i n axi al speci mens oxi di zed up to 2% and 1% burn-
of f , respecti vel y.
7-10
L
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1

TABLE 7-3
REDUCTI ON I N ULTI MATE TENSI L E STRENGTH AND EL ASTI C MODULUS
Burnof f
Temp 9
K ("C)
CA
CA
CA
EA
CR
ER
CR
ER
X Reduction/l% Burnoff
Burnof f Maximum Mean Minimum
Range (2.3% (Most (2.3%
% Probabi l i ty) Probabl e) Probabi l i ty)
CA
CA
CA
EA
ER
,
0.0
0 .o
1.70
3.74
4.32
3.23
3.18
3.72
1073 ( 800)
1273 (1000)
1273 (1000)
1273 (1000)
1073 (800)
1073 (800)
1273 (1000)
1273 (1000)
1073 (800)
1273 (1000)
1273 (1000)
1273 (1000)
1273 (1000)
0- 2
0-2
0-8
0-6
0-10
0-1 4
0-20
0-8
El asti c
0- 2
0-2
0-8
0-5
0-6
(a) CA: center axi al speci mens.
EA: edge axial speci mens.
CR: center radi al speci mens.
11.17
7.32
3.85
6.48
6.06
5.14
3.92
5.93
Modul us
14.04
11.56
4.88
9.53
9.31
5.60
1.73
2.82
5.14
5.32
4.60
3.59
4.79
10.46 1 0.01
3.71
3.26
6.10
7.83
0.0
1.45
1 .96
6.11
n
ER: edge radi al speci mens.
7-1 2
The ef f ect of oxi dati on on UTS f or axi al edge and center specimens
oxi di zed at 1073 K (800C) is shown i n Fi g. 7-2. The data i n Fi g. 7-2
i ndi cate no decrease i n strength occurred i n the center specimens up to 2%
burnoff, whereas a sl i ght decrease was observed i n the edge specimens.
The
UTS reducti on rates f or oxi dati on at 1273 K (1000C) are shown i n Fi g. 7-3.
Again, the edge specimens l ost strength at a hi gher rate than the center
specimens.
shown i n Fi g. 7-4.
2% at ei ther 1073 or 1273 K (800" or 1000C).
The combined data f or axi al center samples at low burnoff are
No strength reducti on was observed f or burnoffs up to
The UTS data f or radi al edge and center specimens are presented i n
Fi gs. 7-5 and 7-6 f or oxi dati on at 1073 and 1273 K (800' and 1000C),
respecti vel y. The radi al specimens l ost strength at a f aster rate than
axi al specimens, and i n both cases edge specimens l ost strength at a f aster
rate than center specimens.
The ef f ect of oxi dati on on el asti c modulus of axi al center specimens
at 1073 and 1273 K (800" and 1000C) i s gi ven i n Fi g. 7-7. No ef f ect of
burnoff up to 12 was observed, but above 12 the reducti on of the el asti c
modulus was si gni f i cant. Changes i n modulus of axi al center and edge
specimens may be compared i n Fi g. 7-8.
i s reduced at a hi gher rate than that of center specimens. Fi gure 7-9 i s a
pl ot of el asti c modulus versus burnoff f or radi al specimens oxi di zed at
1273 K (100O'C).
The modulus of the edge specimens
The trends f or UTS and el asti c modulus are summarized i n Tabl e 7-3 by
comparing the rel ati ve reducti on i n each property at 1% burnoff.
i n Tabl e 7-3 were obtai ned from CONFID, which can be used to cal cul ate, at
95% confi dence, the most probabl e (50% probabi l i ty) or mean decrease i n
property and the maximum and minimum (2.3% probabi l i ty) decrease i n property.
Reducti ons i n strength and el asti c modulus were greater when the specimens
were oxi di zed at 1073 K (800C) compared to 1273 K (lOOOC), and changes
were greater f or edge specimens than f or center specimens.
wa s parti cul arl y si gni f i cant i n modulus data where the average decrease i n
edge specimens at 1273 K (1000C) was twice that of center specimens.
The resul ts
Thi s phenomenon
7-13
0
0
Fig. 7-2.
Tensile strength versus burnoff for H-451 graphite
(log 6484- 34, quarter-length axial edge and center
specimens) oxidized at 1073 K (8OOOC)
7-3 4
20 68
130001
11.24
(25001
-
- -
z
0"
I
I- 13.79
2 (2000)
I
I
W
W
I-
v)
W
v)
z
W
!-
2
10.34
( 1500)
6.89
(1000)
\ 0
1 1
10 20
BUANOFF (96)
Fi g. 7-3. Tensi l e strength versus burnoff f or H-451 graphi te
(l og 6484- 34, quarter-l ength axi al specimens)
oxi di zed at 1273 K (lOOOC)
7-35
17.93
(26001
f
16.55
(24001
0
0 0
0 0 0
0
15.17
(22001
13.79
(2000)
i
2
I
&
11.03
(16001
z
w
a
w 9.65
z
(1400)
z
u1
I-
( 1 200)
a' 27 t
I
(1000)
6' 89 I
I
U
0
0
0 OXIDIZED AT 1073 K (8OOoC)
0 OXIDIZED AT 1273 K (looOC)
A NONOXIDIZED CONTROLS
0
0 0
0
Q
0
' e
I - 1 . - .-_I --- . L - - l - L
I 1 I
0 4 O G 0 8 10 1 2 1 4 1 6 1.8
0 2
EURNOFF l"/)
Fig. 7 - 4 .
Tensile strength versus burnoff for H-451 graphi te
( l og 6484- 34, quarter-length axial center
specimens)
7-36
20.68
(3000
17.24
(25001
- 13.79
- (2000)
2
E
a
I
I-
o
z
W
I
a
d
L;;
E 10.34
W
v)
z
( 1500)
6.89
( 1000)
3.45
5 10 15 20
(500)
BURNOFF (%)
Fig. 7-5. Tensile strength versus burnoff for H-451 graphite
(log 6484-34, quarter-length radial specimens)
oxidized at 1073 K (800OC)
7-1 7
a
0
1.38
I
I
"
BUR N O F F W')
Fi g. 7- 6.
Tensi l e strength versus burnoff f or H-451 graphi te
(l og 6484- 34, quarter-l ength radi al specimens)
oxi di zed at 1273 K (l OOOC)
7-3 8
c
U
I
11
(1.6)
-
W-
I
E! 9.7
'I (1.4)
2
2
* 8.3
3 (1.2)
sc
a
Y
3
0
0
E
I-
0 6.9
* (1.0)
4
w
5.5
(0.8)
4.1
00
0 0
0 OXIDIZED AT 1073 K (8OOOC)
A NONOXIDIZED CONTROLS
OXIDIZED AT 1273 K (l OOOC)
00
0 0 0
1273 K
(1 ooooc)
1 -
0
8
0
I I I I I I 1
(0.6)
1 2 3 4
5 6 7 a
BURNOFF (%)
Fig. 7-7. El asti c modulus versus burnoff f or H-451 graphi te
(l og 6484- 34, quarter-l ength axi al center
specimens)
0 EDGE OF L OG
@ CENTER OF LOG
11.0
(1.6)
9.7
(1.4)
8.3
( 1 .a
6.9
(1 .O)
5.5
(0.8)
I
1 1
1 1 1 1 1
1 1 1 1
4 5 6 7 a 9
4.1 I
(0.6) 1 2 3
BURNOFF (%)
Fig. 7- 8. Elastic modulus versus burnoff for H-451 graphite (log 6484- 34,
quarter-length axial specimens) oxidized at 1273 K (lOOOC)
0

