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A new series of advanced 3Cr-Mo-Ni steels for

thick section pressure vessels in high
temperature and pressure hydrogen service
ARTICLE in JOURNAL OF MATERIALS FOR ENERGY SYSTEMS DECEMBER 1984
DOI: 10.1007/BF02833446

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A New Series of Advanced 3Cr-Mo-Ni

Steels for Thick Section Pressure Vessels in High
Temperature and Pressure Hydrogen Service
R . O . R I T C H I E , E. R. P A R K E R , P. N. S P E N C E R , and J. A. T O D D

A new series of 3Cr-Mo-Ni steels has been developed for use in thick section pressure
vessels, specifically for coal conversion (high temperature and high pressure hydrogen)
service. The new steels rely on minor alloy modifications to commercial 2.25Cr-lMo
(ASTM A387 Grade 22 Class 2) steel. Based on evaluations in relatively small heats
(55 kg), the experimental alloys, which employ additions of Cr, Ni, Mo, and V, with Mn
at 0.5 wt pct and C at 0.15 wt pct, display improved properties compared to commercial
steels. Specifically, they show significantly improved hardenability (i.e., fully bainitic
microstructures following normalizing of 400-mm (16-in.) plates), enhanced strength
(i.e., yield strengths exceeding 600 MPa), far superior hydrogen attack resistance and
better Charpy V-notch impact toughness, with comparable tensile ductility, creep rupture
resistance and temper embrittlement resistance. The microstructural features contributing
to these improved mechanical properties are briefly discussed.

INTRODUCTION
The development of second and third generation coal conversion systems, such as proposed large-scale coal liquefaction and gasification processes, has necessitated the
design of large thick-section pressure vessels. L2.3 Materials
requirements for such vessels include weldable steels with
sufficient hardenability to maintain good mechanical properties throughout plate sections up to a maximum of roughly
400 mm (16 in.). In addition, yield strengths in excess of
350 MPa are required with sufficient toughness, creep rupture, fatigue and environmental degredation resistance to
withstand mechanically and environmentally hostile environments, which in certain instances involve hydrogen plus
hydrogen sulfide atmospheres at temperatures of - 5 5 0 ~
and hydrogen gas pressures up to 20 MPa (3000 psi). 3-6

R. O. RITCHIE, E. R. PARKER, and P. N. SPENCER are Professor, Professor Emeritus, and Research Engineer, respectively,
in the Department of Materials Science and Mineral Engineering,
University of California, Berkeley, CA 94720. J.A. TODD is
Assistant Professor, Department of Materials Science, University
of Southern California, Los Angeles, CA 90089. Presented at
American Society for Metals WESTEC '84, March 1984, Los
Angeles, CA.
J. MATERIALSFOR ENERGY SYSTEMS

Historically, the material favored for hydrogen service

pressure vessel construction has been 2.25Cr-lMo steel, 6,7
such as the normalized and tempered ASTM A 387 Grade
22 Class 2. Although this steel in general has ideal mechanical properties, it does not have sufficient hardenability to
produce the fully bainitic microstructures necessary to provide the desired low and elevated temperature properties in
normalized plate sections of the required 300 to 400 m m
(12 to 16 in.) thicknesses. 8 Moreover, there is also some
doubt as to the resistance of 2.25Cr-1Mo steel to hydrogen
attack under the most severe in-service conditions, 9-13where
elevated temperature and pressure gaseous hydrogen environments can result in an internal reaction b e t w e e n
ingressed hydrogen and carbides in the steel. This leads to
decarburization, cavitation and, in extreme cases, fissuring
from the formation and growth of methane bubbles at interfaces such as grain boundaries. ~4'~5'16
Both laboratory research and in-service experience
have shown that additions of certain alloying elements,
specifically carbide stabilizing elements such as vanadium,
niobium, and particularly chromium and molybdenum,
can have a markedly beneficial effect on hydrogen attack
resistance through the precipitation of stable carbides.~7"~8
However, there is some concern over the elevated temper-

9 1984 AMERICAN SOCIETY FOR METALS

VOL. 6, NO. 3, DECEMBER 1984

151

ature strength of such modified steels, due to their greater

tendency to precipitate M23C6 carbides which tend to
coarsen at service temperatures. 19.20Furthermore, commercial 3Cr-lMo compositions, such as ASTM A 387 Grade
21 Class 2, also have insufficient hardenability for section
sizes in excess of about 200 mm. 2~'22
Over the past few years, several major alloy design programs have been instigated to develop superior alternatives
to commercially available heavy section 2.25Cr-lMo pressure vessel steel for elevated temperature hydrogen service. 5"39-25Notable amongst these studies are the Japanese
Steel Works 3Cr-lMo steel microalloyed with Ti, V and B 24
and the Climax Molybdenum Company 3Cr-l.5Mo steels
containing 0.1 pct V and 1 to 1.4 pct Mn with 0.12 pct C
maximum. 19,21,23
In the current alloy development program the objective
was to design an improved hydrogen attack resistant steel of
higher strength to permit applications with thinner section
sizes, thereby saving in weight and cost. Similar additions
of Mo and Cr were employed to improve elevated temperature strength, oxidation resistance and resistance to hydrogen damage. However, 0.5 to 1 pct Ni was also added for
hardenability coupled with 0.2 pct V for creep resistance
and grain refinement. In particular, the Mn content was
limited to a nominal 0.5 pct in order to minimize potential
problems, from temper embrittlement susceptibility, 19,26,27,28
excess retained austenite following slow cooling* and hand*Both banding and the transformation of excess retained austenite on
tempering can lead to unexpected local susceptibility to hydrogen attack
due to non-uniform distributions of unstable alloy carbides. ~2

