From Charpy to Present Impact Testing

D. Franqois and A. Pineau (Eds.)

~) 2002 ElsevierScience Ltd. and ESIS. All rights reserved 87

CORRELATION BETWEEN IMPACT RESISTANCE AND FRACTURE

TOUGHNESS IN AGED DUPLEX STAINLESS STEELS

L. SANCHEZ & F. GUTII~RREZ-SOLANA

Departamento de Ciencia e Ingenierfa del Terreno y de los Materiales

E.T.S. Ingenieros de Caminos, Canales y Puertos,
University of Cantabria, 39005 Santander, Spain.

ABSTRACT

As a part of a more extensive study [1 ] of aging embrittlement at low temperature (280-4000C)

of cast duplex stainless steels, a close characterization of the evolution of toughness of three
duplex steels with different ferrite content (12, 18 and 22%) has been performed.

Fracture toughness characterization was based on the determination of JR curves, in accordance

with the European Recommendations ESIS PI-92 and following the unloading compliance
single specimen method. Impact toughness was determined with an instrumented Charpy
pendulum, which permits the load-deflection and energy deflection curves to be obtained.

From the obtained results, a phenomenological model based on the presence of brittle ferrite in
the fracture path has been developed. This model enables the impact toughness and the fracture
toughness to be determined as a function of aging time and aging temperature for a duplex steel,
and therefore to predict fracture toughness values from Charpy results. Finally, a comparison
has been made between energy predicted from impact and experimentally obtained fracture
toughness for the three steels.

KEYWORDS

Cast duplex stainless steels, aging embrittlement, microhardness, instrumented pendulum, impact
resistance, toughness.

INTRODUCTION

For many years duplex stainless steels have been widely used in the chemical and petrochemical
industries as well as being employed in risk elements in power plants. These steels have a
biphasic microstructure composed of a discontinuous ferrite network distributed throughout the
austenitic matrix. The presence of ferrite in the duplex structure increases the mechanical
resistance and the resistance to stress corrosion cracking, improves the weldability, and makes
castings more resistant to hot cracking during solidification. However, it has been known since
the 80's that these steels are susceptible to thermal aging processes when they are used in .service
conditions at temperatures of around 280~ This leads to material embrittlement [1-5].

Many studies [1, 4] have shown that the aging processes, taking place in the 280-400~ range,
are principally due to the spinodal decomposition of the ferrite and its G phase precipitation. The
presence of M23C6 carbides and Cr2N nitrides may contribute to these embrittlement processes.
88 L S,~NCHEZ AND F GUTIERREZ-SOLANA

Austenofemtic stainless steel embrittlement, which depends on femte aging may be observed at
two different levels: the local embrittlement of the femte itself and the consequent bulk material
embrittlement. This bulk material embrittlement depends on the percentage and distribution of
the ferrite as well as the evolution in the relative participation of the aged ferrite and its interfaces
in the fracture mechanisms [l ]. These mechanisms are those which determine the limits of the
overall mechanical behaviour of the material.

An extensive research program was carried out in order to analyse the effect of aging at low
temperatures on the mechanical behaviour of three duplex stainless steels with different chemical
composition and ferrite content. Some of the results were presented in previous publications
[1,6-10]. This work summarizes the correlation between fracture toughness and impact energy.

MATERIAL

Table 1 shows the chemical composition and ferrite content of the three steels analysed, named
12F, 18F and 22F after their ferrite content. 12F is a commercial CF8M duplex stainless steel
taken from a valve aged in service for 10 years at -280~ 18F and 22F are similar duplex steels
obtained from experimental casts.

TABLE 1- Chemical composition and ferrite content of the studied CF8M steels.

STEEL C Mn I Si Cr Ni Mol %Ferrite

12F 0.035 0.7-0 1 . 1 0 18.6 10.4 2.00 12.2
18F 0.076 0.83 1.25 19.4 9.6 2.29 17.8
22F 0.045 0.82 1.23- 18.4 8.9[2.36 21.6

The overaging treatments performed on the 12F steel at 280, 350 and 400~ reached up to
18000, 14000 and 14800 hours, respectively. For the 18F steel and 22F different aging
treatments at the three temperatures have also been performed, up to a maximum value around
10000 hours.