7
-
2

1

n
Changes i n strai n at f racture were measured on nonoxi di zed control
specimens and on specimens oxi di zed to bur nof f s up to 12X.
anoni nl ous , showing no changes i n axi al cc%ntcr spcbcimens at 4.3% burnofl ,
about 50X reducl i on i n radi al center specimens at 2.82 to 9.3X burnoffs,
and about 40% reducti on i n radi al edge specimens at 5.5% to 12% burnoffs.
No f i r m concl usi ons can be drawn from these data.
The data were
7.2.2.3. Concl usi ons. The tensi l e strength of H-451 graphi te decreased by
r
an average of 3.6% i n center axi al specimens when oxi di zed to burnoffs up to
2.0% at ei ther 1073 K or 1273 K (800" or lOOO"C), and no si gni f i cant reduc-
ti on i n el asti c modulus i n these same specimens was observed when oxi di zed
to burnoffs of up to 2.0% at 1273 K (1000C).
tensi l e strength and el asti c modulus f or center axi al specimens was greater
at 1073 K (800OC) than at 1273 K (1000C) and, i n general , the reducti on
was hi gher i n radi al specimens than i n axi al speci mens.
The rate of reducti on of
I n general , the reducti on rate of el asti c modulus wi th burnoff was
greater than that of tensi l e strength.
strength and el asti c modulus f or axi al specimens oxi di zed at 1273 K (lOOOC)
The rate of reducti on of tensi l e
was greater at the edge than at the center of a l og.
REFERENCES
7-1.
7-2.
7-3.
7-4.
"Quarterl y Progress Report f or the Peri od Ending August 31, 1976,
HTGR Fuel s and Core Development Program," ERDA Report GA-A14046,
General Atomic Company, September 29, 1976.
"Quarterl y Progress Report f or the Peri od Ending May 31, 1977, HTGR
Fuel s and Core Development Program," ERDA Report GA-A74418, General
Atomic Company, J une 1977.
Peroomian, M. B., A. W. Barsell, and J . C. Saeger, "OXI DE-3: A
Computer Code f or Anal ysi s of HTGR Steam or A i r I ngress Acci dents,"
General Atomic Report GA-A12493, J anuary 15, 1972.
Gi berson, R. C., and G. L. Tingey, "Reacti ons of Gaseous I mpuri ti es
i n a High Temperature Gas Cooled Reactor," USAEC Report BNWL-974,
1968.
7-22
u 7-5.
7-6.
7-7.
7-8.
7-9.
J ohnstone, H. F., C. Y . IChen, and D. S. Scott, "K i neti cs of the
Steam Carbon Reacti on i n Porous Graphi te Tubes," I nd. Eng. Chem. 44,
1568 (1952).
Walker, P. L., J r., F. Riisinko, J r., and L. G. Austi n, "Gas Reacti ons
of Carbon," Advanced Catal ysi s 11, 149 (1959).
Ergun, S., and M. Menken!, "Reacti ons of Carbon wi th C02 and Steam,"
i n Chemi stry and Physi cs of Carbons, v. 1, P. L. Walker, J r. (ed.),
Marcel Dekker, New York, 1965, p. 229.
Vel asquez, C., et al ., "The Ef f ect of Steam Oxi dati on on Strength
and El asti c Modulus of Graphi te H-451," DOE Report GA-A14657, General
Atomic Company, December 1977.
J ohnson, W. R., and G. B. Engl e, "Properti es of Uni rradi ated Fuel
El ement Graphi tes H-451 and TS-1240," ERDA Report GA-A13752,
General Atomic Company, J anuary 31, 1976.
7-10. Bevi ngton, P. R., Data Reducti on and Error Anal ysi s f or the Physi cal
Sci ences, McGraw- Hi l l , New York, 1969, pp. 84 and 314.
7-11. J ohnson, N. L., and F. C. Leone, Stati sti cs and Experi mental Desi gn,
v. 1, J ohn Wiley and Sons, New York, 1964, p. 224.
7-12. Bevi ngton, P. R., op. ci t., p. 104.
-
7-23
8. ACKNOWLEDGMENTS
The author gratfully acknowledges the contributions of R. J. Price,
L. A. Beavan, and R. D. Burnette in helping to summarize the data and
in commenting on the manuscript.
c
8- 1
APPENDIX A
SAMPLING DIAGRAMS
A- 3
EDE
432 ....,
DISCARD
TOP 25.4 mr
I
BE///I 152mm
I\\ BE
END /I 152mm
I\ SLAB 1 I
n
L' - I t
/ I 152,mm
SLAB 4 '+
SLAB 5
D ISCAR fl
Fig. A- 1. Sampling diagram of H-451 for within-log property
measurements: sl abs and secti ons
A- 3
A
-
4

.
.

l
-
l

=
I
a
)

6

h

4
J

L
c

3

b

a

0

$
4

a

.
-
I

.

.
.