ing, which can be promoted by higher Mn contents. The

specific compositions (Table I), consisting of two 3Cr-1Mo1Ni steels, with and without 0.2 pct V (termed Steels C and
B, respectively), and two 3Cr- 1.5Mo-0.5Ni steels, with and
without 0.2 pct V (termed Steels E and D, respectively), are
compared with a conventional 2.25Cr-lMo steel of similar
purity and steelmaking practice (termed Steel A).
Such modified 3Cr-Mo-Ni steels are found to be far
superior to commercial 2.25Cr-lMo steels and to compare
very favorably with other advanced 3Cr-Mo materials. The
microstructural features contributing to the improved hydrogen attack resistance, as well as the superior hardenability
strength and toughness, and comparable ductility, temper

Table I.
Designation
Steel
Steel
Steel
Steel
Steel

152

A
B
C
D
E

embrittlement resistance and creep rupture properties, are

discussed in this paper.

EXPERIMENTAL PROCEDURES
The four experimental 3Cr-Mo steels and the reference
2.25Cr-lMo steel were produced as 55 kg (125 lb) laboratory heats by Climax Molybdenum Company using vacuum
induction melting and casting under argon atmospheres.
Chemical compositions in wt pct are listed in Table I. The
ingots were subsequently upset-forged and cross-rolled
to approximately 30 mm thick plates before austenitizing
for 1 hour at 1000 ~ Following austenitization, samples
were either quenched into agitated oil (i.e., cooling rate
1200 ~
or subjected to slow continuous cooling, at
8~
through the transformation range, using a programmable induction furnace. Based on cooling rate data
supplied by Lukens Steel Company, these treatments simulated both the surface and quarter thickness (0.25 T) locations, respectively, of a 400-mm (16-in.) thick plate during
accelerated surface cooling (herein referred to as normalizing). Tempering was carried out in neutral molten salt
baths at temperatures of 650 ~ and principally 700 ~ for
a range of times varying from 1 to 1000 hours. In terms of
the tempering parameter, P, sometimes referred to as the
Larson Miller parameter and defined as T[20+log t]
10-3 where T and t are the tempering temperature (in
Kelvin) and time (in hours), respectively, these treatments
represent a variation in P between 19.0 and 22.4 (or between 34.2 and 40.3 for temperatures in Rankin).
Room temperature uniaxial tensile tests were conducted
on 6.4-mm diameter specimens of 32-mm gauge length,
machined in the longitudinal direction of the plate, according to ASTM Standard E8-69. A displacement rate of
0.5 mm/min was employed. Standard Charpy V-notch
impact specimens were also prepared in the longitudinal
direction, and tested according to ASTM Standard E23-72
over a temperature range from - 1 9 6 ~ to 160 ~ Constant
load creep-rupture tests were performed in air using smooth
round bar longitudinal specimens of initial diameter 6.4 mm
and gauge length 25 ram, according to ASTM Standard
E-139. Tests were carried out at 560 ~ with engineering
stresses between 138 and 345 MPa (20 to 50 ksi).
Susceptibility to temper embrittlement was evaluated by
testing a further series of Charpy impact toughness speci-

Chemical Composition, in wt pct, of Reference 2.25Cr-1Mo and Experimental 3Cr-Mo Steels Tested
C

Mn

Si

Cr

Ni

Mo

AI

0.15
0.15
0.14
0.15
0.14

0.48
0.50
0.49
0.47
0.49

0.21
0.23
0.24
0.22
0.22

2.24
3.00
2.99
3.00
2.95

-0.98
0.98
0.50
0.50

1.01
1.03
1.02
1.50
1.50

--0.21
-0.21

0.006
0.008
0.006
0.006
0.006

0.0034
0.0040
0.0039
0.0036
0.0034

0.014
0.010
0.009
0.008
0.014

VOL. 6, NO. 3, DECEMBER 1984

J. MATERIALS FOR ENERGY SYSTEMS

mens which had been step-cooled, rather than air cooled,

following tempering at 700 ~ The step-cooling treatment 26
involved holding for progressively longer times at progressively decreasing temperatures from 595 ~ to 470 ~ as
illustrated schematically in Figure 1.
Susceptibility to hydrogen attack was evaluated with respect to both uniaxial tensile and impact toughness properties by prolonged exposure of oversize specimen blanks to
gaseous hydrogen atmospheres at temperatures of 550~ to
600 ~ and at pressures of 14 to 18 MPa (2000 to 2800 psi)
for times up to 1000 hours, prior to machining and testing.
Microstructures were examined with both optical and
electron microscopy. Thin foils for transmission electron
microscopy (TEM) were prepared from 0.6 mm steel slices
by chemically thinning to 0.05 mm in a hydrofluoric
acid/hydrogen peroxide solution before electropolishing at
room temperature in chromium trioxide/acetic acid solution.
Foils were examined using Phillips EM301 and 400 STEM
electron microscopes at 100 kV. Further analysis of the
carbide compositions was performed on the scanning
transmission electron microscope (STEM) using extraction
replicas. Quantitative estimates of the percentage of retained
austenite were assessed using both X-ray and magnetic
saturation techniques.