EXPERIMENTAL

To analyse the effect of aging on these steels a mechanical characterization has been performed
including fracture toughness tests, instrumented impact tests and a fractographic analysis.

Fracture toughness evolution

Fracture toughness at room temperature was determined by J-integral R-curve, following

European Recommendations ESIS P1-92 [11], and the unloading compliance single specimen
method. CT specimens, 20 mm wide, were used, with 2 mm deep sidegrooves machined after
fatigue precracking. Figure 1 shows the JR curves for the 12F steel aged at 400~ Figure 2
shows the same for the 22F steel at different temperatures. These figures demonstrate the
important influence of aging on toughness such that fracture toughness clearly decreases with
longer aging times at any temperature between 280 and 400~

From de JR curves fitted by means of the power function

Jk = A . ~ t9 (1)

the crack initiation parameters Jo.2mL were obtained.

 Correlation Between Impact Resistance and Fracture Toughness 89

Instrumented Charpy impact tests

In order to obtain the brittle-ductile transition curves standardized Charpy impact tests were
camed out at-196~176 20~ and 280~ Figure 3 shows the evolution of the most
representative transition temperature (13") curves with aging for the 18F steel. From this figure
we can conclude that the upper and lower shelf energies decrease and the transition temperature
increases with aging.

Figure 4 shows the load-deflection curves (P-A) for the 18F steel for different aging times at
400~ The results show that thermal aging leads to a reduction of impact energy and an
increase of the strain-hardening rate of the material. The strain-hardening rate increases after
aging for a relatively short time and does not change significantly with further aging, in the same
way as hardness evolves with aging time [l, 10] reaching a final plateau.

12F STEEL 22F STEEL

2000 2000,
9 -400"C AS RECEIVED" .......
~,,~ AS RECI~IVED ..."
.... - . . ' . . . . "
69o~5~. t=51o h 9 ..9"1= 10300h ( 2 8 0 " C )
1500. ..."

j
i~,......
" .'""
..'. ..........
1=1050 h .....
.L~)...

.
1-158Oh (350"C) .

1000- r~6~_ 9..... ' " oO . . . . . . ,..4aa0 h. 1000- 90 " ~'' " " 1=375h 1400~

, . ~ ' ~ , ~ " OO O O " " .... t=14800 h"

9 t-33(X~ (400"C)
4- 9 . .. 9
500- 500- K" ....
/ :'"
~" O, O O
0 .0 " 0 " 0 " " O' '

r,5~~
0 . . . . . ! . . . . 1 . . . . | . . . . I . . . . | . . . . 0 . . . . | . . . . ! . . . . i . . . . | . . . . | . . . .
0 0.5 1 1.5 2 2.5 0 0.5 1 1.5 2 2.5
Crack Growth: &o (ram) Crack Growth: ,.~ (ram)

Figure I. Evolution of JR curves. 12F steel. Figure 2. Evolution of JR c u r v e s . 22F steel.

18F STEEL 18F STEEL

300
t t=1140 h (T=350"C) AS RECEIVED 18 T --40~C

2(~o1 -7==a,~;-;,~.c) 14
E ~. 12 t.310 n \
o
150] ~ l0
(o
1oo 6
5 1-10000 h (T=400"C) 4 t=10000 h~N,

l= 11540 h (T=350*C) 2
.... 1...... i ..... i ------- 1 0 , ~ --
-200 -100 0 100 200 300 0 2 4 6 8 10 12 14 16
Temperature: 9 ('C) Deflection: A (ram)

Figure 3. Evolution of C,, curves. 18F steel. Figure 4. Evolution of P-A curves. 18F steel.