4
-
5

h

u

L
l

h
,

a

0

k

a

M

TO RADIAL
(RADIAL DIRECTION) I
I
I
I DIRECTION
1. I
3 (AXIAL) 3 (AXIAL)
2 (RADIAL)
J
1 (CHORD)
J 1 .
1 (RADIAL) I
I PERPENDICULAR
I TO RADIAL
I DIRECTION
I
I
EE POSITION
- 2 (RADIAL)
MLE POSITION
- 2 (RADIAL)
Fi g. A- 4.
Ori entati on of orthogonal axes for def i ni ti on of
Poi sson's rati o data i n Table B-4
A-6
SLAB 2
FATIGUE SPEC I M ENS
SLAB 3
t
' SLAB4
t
SLAB 5
SLAB 6
ALL DIMENSIONS I N mm
25.4
Fig. A-5. Locations of sl abs (shaded) f or s t at i s t i c al strength t est i ng
H-451 graphite ((log 5651-90)
A- 7
rn
RADIAL SPECIMENS
RADIAL SPECIMENS
216 r nr n-
Fig. A-6.
Coring plan for center zone of A and B sections of slabs
(see Fi g. A-5)
A-a
b-4
25.4 mm
Fig. A- 7. Coring pl an f or edge zone of A and B sections of sl abs (see Fi g. A-5)
SLAB E
25 mm THICK
THIS CORE HAS
BEEN ENLARGED
TO SHOW DETAI L
16 mm DIAMETER ON ROO c
356 mm DEEP
ROD C
-432 mm DIAMETER-
: ORE TAKEN
:OR GLCC
r ENSl LE TEST
iPE C IM E N
mm
--CORE TAKEN
FOR GA TENSILE
TEST SPECIMENS
Fi g. A-8.
Sampling diagram of H-451 logs for t ens i l e strength
A-10
n
u

0

0

(
r

z

w

0

w

v
)

E

n

0

0

(
1

E

0
0

1

E

Y

I

I-
z

0

a
,

a

r
n

d

(
d

.
r
l

3

.
.

n

m

a
,

a
l

r
n

a
,

k

0

c
)

2

(
d

r
n

M

0

r
l

r
n

U

F

&

W

0

E

(
d

k

M

m

0

0

W
J

m
P
)

a
)

m

U

r
l

a

E

(
d

c
n

M

.
I
+

F
r
r

0

N

R

A
-
1

2

n

RADIAL
SPECIMENS
RADIAL
SPECIMENS
Fi g. A- 12. Sampl i ng di agram f or i rradi ati on specimens: center zone, from sl ab 3
(see Fi g. A-1)
.(> '
.

A
-
1
5

n
/
933.6 rnm
196.9 mrn
%
/
/
\
7
\
7
165.1 mrn \
Y
<--;a
/
- 0x1 OAT1 0 N
SPECIMENS
POSITION
QUARTE R-LEN GTH
Fig. A-14. Sampling plan of graphite log showing slab
designated for oxidation tests
U

7

h

M

d

F
r
c

w

P

f
d

r
l

m

(
d

1
c
c

0

7.9-mm COR E
63.5 mm DEEP
7.9-mm COR E
63.5 mm DEEP
196.9 mm
Fig. A-16. Sampling diagram of H-451 graphite: center
sect i on of sl ab from Fi g. A-15
A-1 8
n
E

E

3

P

2

I

A
-
1

9

APPENDIX B
EXPERIMENTAL RESULTS
B- 3
h

r
p

7

7
.