RESULTS
Strength and Ductility
The room temperature uniaxial tensile properties of the
four 3Cr-Mo-Ni steels, after slow-cooling (8 ~
and
tempering at 700 ~ for various times between 1 and
1000 hours, are shown in Figure 2. These heat-treatments
represent a range of tempering parameters (temperatures in
Kelvin) between 19.5 and 22.4. It is apparent that all four

Temperin~

1400 -

120(

IOOO*C, I hr

700Oc, 4 h r

~E

)~

I
SI. . . . .

I "~
~8~

F-~

~o'c,

\ /
'~

-%.

,oo

yield Strengt h'~ '~ "~...~ ? . ~ . ' - - ~z,.."~ t

-':

400

~"
"
200 --~ ' " "%7 "Elont.jotion

"-''~

....

ill

"---

O E
~ O [] 0
4L ~ ~ (~

R.A.
UTS

& (ll rl ~

YS

9 9

Elon(J. ~ . . . .

.....

I
I

J
I
o
I0
I00
1000
Tempering Time (hr$) of 7OO"C
Fig. 2 - - R o o m temperature uniaxial tensile properties for experimental
3Cr-Mo-Ni steels, slow-cooled and tempered at 700 ~ as a function of
tempering time and tempering parameter (in Kelvin).

o--f[
0

steels show similar mechanical properties (the V-containing

C and E steels are marginally stronger), with ductilities
fairly constant at pet RA between 70 and 80 pet, and with
tensile strengths above 600 MPa (87 ksi), even at the
longest tempering times.

Toughness

SC 8tT ot 7 0 0 ~

O Steel e

,, Stee, C

4hrs

~.-

200

os,e.,o
o s,ee~E o / / / / ~

]~50 ~,
E

],oo
,5o
-

STEP COOL

Furnace cool ~ " ~

to 315~
Air COOl

Fig. 1 - Schematic representation of the heat treatments used to assess

susceptibility to temper embrittlement.
J. MATERIALS FOR ENERGY SYSTEMS

ItS

st., 8

\ 495"C, 48 hr

Air cool

~'*/o Red'n. Area

'~l176 fst"'c//7--s'"'~
/ 7/-

,5.,

s~*c,, h,

(Y". . . . . .

600

I hr

80

,.,@,,.

al
t/)

Air COOl

700eC, 4 hr

r\

EMBRITTLED (Slow cooled, tempered and step cooled)

oo~

~0

150-

1000~

~O--~

22

The Charpy V-notch impact toughness, as a function of test

temperature for the four 3Cr-Mo-Ni steels, slow-cooled
(8 ~
and tempered 4 hours at 700 ~ (P = 20), is
shown in Figure 3. The toughness of Steels C, D, and E

UNEMBRITTLED (Slow cooled and tempered)

~eOC/min

Parameter

P = T (K) [20-1- Io9 t(hrs)J=lO -3

19
20
21
1
I
I
HEAT-TREATED

~176 //

-200

-I 0 0

1
0

0
100
200
Test Temperoture (~
Fig. 3 - - C h a r p y V-notch impact toughness transition curves for experimental 3Cr-Mo-Ni steels, slow-cooled and tempered (SC & T) at 700 ~
f o r 4 h.

VOL. 6, NO. 3. DECEMBER 1984

153

200

is clearly similar with a 40 ft-lb (equivalent to 54 J)

ductile/brittle transition temperature just below 0 ~ and
an upper shelf energy above 176 J (130 ft-lb). The 3Cr1Mo-lNi Steel B, however, is distinctly tougher with a
transition temperature b e l o w - 1 0 0 ~ and an upper shelf
energy above 200 J (150 ft-lb). 2~ This steel shows similar
high toughness when oil quenched and when tempered
4 hours at 650 ~ (P -- 19), as seen by the (unexposed) data
in Figure 4.29

>"

td

UNEXPOSED/l

/ P /

~ -.r

0~-][~

-I00

~50

,' , 0 7

,;/,'/'

~o

.,oo,,~o-~..~
f. 9 0Q~'TTOO'C+HE

I
0
TEMPERATURE

I
r00

I
200

(*C)

Fig. 4 - - Charpy V-notch impact toughness for experimental3Cr-l Mo- l Ni

Steel B, oil quenched (OQ) or slow-cooled (SC) and tempered (T) 4 h at
650 ~ or 700 ~ in the prior hydrogen exposed (HE) condition (600 ~
17 MPa pressure) and unexposed condition.~9

Hydrogen Attack Resistance

In Figure 6, the room temperature uniaxial tensile data for
the four 3Cr-Mo-Ni steels are given, as a function of tempering time at 700 ~ following slow cooling from 1000 ~
for samples which have been previously exposed for
1000 hours to 14 MPa (2000 psi) hydrogen gas at 550 ~
By comparing with the scatter bands, which represent the

Steel C ( 3 C r - I M o - I N i - 0 , 2 V )

150

200

SC 8=Tot 700 ~C; 4 hrs

150
"' I00
/

Unembrittled

~ T e m p e r Embrittled

~
50

IOO

~ 50--

0 ""-- I
-200

IO

-I00

I OO
Test Temperoture (~

SC & T ot 7OOeC4 hrs

l/

"Temper Embrittled
(Step cooled)

i$0-

! I~t-~1--

-IOO

I00
Test Temperoture (~C:)

-- 150

~ /~Y

50
I

200

Steel E (3Cr-I.SMo-O.SNi-O.ZV)

200

e~
c
LIJ

150
100

ioo

o 50

~Temper Embrittled
(Step cooled)

50

o
O
-2OO

I~"- I
-IOO

I 'r'l I
0

I0o
Test Temperoture (='C)

w
ii

SCS=Tot 7OO~C4hrs S

Unembrittled

- 200

~''"~

-2OO

~ 1oo

200

Steel O ( 3 Cr- I.S Mo -0.,'5 Ni )

-'12 1 5 0 -

~J

n.