Fractographic analysis

A fractographic study was made using scanning electron microscopy (SEM) to quantify ferrite
presence on the fracture surface. Figure 5 shows a fractography of the unaged 12F steel near
stretch zone in a CT sample. The fracture type was very ductile caused by microvoid coalescence
in austenite and no presence of femte was found. Generally, the percentage of ferrite in the
fracture path increases with aging. Figure 6 shows an example obtained from a broken Charpy
90 L. S,4NCtlEZ AND F. GUTIERREZ-SOLANA

specimen. The embrittled islands of ferrite break by cleavage and the corresponding facets
nucleate voids. The damage material finally breaks.

.s-
f

~ 9 _ , , ~ .~

9'L ~ , " ~ "P . . ,.._ d

, . .

0 8 Q ~ " ~ l g ~ m 1 2 4 3 1 4

Figure 5. Fractography of 12F steel as received. Figure 6. Fractography of 12F steel aged for
14800 hours at 400~

PHENOMENOLOGICAL MODEL

Using the exhaustive fractographic study a phenomenological fracture model was developed [ 1 I.
The crack initiation parameter J0.2mt., as well as tearing modulus, and impact resistance at room
temperature were related to the percentage of broken ferrite on the crack surface by using the
following equations

Jo.2/Bl. = Jo.2/Bt.
Y "X rJR( l- ,Uj "X~ R) (2)

Cv = Cr~ . Xrc, (I - l~c." Xac, ) (3)

where Xr and Xa were, respectively, the unitary fractions of austenite and ferrite on the crack
surface and Jo.2/m.
Y
and C,,Y are values associated with pure austenite which coincide with the as-
received values of each steel because the fracture process occurs only through austenite in the
unaged materials. The parameters pj and Pc are related to the effect of the broken femte
surface on the toughness, measured by Jo.2/m. or C,, respectively. These parameters, as a
function of Xa, come from the preliminary following, experimentally obtained, equations

Pj = 2.1+ 9.5"exp(-9.9" XJa" ) (4)

Xo )Cv
(5)

The unitary fractions of ferrite in the fracture surfaces, both in toughness and impact tests, have
been determined as a function of ferrite aging measured by microhardness increment dJ-/V and
the ferrite content by the equations

XJaR(%)= (-4.20+ 0.65. %a)O.Ol. AHV (6)

X~'" (%)= (-9.12+ 1.02.%a)O.O1.AHV (7)

 Correlation Between Impact Resistance and Fracture Toughness

I M P A C T R E S I S T A N C E AND F R A C T U R E T O U G H N E S S C O R R E L A T I O N

Experimental

From the results of the instrumented impact tests it is possible to obtain the load-deflection
(P-A) and energy deflection (E-A) curves. Figure 7 shows the characteristic curves obtained for
the 12F steel. In the P-A curve there are three singular points: the limit of the elastic zone, the
maximum load point and the point were the fracture was initiated.

Using the values of the P-A curve a new compliance parameter A/P was introduced. This
parameter represents the inverse of the slope of the secant line, stiffness, which joins the origin
with any point in the P(A) curve. The new curve A-A/P makes it possible to determine the point
at which the propagation starts, looking at the maximum change of the slope 16, 8, 12]. Using
this point it is possible to obtain the initiation energy, E,.

The total energy absorbed in the Charpy test, Et, can by separated into initiation energy and a
propagation energy:

E, = E+ + ~,, (8)

12F STEEL
10 -r--r - - I r" l 20
i ; i ENERGY (E) .

8- . ~. ........ ,!

61
i I I
,
, "'" ,'
.,,'[ 15

4
7 I
I LOAD (P)
I
I
." ''1 E.
,'
,,

! 1o

5
z
m

2
.'" '

0 0
0 2 4 6 8 l0 12 14 16
Deflection: ~ (mm)

Figure 7. Curves obtained from an instrumented impact test.

Figures 8 and 9 show the good correlation that exists between ~ and Et for the 12F and 18F
steels. A good correlation can be observed between both variables, which even seems to be
independent of the steel considered. Plotting together the obtained results for both materials, a
general relation can be obtained as follows

E i = - 2 6 . 9 + 0 . 8 6 . E, (9)

with a correlation coefficient R=0.97.