0

.
j

I

U

m

U

U
J

c

U

U

m

.
3

\
o

2

E

J

J

s

..4

B
-

3

TABLE E-2
ULTINATE TENSILE STRENGTH: H-451. LOT 426
MLE
14.04 (2.5) (191
13.69 (2.9) [l a]
14.13 (1.6) [20]
13.75 (1.7) [ 20]
13.91 (2.2) [77]
Log No.
EC
15.87 (2.4) 1201
12.31 (3.0) [201
15.38 (0.8) [l a]
12.33 ( 2. 0) 1201
13.94 (2.6) ( 781
GA
td
.b
I 6484-33
6484-34
6484-40
6484-41
Mean,
lot 426
-
GLCC
92
198
155
184
-
-
~ ~~~~ - ~~
Mean Strength (Wa)(Standard Devi ati on, MPa) [No. of Repl i cates]
Axi al 1 Radi al
MLC
14.54 (1.5) [I 91
14.18 (0.8) [20]
12.99 (1.6) [20]
12.93 (1.2) [20]
13.65 (1.6) 1791
ULE
20.16 (2.3) [151
19.42 (1.8) [20]
18.04 (1.1) [19]
18.66 (1.6) [19]
19.01 (1.9) [731
EC
18.44 (1.3) [ 20]
14.10 (0.9) [20]
16.67 (1.0) (201
11.86 (0.8) (201
15.26 (2.7) 1801
EE
20.14 (1.6) [I 91
18.62 (1.9) [201
16.83 (1.1) 1191
16.53 (1.4) (201
18.01 ( 2. 1) I 781
t
-
MLC
10.44 (1.5) [201
10.38 (2.1) 1181
11.72 (1.4) [201
10.44 (2.9) [ 20]
10.75 (7.1) [781
EE
17.47 (1.2) [20]
14.74 (2.4) [191
15.14 (1.0) (201
13.43 (1.9) 1191
15.22 (2.2) [78]
=c
EC
Log No.
EE MLC
l ot 426
MLC
8.13 (0. 21) [SI
8. 20 (0.14) [8]
7.86 (0.21) [8]
7.58 ( 0 . 2 4 ) [8]
7.93 ( 0. 28) [32]
TABLE B-3
ELASTIC MODULUS IN TENSION: H-451, LOT 426
Mean Modulus (GPa) (Standard Deviation, GPa) [No. of Replicates]
MLE
9.03 (0. 28) [81
9.03 (0.21) [81
8.67 (0.21) [8]
8.62 (0.21) [8]
8.82 ( 0. 28) [321
Axial I
8.41 (0.21) [81
8.13 (0.21) [81
8.55 (0.07) 181
7.31 (0.21) [81
8.13 (0.21) [321
9.03 (0.21) [a]
8.76 (0.55) [E]
8.96 (0.76) [a]
8.00 (0.48) [8]
8.69 (0.62) [32]
7.24 (0.41) [8]
7.72 (0.76) [81
7.31 (0.21) (81
7.17 (0.28) 181
7.38 (0.48) [32]
i . 7 9 (0.21) [E] 7.65 (0.21) [8]
7. 31 tO. - 8) [8] 7.58 ( 0. 28) [8]
7 . + 5 ( 0 . 2 1 ) [8] 7.51 ( 0 . 3 5 ) [81
6.81 (0.21) [E] 7.03 (0.35) 191
7.38 (0.i8) [321 7.45 (0.41)[33]
6.76 (0.21) [81
6.83 (0.34) [a]
7.03 ( 0. 14) (81
6.89 (0.14) [51
6.89 (0.28) 1291
Radial
MLE I EC I EE
Log No.
GA
5651-63
5651-63
5651-63
Mean
Mean
W 5651-63
a\
. I
5651-28
5651-63
Mean
5651-28
5651-63
Mean
Mean
565 1-63
-
LCC
!2
-
!2
!2
!2
8
!2
I8
22
22
-
Location
of
,pacirnen
i n Log
?ILC
XLC
X I C
MLC
MLC
MLC
MLE
MLE
EE
K recti on
f Appl i ed
Stress
Radi al
Radi al
Radi al
Axi al
Axi al
Axi al
Axi al
Axi al
Axi al
(a)Perpendi cul ar to radi al di recti on.
.Q -
Di recti on
Of
Transverse
Strai n
Axi al
Radi al
Axi al
Radi al
Axi al
Radi al
Axi al
Radi al
Radi al
Radi al
Radi al
Radi al
Radi al
Chord (a)
Radi al
Chord ( a)
Radi al
Chord (a)
Radi al
Chord (a)
TABLE 8-4
POISSON'S RATIO: H-451. LOT 266
Poi sson's Rati o (Standard Devi ati on) [No. of Measurements]
'13 = '23
0.120 (0.001) [31
0.096 (0.019) [l o]
0.112 (0. 002) (641
0.110 (0.009) [771
-
' 12 = ' 21
-
0.137 (0.001) [3]
0.104 (0.011) [l o]
0.107 (0.006) 1641
0.108 (0.008) [771
'31 * '32
1.125 (0.009) [61
1.130 (0.019) [2&1
1.125 (0.008) [481
1.127 (0.013) [i 81
"32
).I23 (0.009) [ I 21
0.121 (0.003) [641
0. 121 (0.005) [76]
0.110 (0.010) [40]
I^ .
0.113 (0.007) [ I 21
0.114 (0.006) 16L1
0.114 (0.006) [761
0.1 17 (0.006) [ 40]
TABLE B-5
FLEXURAL STRENGTH: H-451, LOT 426
17.1 ( 4 . 2 ) [ZO]
17.7 (1.4) [ZO]
17.4 (3.1) [40]
Log No.
22.2 (1.2) [20] 21.7 (1.7) I201 22.5 (1.0) [20]
21.1 (1.3) 1201 18.4 (1.1) [201 19.6 (1.7) (201
21.7 (1.4) [40] 20.0 (2.2) [A01 2 1 . 1 (2.0) [A01
6484-40 I 155
lot 426 I
Mean Strength (MPa)(Standard De\
Axial
ati on, Wa) [No. of Replicates]
Radial
TABLE B-6
ULTIMATE COMPRESSIVE STRENGTH AND ELASTIC MODULUS IN COMPRESSION: H-451, LOT 478
- v -
I
GA GLCC MLC MLE EC EE
I I
Loe No. I Axial
MLC MLE EC EE
I Radial
49.4
52.2
53.1
51.6
3.1
55.9
57.8
56.1
56.6
2.2
7194-49
7194-52
7194-87
a L ot mean
I
03
Standard deviation
58.9
58.9
60.5
59.4
1.9
7194-49
7194-52
7 1 9 4-87
Lot mean
Standard deviation
49.2
50.0
53.6
50.9
3.1
15
72
35
15
72
35
Ultimate Compressive St
50.3
51.8
53.7
51.9
2.7
Elastic
6.0
6.4
6.6
6.3
0.8
Modulu
6.8
6.7
7.3
6.9
0.5
xength (MPa)
55.2
58.3
62.9
58.8
5.0
52.4
48.3
48.2
49.6
2.7
in Compression (GPa)
6.2
6.0
6.9
6.4
0.7
6.9
6.8
7.7
7.1
0.8
5.2
4.7
5 .O
5.0
0.5
54.6
54.5
50.3
53.1
3.0
5.4
5.2
