JOURNAL OF NUCLEAR MATERIALS 54 (1974) 55-63.

0 NORTH-HOLLAND PUBLISHING COMPANY

TIIE EFFECT OF CARBON ON 2.25 0-l MO STEEL

(II). Creep-rupture properties*

R.L. KLUEH
Metals and Ceramics Division, Oak Ridge National Laboratoiy, Oak Ridge, Tennessee 37830, USA

Received 15 April 1974

The creep-rupture properties of normalized-and-tempered 2.25 Cr-1 MO steel with 0.009, 0.030, 0.120, and 0.135 wt % C were
determined at 454,510, and 565C; the results show an effect of carbon that depends on temperature. At all three temperatures,
the 0.120 and 0.135 wt % C steels have similar strengths, and at 565C are considerably stronger than the 0.009 and 0.030 wt % C
steels, which also have similar strengths. At 454 and 5 lOC, however, the properties for the 0.030 wt % C steel are superior to
those of the 0.009 wt % C steel and approach those for the 0.120 and 0.135 wt % C steels. These observations can be explained
in terms of the type of carbide precipitation reactions that occur in 2.25 Cr-1 MO steel.

Les prop&t& de rupture par fluage dun acier a 2,25 Cr-1Mo normalise et revenu et contenant diverses teneurs en carbons
(0,009, 0,030, 0,120 et 0,135 en poids) ont et& determinees a454, 510 et 565C. Les resultats montrent que leffet du carbone
depend de la temperature. A ces trois temperatures, les aciers a 0,120 et 0,135% en poids C ont des resistances similaires et sont
beaucoup plus resistants a 565C que les aciers B 0,009 et 0,030% C qui ont aussi des resistances comparables. A 454 et SlOC,
cependant, les proprietds de lacier a 0,030% C sont superieures acelles de lacier h 0,009% C et approchent celIes des aciers a
0,120 et 0,135% C. Ces observations peuvent Btre expliquees en termes du type des r&actions de precipitation des carbures qui
se produisent dans lacier a 2,25% Cr-1% MO.

Die Zeitstandse~enschaften von norm~geg~dhtem und getempertem 2,25 Cr-1 MoStah mit 0,009, 0,030,0,120 und 0,135% C
wurden bei 454,510 und 565C untersucht; es wird ein temperaturabhlbrgiger Einfluss der Kohlenstoffs beobachtet. Bei allen
drei Temperaturen haben die Stable mit 0,120 und 0,135% C eine ahnliche Festigkeit, sie ist bei 565C wesentlich hoher als
fur die Stiihle mit 0,009 und 0,030% C, die ebenfalls eine ahnliche Festigkeit aufweisen. Bei 454 und 510C liegen die Eigen-
schaften des Stahls mit 0,030% C jedoch iiber denen des Stahls mit 0,009% C und n%hern sich denen der Stable mit 0,120 und
0,135% C. Diese Beobachtungen kijnnen mit dem Typ der Carbid-Ausscheidungsreaktionen, die im 2,25 Cr-1MoStahi auftreten,
erkl&rt werden.

1. In~oduction and usually at temperatures somewhat above those of

interest for the liquid-metal fast breeder reactor
In the preceding paper [l] we discussed the effect (LMFBR), where 2.25 Cr-1 MOsteel is being con-
of carbon content on the microstructure, hardness, sidered as a stearugenerator material. In the present
and tensile properties of 2.25 0-l MOsteel. In this work, no~~ized-Ed-tempered steels were studied at
paper, the creep-rupture properties of these same 454,510, and 565C.
materials will be considered. Previously reported
studies 12-71 on the effect of carbon on creep-rup
ture properties were on annealed** 2.25 Cr-1 MOsteel 2, Experimental