,'.E'

J /
2

250

/ ///

ZOO

IOC

E
~

b.V SC+ T?OO~C

SCS=TOt700C 4hr

,~....-,--"T . . . . . . .

Charpy V-notch toughness transition curves for the four

3Cr-Mo-Ni steels in a temper embrittled condition, induced
by a step-cooling treatment (Figure 1) following tempering
4 hours at 700 ~ are compared in Figure 5 with transition
curves of corresponding unembrittled microstructures. With
embrittlement, all steels show a reduction in upper shelf
energy of between 10 and 40 J and a shift (AT) between 15~
to 55 ~ in the 40 ft-lb transition temperature to higher
temperatures (Table II). Although behavior is again somewhat similar in the four steels, the 3Cr-lMo-lNi Steel B still
displays the lowest ductile/brittle transition temperature.

STEEL

/ ~//

Temper Embrittlement Resistance

Steel B ( 3 C t - I M o - I N i )

INi

z ~ / o

0 ~,~r .
-200

ISC

3 Ct-IMo-

I
200

"~t-emper Emlxittled

50--

50
r

-200

-I0O

V"-

IOO
Test Temperoture (*C)

200

Fig. 5--Charpy V-notch impact toughness transition curves for experimental3CR-Mo-Nisteels, slow-cooledand tempered (SC & T) 4 h at 700 ~ in the
temper embrittled (step-cooled) and unembrittledconditions.

154

VOL.6, NO. 3, DECEMBER 1984

J. MATERIALS FOR ENERGY SYSTEMS

Table II.

Effect of Temper Embrittlement on Charpy V-Notch Impact Toughness

40 ft-lb (54 J) Transition Temp.

Steel*

Unembrittled

A
B
C
D
E

- 13
-105
- 25
- 20
- 10

*Slow cooled
,o1, (8 ~

Temper Embrittled

~
~
~
~
~

--40
-I0
25
15

Shift

Unembrittled

Temper Embrittled

(J)
122
206
186
203
176

(J)
-165
175
175
163

~
~
~
~

AT

-65 ~
15 ~
45 ~
25 ~

tempered
~ered 4,. hr at 700 ~

Tempering

1501 I

Parameter

P = T ( K ) [ : > 0 + log t (hrs)] x 10-3

,,~
1400[-

Upper Shelf Energy

~o

~,,

~,~

HYDIRoGE__
N EXPOSED

II

- 200

H ~ ' T - T R E A T E D S'EELS

80

I\
I ~

--'"

I %'"
,~oo~/~...

150

o . . ._. . . , a . . . _ _ o . _ . L

~_

. . .... . ... . . .

....

'=

~...d'n~..~

I00

I ' , \

L><2

's

5O

".

..

'x "

"

"II-.

"~"-L~."-.

~oo

Yield Strength /

-'<

,=t

O~

:~

- -:>-~-::--.

,_"

:0

~EM.ER,.G T,ME ,..S,"OOAT,OO'~ 't~176176

(a)

~._~.-e--~

.~/~,...~......~.~"t
20C

CB

:o

OE

"&Elongation

=
I
Tempering

A 000
R.A.
~ ~ $ UTS

IOC

bounds of the corresponding data on unexposed samples

from Figure 2, it can be seen that, apart from a slight
decrease in pet RA in the higher strength conditions, there
is little evidence of hydrogen attack damage in these steels
(tempered at 700 ~ for this hydrogen exposure.
A similar result is obtained when comparing the effect of
hydrogen attack damage on room temperature Charpy Vnotch toughness (F'gure 7). In Figure 7(a), the toughness of
unexposed samples is plotted as a function of tempering

//f

Z
I,u

U
<I
O.

I
!
I
I

~E

o.
5C
rr
"I"
t.3

. . . . . . . . .

7/-

,-,~

150
I

~
,,/0

/ . . . .

/1

-E

~
I

- IOO~
o

STEEL B

50

D STEEL O
O STEELE

(HEAT-TREATED)
0 ~.(I
0

_J

AND
HEAT TREATE'D

I
I

//

/
/

~N-EXPOSED

7,
tlJ

t
0

0----

I0//

200

"I//
l-

)-

I000

Fig. 6 - - R o o m temperature uniaxial tensile properties for prior hydrogen

exposed 3Cr-Mo-Ni steels, slow-cooled and tempered at 700 ~ as a
function of tempering time and tempering parameter. Hydrogen exposure for 1000 hr at 550 ~ with 14 MPa pressure. Scatter bands represent bounds of data for corresponding unexposed conditions, shown in
Figure 2.