5.4
5.3
0.3
5.4 1 5.7
5.4 I 5.5
0.45
TABLE 8-7
T H E W EXPANSIVITY: H-451. LOT 426
Ec EE
4.00 (0. 18) 181 3.88 (0.09) [81
4.31 ( 0. 08) [E] 4.13 (0.12) [E]
3.90 (0.13) [E] 3.89 (0.09) [E]
4.07 (0.22) [24] 3.97 (0.15) 1241
I
Mean Thermal Expansi vi ty x l o6 K-l (" C-' ) [Standard Devi ati on x l o6 K-' ("C-')I [No. of Repl i cates]
ULC
4. 51 (0.29) [81
4.63 ( 0. 20) [8]
4.42 (0.18) [E]
4.52 (0.23) [241
Log No. I Axi al I
92
198
184
GA
4.08 (0.14) [El 3.86 (0.20) [8]
4.10 (0.10) [8] 3.92 (0.19) I81
3.92 (0.07) [81 3.90 (0.09) [81
4.03 (0.13) [24] 3.89 (0.16) [241
6484-33
W
I 6484-34
u)
6484-4 1
Mean,
l ot 426
4.65 (0.13) [8]
4.66 (0.25) [E]
4.50 (0.18) [8]
4.60 (0.20) [24]
I
mcc ULC I MLE
<.i o ( 0. 1~) [8] 4 . 7 0 ( 0. 21) [8]
4.55 ( 0 . 2 7 ) [ e] 4.59 (0.10) [ El
(1.43 (0.16) (81 4.59 (0. 18) [81
4.56 ( 0. 22) [241 4.63 (0. 17) (241
Radi al
MLE I EC I EE
.
GA GLCC
64 84-33 92
-34 198
-4 1 184
TABLE B-8
ANISOTROPY FACTOR: H-451, LOT 426
MLC MLE EC EE
1.12 1.18 1 .I2 1.17
T--
Log No.
a (radi al ) ( a)
Mean Anisotropy Factor,
( a ) ~ e a n of three logs.
B-10
% '
$73 K (200C) (a)
120 (27) [81
115 (6) 181
125 (14) [71
112 (7) [71
122 (21) [15]
114 (6) 1151
* c .
673 K (400C)(a:
92 (7) [81
88 (6) [81
92 (4) [71
88 (4) [71
92 (6) [151
88 (5) 11. 51
Log No.
Or i ent at i on
Axi al
Radi al
GA
Mean Tensi l e St r engt h
( +St andar d Devi at i on)
( ma)
18. 9 2 1. 8
13. 9 + 2. 3
6484- 34
6484- 34
6484- 4 1
64 84- 4 1
Mean,
Lot 426
W
I
GLCC
198
198
184
184
Or i ent at i on
Axi a1
Radi al
Axi al
Radi al
Axi al
Radi al
TABLE B- 9
THERMAL CONDUCTI VI TY: H- 451, LOT 426, MLC
Mean Ther mal Conduct i vi t y, W/ m*K
( St andar d Devi at i on, W/ m*K) [ Number of Repl i cat es]
295 K (22C) (a)
~~
136 (17) [81
129 (10) 181
147 (17) [71
139 (13) [71
141 (18) 151
134 (13) 1151
' ( a) Temperat ure of meas
TABLE B-10
MEAN TENSI LE STRENGTH OF UNI RRADI ATEDH- 451 GRAPHI TE
SPECI MENSUSED I N FATI GUE STUDY
1073 K ( 800"Cf a)
TABLE B-11
I RRADI ATI ON CONDI TI ONS AND MEAN TENSILE STRENGTH OF I RRADI ATED H-451 GRAPHITE
USED I N FATIGUE STUDY
(ALL SPECIMENS MLC LOCATION)
Ori entati on
I Axial
W
tQ
&a
Radi al
Axial
1 I I 1
Mean Tensi l e MeanTensi l eStrength
Fast Neutron Strength of Uni rradi ated
Fl uence N/m ) I rradi ati on Temperature (+-Standard Companions
Devi ati on) ( 2 StandardDevi ati on)
(E > 29 fJIHTGR K O C (ma) (Wa)
3 .O 1173 900 14.5 2 2.1 10.8 2 0.9
5.7 1223-1 263 950-990 22.4 ?r 2.6 11.5 t 1.7
20.2 2 1.9 10.8 t 0.9 8.5 1 1 73-1 243 900-970
. ,
TABLE B-12
SUMMARY OF IRRADIATION-INDUCED CHANGES IN THERMAL EXPANSIVITY OF H-451 GRAPHITE
IRRADIATED IN CAPSULES OG-1. OG- 2. AND OG-3
B-3 3
TABLE B-13
SUMMARY OF IRRADIATION-INDUCED CHANGES IN THERMAL EXPANSIVITY OF
H-429 GRAPHITE IRRADIATED IN CAPSULES OG-1, OG2, and 063
GA
Log No.
4 9 74-04A
Orientat ion
Axial
Radial
Mean
Irradiation
Temperature
K
1165
1180
1170
1435
1460
1480
1705
1675
1165
1145
1170
1435
1460
1480
1705
1675
O C
89 2
907
89 7
1162
1187
1207
1432
1402
__ .
892
872
89 7
1162
1187
1207
1432
1402
3.0
5.2
7.2
5.6
8.6
11.4
6.6
8.8
3 .O
5 - 6
7.2
5.6
8.6
11.4
6.6
8.8
Q
.
Average
Percent
Change in
CTE
295-773 K
(22-5000C)
-8
-4
-21
-1 3
-28
-4 1
-22
-30
+2
+1
-1 9
-9
-29
-39
-1 7
-27
GA
Log No.
5651 -73
m
I
U
cn
TABLE B-14
SUMMARY OF IRRADIATION-INDUCED CHANGES I N THERMAL EXPANSIVITY OF
TS-1240 GRAPHITE I RRADI ATED I N CAPSULES 06-2 AND 0 6 3
Ori entati on
Axial
Radi al
Locati on
i n Log
Midlength-
center
Midleng th-
edge
Midlengt h-
center
mdl ength-
edge
Mean
I rradi ati on
Temperature
K
895
1040
1195
1250
1380
1415
880
865
1080
1195
1200
1475
1500
8 80
O C
622
767
922
977
1107
1142
607
592
807
92 2
927
1202
1227
607
--
Fl uence
(E > 29 fJ I HTGR
(x ~ / m ~ j
1.2
1.7
2.5
4.9
2.9
5.9
2.3
1.2
1.7
2.5
4.9
2.9
5.9
2.3
Average
Percent
Change
i n CTE
295-773 K
(22C-5000C)
+7
+2
-1
-36
+1
-33
+6
-1
-4
-4
-20
-11
-4 7
+4
Lot
-25
Mean I rradi ati on Fl uence x 10
2
(N/m )
Temperature
GA Locati on
Log No. Ori entati on i n Log K O C (E > 29 fJ I HTGR
6484- 22 Axi al Midlength 1040 767 I 2. 4
center 1655 1382 2.9