Taking into account that E~ is the energy necessary to initiate the propagation in an impact test,
the possibility of establishing a correlation between E, and the initiating parameter J0.2mL
obtained from the JR curves was studied. Despite the fact that the correlation between E, and F-,t is
good, the direct correlation between the resilience C,, and the J0.~L parameter it is more useful.
This is because most of impact toughness results from conventional pendulum are not
instrumented. Figures 10, 11 and 12 show the obtained results for the 12F, 18F and 22F,
respectively. Figure 10, representing 12F steel, offers a good correlation between both
parameters for a wide range of values. In the case of the 18F and 22F steels the number of data
92 L. SANCtlEZ AND F. GUTh~.RREZ-SOLANA

is smaller (Figures 11 and 12), and although it is possible to consider a linear correlation, this
was only made for the 22F steel because results for the 18F steel are clustered mainly in two
zones low aging and high aging conditions. For the 12F and 22F steels the linear correlation
found shows a parallel behaviour, with greater value of toughness for a given resilience in the
22F steel. Finally, Figure 13 shows the correlation between resilience C,, and J0.~L fracture
toughness parameter for the 12F and 22F steels. Correlation curves are very similar when
analysing the data separately or together. The difference between both steels is the shift to higher
toughness values for a given impact resistance C,,, with the increase in ferrite content.

12F S T E E L 18F S T E E L
200= 200-

~ -g----~.c] O
,~ 1N)'C o 0 , "o
![ o +,
++
+ ~ U ...'
150-
_c 4o0:% ... o 1 5O
o.. ..,o
.d"O
or .. ..'i) e O
"" 100 . !
w-
100-1
~.~o.AAZ~ w- 1 ...a"
-4 94 .....
.1~-
50- 50 9 jpr,.J "
[2 .' i, ~.. '
E, 9 -37.3 + 0.91F~ (R= 0.96) E, = -23.1 + 0.84E, (R= 0.97)
0 --'-"-" 9 ' i " - ,--.,r "-I'~'-""~ T--'---'- - ' - 0 t - - - - " - - ~ - ' - - .--,---,---,---r--T---r--
T- T--,---i--r---r---,--,
q
50 I O0 150 200 250 50 l/X) 150 2OO 25O
E, (J) Et (J)

Figure 8. Correlation E,-E t . 12F steel. Figure 9. Correlation E i -E t . 18F steel.

12F S T E E L
18F S T E E L
Iii~176 ~o 28o-c
350~
o I I00 I
i 0(X) 9 AS
RECEIVED]
o 280*C
~
O
~4(X)*C
c I 9

.[ soo], -J
I
- /
o /o "=)
" 7(X)-
I o o

-~
9")= 50O .]
4oo-~
300, Joza~= -218.0 + 4.69 C.(R= 0.96) ] 300i n
200 ~ . . . . .
so ,oo ,~o. . . . 26o- 2so 3oo so . . . . ,6o ,~o -26o " - 2~o- " - 300
C (Jlcm ~) C, (Jlcm z)
Figure 10. Correlation Cv - Jo 2/Bt.. 12F steel. Figure 1 1. Correlation C,, - Jo.zmL. 18F steel.

22F STEEL T =20~

1100 . . . . . I I00 to,,
I000
1 0 280"C / ~)
/ ,, ~'c I o/ 9 o o i ~ - - - -"L- - ~ J , ~
.=. 8OO
800 . . . . . . . .
700 ~q '
6o0
' 1
":,~ S00

400] i
400-i
3ool
2OO I
300-, C, (R= 0.96) 100-~ JO2ABt= " 55.4 + 4.56 C (R= 0.93)
t
2(:)01 n T==. . . . . . . ). . . . . . =="==~. . . . 0
50 I00 150 21JO 250 3(X) . . . . 5b. . . . ~s 26o 2~0--3oo
C, (Jlcm ~) c , (J/era2)
Figure 12. Correlation Cv-Jo.2mt.. 22F steel. Figure 13. Correlation Cv-Jo.2/BL. 12F-22F steel.
 Correlation Between Impact Resistance and Fracture Toughness 93

From modelling

With the phenomenological model described before it is possible to establish, for each tested
steel (12F, 18F and 22F) or a new one, pairs of C,, - J0.2VaL values obtained for increasing HV
values, simulating the aging process. Figure 14 shows the obtained values using this method,
correlating C,, and Jo.2mL for the three steels. On it two linear zones, A and B, can be
distinguished. Zone A is the same for the three steels and defines the correlation zone for highly
embrittled conditions. A linear correlation has been established for zone B independently for
each steel, as a function of ferrite level. A similar slope has been obtained for all steels according
to the experimental correlations.