* Research sponsored by the US Atomic Energy Commission
under contract with Union Carbide Corporation,
** Throughout this report, the terms annealed and normalized
will be used in the context commonly used by steelmakers.
Annealed refers to a steel that has been austenitized by
holding the steel at a temperature above As, then slowly
cooled-usually a furnace oooI. Normalized refers to a
steel similarly heated, but cooled in air.
Creep rupture properties of 2.25 Cr-1 MOsteel
with 0.009,0.030,0.120, and 0.135 wt % C were
determined at 454,510, and 565C. The 0.009,0.030,
and 0.120 wt % C steels were obtained as 2.2 cm diam
rods and will be referred to as low-, medium-, and high-
carbon rods (the 0.120 wt % C steel is a remelted com-
mercial heat). The 0.135 wt %C steel was a 2.5 cm
56 R.L. Kb&?h, Effect of C&m or1 2.25 Cr-1 IWO steel (If)

commercial plate obtained from Babcock and Wilcox.
The tests were conducted on norm~ized-and-tempered
material: Austenitized I h at 927C then air-cooled;
tempered 1 h at 704C, then air-cooled. After this
heat treatment, the low- and medium-carbon steels
were primarily proeutectoid ferrite with 1 to 2 and 15
to 20% granular bainite, respectively. The other two
materials were entirely bainite. For further informa-
tion on the test materials, the reader is referred to the
preceding paper [ I J.
For the creep-rupture tests, specimens with a 0.25
in diam by 1.25 in long reduced section were used.
The tests were done in air on lever-arm creep frames
with 12 : 1 and 20 : 1 ratios; the specimens were
heated by a Marshall resistance furnace. During test
the temperature was monitored and controlled by
three chromel-alumel thermocouples attached along
the specimen gage section. Temperatures were con-
trolled to *I C, and the temperature varied less than
t3C along the gage length. Creep strains were mea-

ioo -

80

RUPTURE TlWlE (hr)

80

60

10-z to-
MINIMUM CREEP RATE (70 hr)
Fig. 1. Creep-rupture properties of normalized-and-tempered 2.25 O-1 MO steels at 454C. (a) Rupture life. (b) Minimum creep
rate.
 R.L. Kiueh, Effect of carbon on 2.25 0-l MOsteel (II} 57

sured with a mechanical extensometer attached to the
specimen shoulders, and the strain was read periodical-
ly on a dial gage with a sensitivity of 10B5 in.
3. Results
The creep-rupture curves along with minimum
creep rates as a function of stress are given in figs. 1, 2,
and 3 for 454,510, and 565C, respectively. At all
three temperatures, an increase in carbon content in-
creased the creep-rupture strength, though the refa-
tive differences between steels changed with tempera-
ture. This effect was noted for both the rupture and
minimum creep rate curves. In each case the creep-
rupture data for the low-carbon material fell signifi-
cantly below the data for the high-carbon rod and the
commercial steel plate. The medium-carbon rod ma-

100 T -

80

60
.&

w-

-I-

RUPTURE TIME fhr)

80

$0
to-4 10-3 i0-2 40-i iOO
MINIMUM CREEP RATE (%/Iv)
Fig. 2. Creep-rupture properties ofnormalized-and-tempered2.25 0-l MO steels at 510C. (a) Rupture life. fb) Minimum creep
rate.
terial, however, changed relative to the low- and high-
carbon data as the temperature changed.
When the three rod materials (0.009,0.030, and
0.120 wt % C) are compared at 454C, the creep-
rupture curve for the low-carbon steel falls consider-
ably below those of the other two. On the other hand,
when the curves for the medium- and high-carbon rod
materials are extrapolated beyond 1000 h, assuming
no curvature, we would expect the curves to intersect.
100
80
60
RUPTURE
MINIMUM
Fig. 3. Creep-rupture properties of normalized-and-tempered
rate.
A comparison of the 454C creep-rupture data from
this study with the data in Smiths IS] compilation on
the properties for commercial normalized-and-tem-
pered material shows that Smiths scatter-band (in-
cluding material quenched and tempered to less than
11.5000 psi ultimate tensile strength) is bounded at
the upper end by the high-carbon rod data and at the
lower end by the medium-carbon rod data.
At 5 10C, the creep-rupture curves (fig. 2) for the
(02
TIME (hr)
CREEP RATE f%,hr)
2.25 0-l MO steels at 565C. (a) Rupture life. (b) Minimum creep
 R.L. Klueh, Effect of carbon on 2.25 Cr-1 MOsteel (II) 59