Radi al Midlength 101 0 737 2.4
center 1655 1382 2.9
4B
Average
Percent
Change
i n CTE
395-773 K
(2Z0-5OO0C)
+3
-1 2
+7
-1 1
td
I
Q\
Y
.
875
890
900
1195
1205
1210
1625
1625
1620
t
c
2
602
617
627
922
932
937
1352
1352
1347
TABLE B-16
SUMMARY OF IRRADIATION-INDUCED CHANGES IN T H E W CONDUCTIVITY OF H-451 GRAPHITE IRRADIATED I N
CAPSULES OG-1, OG-2, AND 0 6 3
(ALL SPECIMENS FROM MLC OF PARENT LOG)
~~
GLCC
Lot No.
266
266
426
GA
Log No.
5651-28
565 1-28
64 84- 34
Orientation
Axial
Radial
Axial
Radia
Me an
Irradiation
Temperature
K OC
875
890
900
1195
1205
1210
1625
1625
1620
602
61 7
627
922
9 32
937
1352
1352
1347
--
925 652
1615 1342
1220 I 947
--
-25
Fluence x 10
2
(N/m
(E > 29 fJIHTGR
0
2.0
3.7
5.5
2.8
5.3
7.7
3.2
6.1
9 .o
0
2 .o
3.7
5.5
2.8
5.3
7.7
3.2
6.1
9.0
0
1.8
2.4
2.9
0
1.8
2.4
2.9
Mean Thermal Conductivity
(W/m.K) f Standard Deviation
At
293 K ( 2OoC)
145.2 2 1.3
34.7 2 1.4
30.1 2 0.9
29.6 2 1.4
48.8 2 1.8
41.3 2 8.4
43.6 2 6.8
79.8 f 4.2
80.9 2 4.0
68.9 2 9.2
123.0 2 7.1
32.0 2 1.9
27.8 2 3.1
25.9 2 0.8
42.9 f 3.3
34.2 f 4.3
31.2 f 5.1
83.5 5 7.2
65.7 f 8.2
56.2 2 2.8
136.0 f 17.2
34.0 f 3.0
60.8 4 5.1
82.4 f 1.1
128.9 2 10.0
29.6 2 4.1
58.9 2 3.1
72.4 f 1.3
At Irradiation
Temperature
--
33.3 f 2.7
32.5 f 4.3
31.5 2 4.4
40.0 2 1.7
39.8 f 3.0
34.1 2 5.9
41.1 2 1.2
40.7 f 0.6
34.5 2 3.8
--
33.3 2 2.7
29.5 f 3.2
28.0 f 4.7
36.1 2 2.8
29.5 2 2.0
30.7 2 6.1
39.3 f 3.4
36.4 2 2.0
33.1 f 4.4
--
32.0 f 6.6
39.0 2 6.7
32.5 f 6.3
29.8 f 6.7
35.4 f 6.4
31.9 f 6.3
--
TABLE B-17
SUMMARY OF I RRADI ATI ON-I NDUCED CHANGES I N THERMAL CONDUCTI VLTY OF TS-1240 GRAPHI TE
I RRADI ATED I N CAPSULES OG-2 AND O G 3
(ALL SPECI MENS FROM MLC OF PARENT LOG)
910
915
1220
1220
1620
1615
ucc
L ot No.
637
642
947
947
1347
1342
1
910
915
1220
1220
1620
1615
m
I
00
U
637
642
947
947
1347
1342
GA
Log No.
5151-73
5651-73
O r i en t at i o n
~~
A x i a1
R adi a1
Mean
I rradi ati on
T emper at ur e
K OC
-25
Fl uence x 10
0
1.7
3.5
2.5
4.9
2.9
5.8
0
1.7
3.5
2.5
4.9
2.9
5.8
Mean T her mal C o nduc t i v i t y
(W/m.K) 2 Standard D ev i at i o n
A t I r r ad i a t i on
293 K (22C) T empe ra t ur e
97.9 2 8.4
30.5 f 1.2
26.5 f 0.9
45.5 f 3.7
51.5 f 2.1
68.8 t 3.4
66.0 f 7.9
103.3 f 4.2
28.5 f 2.8
27.5 f 0.8
37.0 f 2.2
50.1 t 1.4
64.5 f 5.5
65.4 2 2.8
--
34.1 f 1.7
27.9 2 5.0
38.2 f 2.4
36.5 f 4.0
37.2 f 1.5
37.5 f 4.6
--
32.6 f 0.3
25.1 f 3.4
29.9 f 1.7
37.6 2 4.7
33.5 f 1.2
37.0 t 3.5
C '
(N/U12)
(E > 29 fJIHTcR
0
1. 8
2.4
2.9
I ',
At
293 K (22OC)
135. 1 f. 5.0
28.6 ?I 0. 8
50. 5 2 0. 8
64. 5 f. 4. 9
TABLE B-18
SUMMARY OF IRRADIATION-INDUCED CHANGES IN THERMAL CONDUCTIVITY OF SO81 8 GRAPHITE
IRRADIATED IN CAPSULE OG-3
(ALL SPECIMENS FROM MLC OF PARENT LOG)
4-B
4-B
AirCo
64 84-2 2
6484-22
925
1220
1615
Orientation
Axial
652
947
1342
Radial
Mean
Irradiation
Tem erature
-7F-p-
---I---
--
925 652
1615 1342
1220 1 947
I
*
c
I
Mean Thermal Conductivity
(W/m-K) f: Standard Deviation
-25 I
Fluence x 10
0
1.8
2.4
2.9
125.9 f. 5. 0
28.4 2 0. 8
43.7 f: 4. 2
65. 8 f: 2. 3
At Irradiation
Temperature
--
26.7 f. 4.6
36.7 2 4. 2
34. 3 2 4. 4
--
27.0 2 5. 0
32. 3 2 4. 3
33. 0 f. 4. 2
-
T emper atur e
K ("C)
573 ( 300)
-
w
I
h)
0
1673 (400)
TABLE B- 19
CALCULATED THERMAL CONDUCTI VI TY AT I RRADI ATI ON TEMPERATURE OF NEAR-I SOTROPI C GUPHI T E
I RRADI ATED BETWEEN 573 AND 873 K (300' AND 600C)
Fast Neutron Fluence,
( N/ m2 x
(E ' 29 fJ )HTGR
0. 9
1.8
2. 7
3. 6
4. 5
8.9
13. 4
0. 9
1.8
2. 7
3. 6
4. 5
8. 9
13. 4
T her mal C onduct i vi t y
(W/m-K)
R adi al
11. 7
9. 2
7. 9
7.1
6. 7
5. 9
5. 9
19. 7
14. 6
13. 0
11. 7
10. 9
9. 6
8.8
A x i al
13. 4
10. 5
9. 2
8. 4
7. 9
7. 1
6. 7
23. 0
17. 2
15. 1
13. 8
12. 6
11. 3
10. 5
Tempe]
K
773
873
. tur e
DC
500
600
-
Fast Neutron Fluence,
( N/ m2 x
(E ' 29 fJ )HTGR
0. 9
1. 8
2. 7
3. 6
4. 5
8. 9
13. 4
0. 9
1.8
2. 7
3. 6
4. 5
8. 9
13. 4
T her mal C onduct i vi t y
(W/m.K)
R adi al
~
28. 9
20. 9
18. 4
16. 7
15. 1
13. 0
11. 7
3 2 . 2
2L. 3
20. 5
18. 0
16. 7 -
15. 5
13. 8
A xi al
0. 080
0. 058
0. 052
0. 046
0. 042
15. 1
0. 033
37. 2
18 .O
23. 8
20. 9
19. 7
18. 0
16. 3
i
m
c