J. MATERIALS FOR ENERGY SYSTEMS

,,

Oh

IO
I00
Time (hrs) at 7 0 0 " C

S?EL B (HEAT-TREATED)7
._1

& (! I! ~, YS
.....
9 9 9 9 Elong.-- . . . .

o~'f

t5o

I0
I00
TEMPERINGTIME(HRS)AT 700=C
(b)

I000

Fig. 7 - - R o o m temperature Charpy V-notch impact energy as a function

of tempering time at 700 ~ for slow-cooled 3Cr-Mo-Ni steels in the (a)
heat-treated (unexposed) and (b) hydrogen-exposed conditions. Hydrogen
exposure for 1000 h at 550 ~ with 14 MPa pressure. Scatter bands represent bounds of data for unexposed conditions.
VOL. 6, NO. 3, DECEMBER 1984

155

time at 700 ~ following slow-cooling from 1000 ~ As

noted above, Steel B is distinctly tougher and reaches a high
room temperature toughness, corresponding to upper shelf
ductile fracture by microvoid coalescence, after only short
tempering times at 700 ~ The other steels show mixed
mode transitional behavior, with consequent lower toughness, as their respective transition temperatures are closer to
room temperature ( c . f . , Table II). Following prior
1000-hour exposure to 14 MPa hydrogen at 550 ~ the
toughness in all steels is essentially unchanged [Figure
7(b)], with no apparent differences in fracture morphology
compared to corresponding unexposed conditions. Steel B,
however, does show a slight decrease in toughness. This
may be more associated with entrapped hydrogen rather than
hydrogen attack damage from internal voids and fissures,
because subsequent re-heating of prior damaged samples for
80 hours at 275 ~ (which bakes out dissolved hydrogen)
returns the toughness to undamaged levels (i.e., excess
of 135 j).25
The effect of more severe hydrogen exposures [corresponding to 17 to 18 MPa (2500 to 2800 psi) pressures] is
shown in Table III and Figure 4 for the 3Cr-lMo-lNi Steel
B, with samples tempered either at 650 ~ or 700 ~
(4 hours) following either oil quenching or slow-cooling
(8 ~
z9 For all structures, some small degree of softening can be seen (tensile strengths reduced by 7 to 17 pet),
together with a small decrease in upper shelf toughness
(by between 2 and 22 pct) and a shift in the ductile/brittle
transition temperature (by 65 ~ to 97 ~
Fracture surfaces
on broken Charpy specimens were predominately intergranular close to the notch in prior hydrogen exposed sampies, but there was no evidence of voids on the intergranular
facets which are so characteristic of hydrogen attack damaged structures. ,2
By comparison with Figure 5, it is felt that this decrease
in toughness following prolonged hydrogen exposure is
again probably not predominately due to hydrogen attack,
but rather to temper embrittlement occurring during the ther-

,501

Condition

Slow-cooled, 4 hr at 650 ~
Slow-cooled, 4 hr at 700 ~
Oil Quenched, 4 hr at 650 ~
Oil Quenched, 4 hr at 700 ~

U.T.S.
(MPa)

ZOO

Slow cooled ond tempered f

at 700 * C / 4 h
<u

~J~ IOC

Unembrittled\

~
o.

,~

~--Temper Embrittled

/~

o
J=
u

{600eC/IOOOh/17MPo)

-200

'~

C/~HydrogenExposed

~11
-I00

150

0
I O0
Test Temperature (*C)

50
0

200

Fig. 8 - - E f f e c t o f prior temper embrittlemcnt and hydrogen attack on

Charpy V-notch impact toughness of experimental 3Cr-1Mo-1Ni Steel B,
slow cooled and tempered 4 h at 700 ~

mal exposure. 25 In fact, duplicate Charpy specimens, slow

cooled and tempered 4 hours at 700 ~ when heated for
1000 hours at 550 ~ in an inert atmosphere, were found to
have similar toughnesses to the hydrogen exposed samples.
Furthermore, the toughness of step-cooled (temper embrittled) samples in this steel was almost identical to that
following hydrogen exposure (Figure 8).
Thus it is apparent that there is only a small influence of
hydrogen attack damage in these steels, with the susceptibility to embrittlement being far less than that reported
for 2.25Cr-1Mo steel or for 3Cr-1Mo-1Ni steels containing
higher (i.e., 1 pet) Mn contents. ]2

Creep Rupture Resistance

Creep-rupture data for the four 3Cr-Mo-Ni steels (slowcooled and tempered 4 hours at 700 ~ are shown in Figures 9 and 10. Results at 560 ~ are compared to
2.25Cr-lMo steel :~176 in terms of applied stress vs life
(Figure 9) and creep rupture ductility (pet RA) vs life
(Figure 10). On the basis of these data, the elevated temperature properties of the 3Cr-Mo-Ni steels are clearly

Table lU. Effect of Hydrogen A t t a c k o n Uniaxial Tensile and Toughness Properties in 3 C r - l M o - l N i

Yield Stress
(MPa)

S,~e___L~._(3Cr-'
N~______)
Mo-1
~

pet Elong.*

pct Redn.
Area

Upper Shelf
Charpy Energy
(J)

UE

HE

UE

HE

UE

HE

UE

HE

UE

HE

691
627
660
545

552
552
537
502

781
779
782
664

647
661
638
616

20
24
24
24

22
23
22
25

75
73
76
76

73
73
73
71

189
206
190
230

162
161
186
178

Steel B
40 ft-lb (54 J)
Transition Temp.
(~
UE
-100
-105
-115
-120

HE
~
~
~
~

-23
-40
-50
-23

~
~
~
~

*On 32 m m gauge length.

Legend: UE = Unexposed, HE = Hydrogen Exposed (600 ~

156

VOL. 6, NO. 3, DECEMBER 1984

17 MPa)

J. MATERIALS FOR ENERGY SYSTEMS

Fig. 9--Creep rupture properties at 560 ~ of experimental 3Cr-Mo-Ni

steels, slow-cooledand tempered4 h at 700 ~ Results are comparedwith
previous data2~176 on 2.25Cr-lMo steel.
I

Fig. 11--Optical micrographs of microstructures after slow-cooling at

8~
to simulate the 0.25T cooling rate in normalized 400 mm
(16 inch) plate. (a) 2.25Cr-lMo steel, showing bainite and 40 pct polygonal ferrite, and (b) 3Cr-lMo-lNi steel, showing 100 pct bainite (etched
in nital).