In order to simplify, for the three steels zone B correlation lines, a single slope has been chosen
from the mean value of all of them: 6.3. Also in zone A the lowest line with the best fit has been
chosen in order to ensure safety conditions in the correlation. Taking this into account the
following equations define the final correlation between C,, and Jo.2mL obtained from the model
of aging embrittlement behaviour. For zone A:

Jo2/m. = 86. I + 1.7. C,, ( 1O)

For zone B:

9 if 12Fsteel
JO.2/BL - - - 623.2 + 6.3. C~ (11)

9 ifl8Fsteel
JO.2/BL = - - 53 I. 6 + 6.3. Cv (12)

9 if22Fsteel
Jo.2/lJt. = - 438.5 + 6.3. C v (13)

Figure 15 show the correlation equations together with the obtained experimental data for the
12F and 22F steels. It can be seen that the 12F steel fits well with the model, and is generally on
the safe side. The 22F steel is also accurate but with greater dispersion. However, it never
deviates more than 20% away from the experimental values.

1 I(X)
I I00 4 22-F--i8-(:-i 2 F---
I(X)O- + ~2F I ~ I---o- -'~FI /./~/
9(X)-i--o--18F I ,xx)- -t_._
- 9 22F I 9
800 [ -. .O. .-.-. . . 2 2 F .J
'
700- Joz~l. ='43'85.6"3C, (R-0~
80o~
000_ Jo~= --432.1 . 5 6 C
50O-
'TJ
(R=09~
"" 70oi

5O01
.-jo 400!

Joz/B. = ' 6 4 8 2 . 6 8 C , (R'0.~ I 30O:

20oi ~ \
10O! Jo ~ =86.1 +1.7C v R= 0.999
O-r . . . . . , ...... r ....
0 50 100 150 200 250 300
C v (Jlcm a) c, (Jlc~)

Figure 14. Correlation Cv - J0.2/BL. Figure 15. Correlation Cv - J0.2/BL.

94 L. S,~NCIIEZAND F. GUTIERREZ-SOLANA

CONCLUSIONS

In duplex stainless steels the effect of aging leads to a reduction in both impact resistance at any
temperature and fracture toughness. The effect is greater for longer exposure at elevated
temperatures and for increasing ferrite content.

The transition curves for impact toughness show a decrease in the upper and lower shelf
energies, and a shift of the transition temperature towards higher temperatures with increasing
aging levels. Also JR curves show the effect of aging on both fracture toughness and tearing
modulus.

The fractographic analysis performed at both static and dynamic testing procedures show that
austenite produces ductile fracture by coalescence of microvoids regardless of the aging level,
while ferrite suffers brittle fracture at elevated aging levels. The tendency of the fracture path to
follow the ferrite phase, previously broken, increases with aging.

A linear correlation was established between the fracture behaviour and the impact resistance for
these steels, with the same slope independently of ferrite content. A phenomenological model
based on the fracture micromechanisms observed was used to predict the values of J02mL and C,,
determined at each aging condition. Therefore a new correlation can be obtained between both
toughness parameters that differentiates two zones of behaviour: the zone for highly embrittled
conditions with a single correlation and the rest where the correlation depends on ferrite content,
maintaining the same slope. Good agreement with the experimental results have been shown,
always within the range of 20% of scattering which is comparable with the level of experimental
scattering due to non-uniform material behaviour and experimental variation effects.

REFERENCES

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189, Behal, V.G. and Melilli, A.S. (Eds). ASTM, Philadelphia, PA.
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Monterey, CA.
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