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t
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MINIMUM STRESS, (JMIN (MPa)
td
I
h)
w
MI NI MUM STRESS 'MIN
MEAN TENSI LE STRENGTH -s
Fig. B-2. Constant life fatigue diagram (Goodman diagram) for H-451 graphite: axial direction (from
Ref. 5-10)
W
(1
2
a
m -1
t a
.+ 0
5 -2
h) z
VJ
z
w
E
Q -3
-4
0 IRRADIATION TEMP 875 K - 975 K
0 IRRADIATION TEMP 1075 K - 1175 K
1 I I I I I I 1 I
Fig. B-3. Dimensional change in H-451 graphite: axial direction; irradiation temperatures 875 K to 975 K
and 1075 K to 1175 K (602' to 702OC and 802' to 902OC) (from Ref. 6-3)
s
z
-
a

N

W

z

c

-
4

0

z

n

7

c

r
n

z

c
)

m

r
n

=
a

6

-
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0

2

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1

3
,

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n

r
n

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H
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/
P

(
5
6
)

0

I

4

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b

w

0
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r
n
r
n

5
5

w
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m
u

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D

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a

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-
z

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w

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o
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0

.

2

v
)

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0

2

W

a

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2

-
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l
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a

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n

c

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I
-

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5

0

9

a

E

c

N

c
)

c

I

I

I

(
9
6
)

b
D
V

3
9
N
V
H
3

l
V
N
O
I
S
N
3
W
I
O

c

0

d

I

n

B
-
2
6

i c '
,
B
1625 K
- (1352'
0 IRRADIATION TEMP 1475 K - 1575 K
0 IRRADl ATl ON TEMP 1575 K - 1675 K
B
0
I I I I 1 I
I I I
1 2 3 4 5
NEUTRON FLUENCE (lo25 N/rn2) (E >29 f J)HTGR
Fig. B-6. Dimensional change in H-451 graphite: axial direction; irradiation temperatures 1475 K to
1575 K and 1575 K to 1675 K (1202O to 1302OC and 1302" to 1402OC) (from Ref. 6-3)
e
1525 K
(1 252OC)
0 IRRADIATION TEMP
0 IRRADIATION TEMP
875 K - 975 K
1475 K - 1575 K
I I I I I I I I I
1 8 9 10
Fig. B-7. Dimensional change in H-451 graphite: radial direction; irradiation temperatures 875 K to
975 K and 1475 K to 1575 K (602' to 702OC and 1202' to 1302OC) (from Ref. 6-3)
!
C '
,
c
1
1
0
.o
0- - 1
5
2
9
1
w
W
L
0 -2
0
2_
a
VI
2
w
-3
-4
0 IRRADIATION TEMP 975 K - 1075 K
0 IRRADIATION TEMP 1275 K - 1375 K
I I I I I I 1 I I
NEUTRON FLUENCE (1025 N/rn2) (E >29 f J)HTcR
Fig. B-8. Dimensional change in H-451 graphite: radial direction; irradiation temperatures 975 K to
1075 K and 1275 K to 1375 K (702' to 802OC and 1002' to 1102OC) (from Ref. 6-3)
I

I

I

I

?

I

I

I

I

I

I

1

I

I

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I

I

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V

0

N

U
I

m

Y

u
)

N

N

-

c

N

m

c

0

c

I

(
%
I

A
h
V

3
9
N
V
H
3

l
V
N
O
I
S
N
3
U
U
I
O

!?

m

m

b

a

a

I-

I

=
!

A

w

E

W
m

N

-

N

.

z

-
z

0

-

W

0

z

w

3

-
I

U

b
Z

0

a

!-

3

W

z

m

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c

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.
.
.

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I

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m
m

w
w

=
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e

I
I

Y
Y

0
0

I

c

0

c

N

0

I

(
%
)

r
l
D
V

3
9
N
V
H
3

l
V
N
O
I
S
N
3
H
l
l
O

0

U

M

U
N

a
0

k
m

d
-
-

a

-
0

r
l
c

c
d
c
d

d

a
v

C
d
O

k
N

0

m

a
0

&
U

.
.

c

d
o

u

B
-
3
1

n
0
- 1
-2
-3
s
-
w
U
z
I
u
a
-1 -4
a
0
z
z
v)
z
w
0
0
-- 1
-2
- 3
RADIAL
0 5 10 15 20 25 30 35 40
Fig. B-11. Dimensional changes in near-isotropic graphite irradiated at
633 K t o 7 7 3 K (360' to 5OOOC) (data from Refs. 6-4 and 6- 6)
..
u-32
0
- 1
-2
- -3
ae
-
w
c3
2
I
0
a
A -4
a
0
v , '
5
z
z
w
0
0
- 1
-2
-3
7
SOURCE I RRADl ATl ON
OF DATA TEMPERATURE
K
UKAEA I 773-823 500-550
UKAEA 823-873 550-600
DRAGON 1873 600
I I I I I I I
GA 798-868 525-595
AXIAL
RADIAL
5 10 15 20 25 30 35 40
FAST NEUTRON FLUENCE N / d ) (E >29 fJ)HTcR
Fig. B-12. Dimensional changes in near-isotropic graphite irradiated at
773 K to 873 K (500' to 600OC) (data from Refs. 6-4 and 6-6)
B-33
200
100
TENSILE STRENGTH
TI R R =860- 940 K
(587'- 667'C)
DESIGN
VE
0
I I 1 I J
TI RR' 1600-1630 K
200
(1327'-1357'C)
loo t ~ 0
DESIGN CURVE
0 2 4 6 8 10
H-451 YOUNG' S MOOULUS
TI R R =860-940 K
200 *
(587'-667'C)
u
t;
I!
w
W
v)
w
re
0
a
z
Tl RR= 1110-1250 K
T
(8370-977'C)
200 c d
200
100
0
TlRR =1600-1630 K
(1327'-1357'C)
T
0 2 4 6 8 10
FAST NEUTRON FLUENCE N h 2 ) (E>29 fJ)HTGR
Fig. B-13. Changes in tensile strength and elastic modulus of H-451
graphite as a function of fast neutron fluences.
denote 2 one standard deviation (from Ref. 6-3)
Error bars
.
Q
B-34
W
I
W
cn
C '
+l oo
. +80
ae
l w +60
3 -20
-40
0
1173 K
673 K CLIrrn,.nn\ m
1673 K
% (14OO0C)
A R
0 e 673 K (400OC)
-1
A A 1473 K (12OOOC)
1673 K (14OO0C)
0 1 .o 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0
FAST NEUTRON FLUENCE N h 2 ) (E>29 fJ)HTcR
Fi g. B-14. Fracti onal changes i n soni c el asti c modulus of extruded near-i sotropi c pi tch coke graphi te
(Dragon code No. 100) (from Ref. 5-7)
F
R
A
C
T
I
O
N
A
L

C
H
A
N
G
E

I
N

E
L
A
S
T
I
C

M
O
D
U
L
U
S

(
E
/
E
,
)