I00

-- -- 0

*~ 8 O

. . . . .
C~

(]5

13

09

00

6O

SC a T o t 7 0 0 ~
9 Steel A
0 Steel B
Steel C
I~ Steel D
0 Steel E

"o

0.I

4 hrs; Tests ot 5 6 0 " C

(Bose 2 . 2 5 C r - I M o )
(3Cr-IMo-INi)
( 3 C r - I Mo-I Ni-O.?V)
(3Cr-I 5 Mo-OSNi)
( 3 C r -I.5 MO-0.5 Ni-O.2V)
I
I

1
I
I0
I00
Rupture Time (hours)

I
I000

I0,000

Fig. 101Creep rupture ductility (pct RA) v s time to rupture for experimental 3Cr-Mo-Ni steels, slow-cooled and tempered4 h at 700 ~ from
constant load tests at 560 ~ at stresses between 138 and 345 MPa.
comparable with those of 2.25Cr-lMo steel. Furthermore,
at longer lives (above 1000 hours), the 3Cr-Mo-Ni steels
actually out perform commercial 2.25Cr-lMo alloys, particularly in the V-containing C and E steels which tend to
display the best performance at the lower applied stresses.

Fig. 12--Scanning electron micrograph of 3Cr-l.5Mo-0.5Ni Steel D in

the slow-cooledand untempered condition, showing 100 pct granular bainitic microstructure (etched in hot picric acid and nital).

Hardenability
For cooling rates as slow as 8 ~
typical of the conditions at quarter thickness of a 400-mm thick plate during
normalizing, commercial 2.25Cr-lMo steel generally has
inadequate hardenability to ensure fully bainitic microstructures, as evidenced by the substantial proportion
( - 4 0 pct) of the polygonal ferrite in as-cooled structures
[Figure ll(a)]. The experimental 3Cr-Mo-Ni steels, conversely, with their increased Cr + Ni additions, show
vastly enhanced hardenability and 100 pct granular bainitic
structures after a similar slow cooling rate of 8 ~
[Figure 1l(b)].

Microstructures
As noted above, the microstructure of all four 3Cr-Mo-Ni
steels was found to be 100 pct granular bainite, with a prior
austenite grain size of approximately 50/xm (Figure 12). In
the as-cooled untempered conditions, fine autotempered
J. MATERIALSFOR ENERGY SYSTEMS

M3C (cementite) precipitates (Figure 13) and films of retained austenite (Figure 14) are evident between bainitic
laths. X-ray and magnetic saturation studies on Steel B have
indicated that the proportion of such interlath austenite is
approximately 17 pct in the as-cooled condition, compared
to 5.5 to 7 pct in the as-quenched state. 29
On tempering at 700 ~ for 1 hour, fine accicular intralath carbides (--0.05 /xm in size) together with coarser lath
boundary carbides (--0.25 /zm in size) were observed and
identified, using selected area diffraction, as cubic M23C6
(Figure 15). 32No evidence of the hexagonal M2C or M7C3 or
orthorhombic M3C carbides could be detected. This is in
stark contrast to 2.25Cr-lMo steel where, at 700 ~ M3C
precipitation can persist up to tempering times of 30 hours
(Figure 16).33 After 1000 hours at 700 ~ M23C6 precipitates in the 3Cr-Mo-Ni steels are typically 0.5 to 1 bcm in
size (Figure 17) with additional evidence of the Mo-rich
M6C precipitates (Figure 18), and in the C and E steels VC
VOL. 6, NO. 3, DECEMBER 1984

157

Fig. 13
T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s of s l o w - c o o l e d
3Cr-1Mo-INi Steel B in the untempered condition, showing (a) bright field
of ferrite (a) and_f'me autotempered cementite (0), (b) dark field of cementite from (210)o reflection of (c) selected area diffraction (SAD)
pattern, and (d) interpretation of (c). 32

Fig. 1 5 - - T r a n s m i s s i o n e l e c t r o n micrographs of slow-cooled

3Cr-l.5Mo-0.5Ni Steel D after tempering at 700 ~ for 1 h, showing
(a) bright_field of ferrite and M23C~ precipitates, (b) dark field of carbide
from (022) M23C6 reflection of (c) SAD pattern, and (d) interpretation
of (c).32

Fig. 16--Experimental data of Baker and Nutting33 showing the sequence

of carbide formation during tempering of a normalized 2.25Cr-lMo steel.
Fig. 1 4 - - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s of s l o w - c o o l e d
(3Cr-l.5Mo-0.5Ni) Steel D in the untempered condition, showing
(a) bright field of ferrite (a) and interlath retained austenite (3), (b) dark
field from (200)v austenite reflection of (c) SAD pattern, and (d) interpretation of (c). 32

precipitates. The types of carbide in these structures were

confirmed with extraction replica studies in the STEM using
analyses developed by Titchmarsh 34 and Shaw. 35 Carbide
types in Steels B, D, and E are shown in Table IV together
with their respective compositions in atomic percent.
158

VOL. 6, NO. 3, DECEMBER 1984

DISCUSSION
On the basis of the TEM and STEM studies (Figures 15, 17,
and 18), it is clear that the increased Cr and Ni content in the
present 3Cr-Mo-Ni series of steels leads to a markedly accelerated tempering response compared to 2.25Cr-lMo
steel. In particular, the iron and chromium-rich M23C6 carbide replaces the less stable M2C, M3C and M7C3 carbides
J. MATERIALS FOR ENERGY SYSTEMS