A
N
D

S
T
R
E
N
G
T
H

(
S
/
S
,
)

m

I

w

m

c

300
200
a
/
/'
I I I I I I
6 8 10 12
0 2 4
FAST NEUTRON FLUENCE N/m2) (E >29 f J)HTGR
Fig. B- 16. Calculated percent increases i n s t at i c e l as t i c modulus of near-
i sot ropi c graphites ( s ol i d parts of curves correspond t o data
i n Refs. 6-6 and 6-8; broken parts are extrapolated)
B-37
1 4
1 2
I ?
X
a -
0.4 t
-
-
-
0
0
0 0 0
0 90'90 e - 3
0
95' 95
99/95 - -
LOWER TOLERANCE
LIMITS
H-451 GRAPHITE
AXIAL ORIENTATION
MIDLENGTH CENTER LOCATION
IRRADIATE0 AT 1173 K (900C)
TO 3.8 x 1025 ~ i m 2 (EFFGO)
[3.0 x N/m2 (E >29fJ)HTGRI
1 I I 1 1 I I I l l I I I l l 1 1 I l l I I I l l I 1 1 1
1 IO 100 1000 10.000 101
0
NUMBER OF CYCLESTO FAILURE
Fi g. B-17. Fati gue test data i rradi ated to 3.0 x N/m2 (E > 29 fJ )HTGR at 1173 K (900OC). Log-log
pl ot of normal i zed peak stress versus number of cycl es to f ai l ure, wi th stress rati o, R =-1.
Lower x/y tol erance l i mi t s represent the ltmtts above wWch x% of al l data would f al l , wi th
y% confi dence; axi al specimens; open ci rcl es represent run-outs (from Ref . 5-10).
OESIGN
CURVE
0
u
0
0
In
0
cv
0
c!
Y
m
I
In
cv
r-
m -40
L
t
Tl RR =865 - 1045 K
(592' - 772'C)
0
SYMBOL
0
0
0
8
+
A
v
0
X
GRADE
H-451
H-451
H-451
H-451
H-451
H-451
H-429
H-429
TS-1240
TS-1240
TS-1240
TS-1240
SO818
SO818
LOT
266
266
266
266
426
426
-
--
_ _
-_
_-
- -.
- ..
4B
40
-
923 K ( 65OOCl
MLC
MLC
MLE
MLC
2 20
E
w
I
+
W
W
a
a
5
a
E o
>
w
W
z
I
I-
z
w
u
ce
w
-20
n
-40
-60
Ti RR 1080 - 1205 K
(807' - 932OC)
I I I I
0 2 4 6 8 10
FAST NEUTRON FLUENCE
N/m2 (E>29 fJ)HTGR
Fig. B-18. Percent change in thermal expansivity 1295 K to 773 K (22" to
500C)] of near-isotropic graphites as a function of fast
neutron fluence: irradiation temperature 865 K to 1205 K
(592' to 932OC) (from Ref. 6-3)
B-39
2o
t
0
-20
-40
SYMBOL
e
0
.8 +
X
A
A
V
0
I I ORI EN- I L OC A- - ~
H --45 1
H -45 1
H--451
H- 429
H -429
H -45 1
TS-1240
TS-1240
TSS1240
TS- 1240
50818
SO818
A X
RA D
A X
RA D
A X
RA D
A X
RA D
A X
RA D
A X
RA D
MLE
MLE
MLC
MLC
MLC
MLC
MLC
MLC
MLE
MLE
MLC
MLC
r T ~ R R =1250 - 1380 K
(977' - 1107OC)
-CURVE
1323
(1050C)
I
-60 I I I I I I
20
0
-20
$
-40
DESIGN
CURVE
1523 K
(125OOC)
+
DESIGN
I I I I I
0 2 4 6 8 10 12
-
FAST NEUTRON FLUENCE N/m2) (E>29 fJ)HTGR
Fig. B-19. Percent change in thermal expansivity [295 K to 773 K (22' to
500C)] of near isotropic graphites as a function of fast
neutron fluence: irradiation temperature 1250 K to 1705 K
(592' to 932'C) (from Ref. 6-3)
B-40
c
0 623 K (35OOC)
A 625-773 K (35O0-5OO0C)
0 773-823 K (50Oo-55O0C)
1 -
I I I I
5 C
4
3
2
TEMPERATURE
Fig. B-20. Change i n thermal expansivity of near-isotropic graphite
irradiated at 350" t o 55OoC (data from Ref. 6- 4)
B-4 1
AXI AL RADI AL
0 H-451 GRAPHITE, L OT 266
A H-451 GRAPHITE, LOT 426
0 TS-1240 GRAPHI TE
0 H-451 GRAPHITE, LOT 266
A H-451 GRAPHITE, LOT 426
0 TS-1240 GRAPHITE
O S 0 8 1 8 GRAPHI TE 0 SO818 GRAPHITE
100
50
0
TI RR=1195- 1220K
(922' - 967'C)
I
Tl RR =1615 - 1625 K
(1342' - 1352'C)
50 c
TI RR= 1195- 1220 K
(922' - 967'C)
Tl RR =1615 - 1625 K
(1342' - 1352'C)
X
Y
"
0 5 10 0 5 10 a
-
FAST NEUTRON FL UENCE N/m2) (E>29 f J ) HTc R
Fig. B-21. Thermal conductivity at the irradiation temperature for H-451
and other near-isotropic graphite8 as a function of fast
neutron fluence (from Ref. 6-3)
B-42
20
7
I
c
10
5
/ O 623 K (35OoC)
/------------
/ -4-
0
0-
0 '
0
0
-// 0 0
O O
0
8
SYMBOL
0
SOURCE T EMPERA T URE
OF D A T A
U KAEA 643-713 K (37Oo-44O0C)
DRAGON 708-723 K (435O-45OoC)
UKAEA 723-743 K (45Oo-47O0C)
UKAEA 823 K ( - 550OC)
DRAGON 895-921 K (622O-648OC)
5 10 15 20 25 30 35 40
0
FAST NEUTRON FLUENCE N/m2) (E >29 fJ)HTGR
6
Fig. B-22. Irradiation-induced changes in thermal resistivity of near-
isotropic graphite (data points from Refs. 6-6 and 6-8; curves
from Ref. 6-10)
B-43
GENERAL ATOMIC COMPANY
P. 0. BOX 81608
SAN DIEGO, CA L I FORNI A 92138