Fig. 1 7 - - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h s o f s l o w - c o o l e d
3Cr-lMo-lNi Steel B after tempering at 700 ~ for 1000 h, showing
(a) bright field of ferrite and M23C6 precipitates, (b) SAD pattern, and
(c) interpretation of (b). 32

Fig. 1 8 - - T r a n s m i s s i o n e l e c t r o n m i c r o g r a p h o f s l o w - c o o l e d
3Cr-I.5Mo-0.5Ni-0.2V Steel E after tempering at 700 ~ for 1000 h,
showing (a) bright field of ferrite, and M23C6 and M6C carbides, (b) dark
field of (026) M6C reflection of (c) SAD pattern, and (d) interpretation

of (c).32

Table IV. STEM Analysis of Carbide Precipitates in 3Cr-Mo-Ni

Steels Tempered for 1000 hr at 700 oC

Pct Cr

Pct Mo

Pct Fe

Pct V

/
~j

Composition (Atomic Pct)

'

'

-- 150~- _Stee_.~lB (._3.3Cr-!Mo-INi)

200

Quenched ond tempered

ot 650 =C/4 h

lo Unexposed

. . . .

I /% H:~exposed , *

i O0 -

Type
Carbide

(6000c,

o, o

--2:

150

~--

~.~--'e'-

I00
Steel B
Fine ppts (0.1 /zm)
Elongated ppts (1.0/zm)
Massive ppts (1.0/xm)

43.9
24.7
37.7

11.6
32.7
11.2

44.5
42.6
51.1

Steel D
Fine ppts
Elongated ppts
Massive ppts

17.2
36.3
46.0

36.5
17.5
7.3

Steel E
Fine ppts
Elongated ppts
Massive ppts

8.8
t0.6
I 1.9

4.0
45.8
43.1

--

M23C6

--

M6C

:~

--

M23C6

~.

46.3
46.2
46.7

---

M6C
M23C6

--

M;~3C6

1.2
43.6
45.0

86.0
---

/
.s"

VC
M6C
M6C

after only an hour of tempering at 700 ~ compared to

approximately 400 hours in 2.25Cr-lMo steel (Figure 16).
It is felt that specifically the rapid elimination of Fe3C (i.e.,
within 1 hour at 700 ~ compared to roughly 30 hours in
2.25Cr-1Mo) and the rapid precipitation of more stable alloy
carbides on tempering is primarily responsible for the enhanced hydrogen attack resistance in the 3Cr-Mo-Ni steels.
This enhanced resistance to hydrogen damage can be seen
clearly in F i g u r e 19 where the impact toughness
3Cr-lMo-lNi Steel B is compared to 2.25Cr-lMo Steel A
in the prior hydrogen exposed and unexposed conditions
J. MATERIALS FOR ENERGY SYSTEMS

-200

/~
/

~
-IO0

-,)

225Cr-IMo Steel

Z~I~"

at 6500C/4h
- 50
9
f H2 e~posed(550 C. 14 MPa)
0

I00

200

Temperoture (=C)
Fig. 1 9 - - C o m p a r i s o n o f Charpy V - n o t c h impact t o u g h n e s s o f
2.25Cr-lMo steel and experimental 3Cr-lMo-lNi Steel B, both quenched
and tempered 4 h at 650 ~ prior to, and after, 1000 h high temperature
exposure to gaseous hydrogen (550 to 600 ~ 14 to 17 MPa pressure).

(both steels were oil quenched and tempered 4 hours at

650 ~
Even though the 3Cr-lMo-lNi steel suffered a
higher exposure (17 MPa hydrogen pressure at 600 ~ compared to 14 MPa at 550 ~ its toughness remained superior
to the 2.25Cr-lMo steel, both in terms of a lower transition
temperature and higher upper shelf energy.
The Cr + Ni combinations in the experimental steels also
provide a potent effect in vastly increasing hardenability, as
evident by the fully bainitic microstructures (Figure 11)
following simulated normalizing of 400-mm thick plates
(0.25T location). Mn contents, however, were deliberately
limited to 0.5 pct as prior experience ~2with a 3Cr-IMo-IN;
VOL. 6, NO. 3, DECEMBER 1984

159

steel containing 1 pct Mn had indicated lower creep

strength and problems with hydrogen attack susceptibility
where, particularly after slow cooling, the transformation of
high carbon retained austenite on tempering lead to a prolonged stability of Fe3C carbides. Higher Mn contents are
also known to promote banding, which again is detrimental
to hydrogen attack resistance, and to increase susceptibility
to temper embrittlement.26,27,2s
Aside from generally improving temper embrittlement
resistance, the Mo content of 1 to 1.5 pct provides for good
elevated temperature strength and creep-rupture properties.
This is further enhanced in Steels C and E by the precipitation of a vanadium carbide. Although in the past there has
been some question about the creep resistance of 3Cr-Mo
steels, 19'2~the present series of alloys compared very favorably with 2.25Cr-lMo steel, at least over the testing range
of temperatures and stresses (Figures 9 and 10).
Although not studied in the present investigation, the
weldability of these steels should not cause problems with
standard welding and pre-heat practices due to the relatively
low carbon contents (i.e., O. 15 max wt pct). In addition,
preliminary data on fatigue crack propagation behavior indicate a crack growth resistance similar to 2.25Cr- 1Mo steel.36
Thus, the present series of experimental 3Cr-Mo-Ni steels
provides superior alternatives to 2.25Cr-1Mo steel for thick
section pressure vessel applications involving hydrogen at
elevated temperatures and pressures. Although evaluations
have only been completed to date on relatively small heats
(55 kg), the new steels appear to out perform 2.25Cr-lMo
with respect to hardenability, strength, toughness and hydrogen attack resistance and to be comparable with respect
to ductility, temper embrittlement and creep resistance
(Table V). There may be applications for lower temperature (i.e., below 500 ~ hydrogen service where the
3Cr-lMo-lNi Steel B may be preferred because of its very
high toughness. 25 For service at higher temperatures, the

vanadium containing Steels C and E may be preferred because of their superior creep strength.
Finally, the present series of steels compare very favorably with other recently developed 3Cr-Mo alloys for thick
section, hydrogen service pressure vessel application,
namely the 3Cr-I.5Mo-0.1V steels developed by Climax
Molybdenum~9'2~'23 and the 3Cr-lMo-0.25V, Ti, B steels
developed by the Japan Steel Works. 24 As shown in Figures
20 to 22, all three series of steels out perform 2.25Cr-lMo
steels. However, whilst the creep rupture (Figure 20) and
temper embrittlement resistance of the three 3Cr-Mo steels
is similar, the current 3Cr-Mo-Ni alloys appear to offer the
best combinations of strength and toughness (Figures 21
and 22).

Fig. 2 0 - - C o m p a r i s o n of the creep rupture strength of slow cooled and

tempered experimental 3Cr-Mo-Ni alloys with 2.25Cr-lMo steel, 3~ the
Climax Molybdenum 3Cr-l.5Mo steels, x9'21 and the Japan Steel Works
3Cr-lMo-0.25V, Ti, B steel. 24

Table V. Comparison of Mechanical Properties of New 3Cr-Mo-Ni Steels with 2.5Cr-lMo,

and Tempering at 700 oC (4 hr)*
Following Slow Cooling (8 ~

Code

A
B
C
D
E

Yield
Stress

UTS

Elong.**

RA

MPa (ksi)

MPa (ksi)

Pct

Pct

641
779
772
799
821

24
24
26
22
21

73
73
75
73
74

Alloy

2.25Cr-lMo
3Cr-lMo-lNi
3Cr-IMo-INi-0.2V
3Cr-l.5Mo-0.5Ni
3Cr-I.5Mo-0.5Ni-0.2V

496
627
593
655
676

(72)
(91)
(86)
(95)
(98)

(93)
(113)
(112)
(116)
(119)

Upper
Shelf
Charpy
Energy
J (ft-lb)

122
206
186
203
176

(90)
(152)
(137)
(150)
(130)

40 ft-lb
Transition
~ C (~

- 13
-105
- 25
- 20
- 10

(
9)
(-157)
( - 13)
(4)
(
14)

Creep
Rupture Life
at 200 MPa
(560 ~
hr
457
269
947
212
1253

*Tempering Parameter (K) = 20.04

**On 32 m m gauge length

160

VOL. 6, NO. 3, DECEMBER 1984

J. MATERIALS FOR ENERGY SYSTEMS

CONCLUSIONS
A new series of 3Cr-Mo-Ni steels has been developed to
provide alternatives to 2.25Cr-1Mo steel for thick section
pressure vessel applications involving high temperatures (up
to 550 ~ and high hydrogen pressures (up to 18 MPa). The
nominal compositions of these steels are 3Cr-1Mo-1Ni and
3Cr-l.5Mo-0.5Ni, with and without 0.2V. Based on evaluations on 55 kg heats the new steels are found to be superior
to 2.25Cr-lMo steel with respect to hardenability, room
temperature strength, impact toughness and resistance to
hydrogen attack, and to be similar with respect to room and
elevated temperature ductility, creep strength and rupture
ductility and temper embrittlement resistance. In addition,
their mechanical properties compare very favorably to the
recently developed 3Cr-1.5Mo-0.1V Climax Molybdenum
and 3Cr-lMo-0.25V, Ti, B Japan Steel Works steels, and
actually are somewhat superior to these steels with respect
to strength and toughness.

Fig. 2 1 - - C o m p a r i s o n of tensile strength of present experimental

3Cr-Mo-Ni alloys with 2.25Cr-lMo steel, 37'38 the Climax Molybdenum
3Cr-l.5Mo steels, ~9'2~ and the Japan Steel Works 3Cr-IMo-0.25V, Ti, B
steel. 24

ACKNOWLEDGMENTS
This work was supported by the Department of Energy,
Advanced Research and Development Fossil Energy Materials Program, through the Oak Ridge National Laboratory
(ORNL), under Subcontract 7843 with the University of
California, Berkeley, under Union Carbide Contract W7605-eng-26 with the U.S. Department of Energy. The authors would like to thank R.W. Swindeman of ORNL for
many helpful discussions, Dr. D. S. Sarma for transmission
electron microscopy assistance, and T. George, R.K. Anders, R. I. Huntley, and L. -H. Chan for experimental help.

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Fig. 22--Comparison of the tensile strength/toughness characteristics

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Climax Molybdenum 3Cr-l.5Mo steels, ~9'2~ and the Japan Steel Works
3Cr-IMo-0.25V, Ti, B steel, z4 Note lower ductile/brittle transition temperature implies higher toughness.
J. MATERIALS FOR ENERGY SYSTEMS

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