medium- and high-carbon rod materials appear to cross decreased ductility, while that of the 0.030 wt % C
after several hundred hours and 43 000 psi. Consid- steel was slightly increased. For the two high-carbon
ering the limited amount of data taken, along with steels, the elongations and reductions in area for the
inherent scatter, it is probably more correct to say the high-ductility fractures generally exceeded 20 and 70%,
curves merge beyond this point. At this temperature, respectively; a slight increase with increasing tempera-
results for the medium- and high-carbon rods and ture was noted.
Smiths data agree quite well. Finally, comparison of
the three rods at 565C (fig. 3) shows that the creep-
rupture curve for the medium-carbon rod is displaced 4. Discussion
downward relative to the high-carbon rod. Now, the
properties of the medium- and low-carbon materials Fig. 4 compares the Larson-Miller curves (minus
approach each other. The data for the high-carbon rod data points) for all four test materials, and comparison
agree quite well with Smiths data [8]. of the curves verifies the qualitative conclusions pre-
The high-carbon rod (0.120 wt % C) and the com- viously drawn by comparing creep-rupture diagrams.
mercial plate (0.135 wt % C) show little difference in As indicated above, the creep-rupture strength of the
creep-rupture strengths at 454C and for long times medium-carbon steel approaches that of the high-
(low stress) at 5 10C. For shorter times (high stress) carbon steel for tests longer than 1000 h at the lower
at 510C and at all times and stresses at 565C the temperatures, and this is shown by the approach of
commercial plate has a slight strength advantage. the Larson-Miller curves for these materials for in-
At 565 and 510C the data for all four materials termediate parameter values (17 to 18.5). At high
indicate that the creep-rupture curves are nonlinear. stresses and low parameter values, the curves again
At 454C, however, with the exception of the low- deviate because the medium-carbon steel is limited by
carbon steel data, the creep-rupture curves appear the ultimate tensile strength (61000 psi at 454C).
linear. Similar observations on curvature appear to Since the solubility of carbon in ferrite is limited
apply to the respective minimum creep rate curves. It and probably above 0.009 wt %, the effects observed
must be cautioned that these conclusions are drawn are apparently inherent in the microstructures, that is,
from few data and apply only to times out to a few
thousand hours. T(V) (zo+log t) XIO-3
26 30 32 34 36
Curvature in creep-rupture curves often indicates a 100
change in fracture mode. However, only the 0.120 and
00
0.135 wt % C steels exhibited a change. At 565C,
both steels showed a reduced elongation and reduc-
60
tion in area for rupture times greater than 1000 h (the
0.135 wt % C steel showed reduced ductility after 362
h); the elongations decreased from about 23 to 15%
and the reduction in area from 85 to 35%. A similar
reduction in ductility was observed at 5 1OC for the
0.135 wt % C steel that ruptured after 1558 h. These
four low-ductility tests exhibited a flat fracture with-
out a neck and with a multitude of grain boundary 20
cracks parallel to the fracture surface.
For all tests on the 0.009 and 0.30 wt % C steels
and the majority of tests on the 0.120 and 0.135 wt
% C steels, the high-ductility fractures were of a cup- 1OOOhr 454oc
10 .
cone type. At 454 and 51OC, the 0.009 and 0.30 wt (5 16 17 16 19 20
% C steels had elongations and reductions in area of TPK) (2O+log ~)x!O-~
greater than 30 and 75%, respectively. At 565C, the Fig. 4. Comparisonof Larson-Miller parameter diagrams for
ductility of the 0.009 wt % C steel showed a slightly the four steels studied.
60 R.L. Klueh, Effect of carbon on 2.25 Cr-I
carbide precipitate as opposed to solution strength-
ening. ~thou~ we presently have no direct evidence
of the precipitation processes that occur in our mate-
rials, there is enough evidence available on the effects
of precipitates on creep and the types of precipitates
formed in commercial 2.25 Cr-1 MO steel [9-l I] to
qualitatively explain the observations of this study.
(Further electron microscopy of creep-tested speci-
mens is planned.) In fact, most of what we will discuss
has been stated earlier by Irvine et al. [lo] and Baker
and Nutting [9]. In our discussion we will attempt to
use and, where necessary, extend these ideas to ex-
plain the results of our observations on the effect of
carbon on CT-2 strength.
According to Irvine et al. [IO], possible creep-
strengthening mechanisms in steels include: solid-
solution hardening, grain size, precipitation hardening,
which involves coherent precipitates, and dispersion
hardening, which involves noncoherent precipitates.
Since it is assumed that the ferrite solid solutions are
the same for all four steels, solid-solution hardening
will not be discussed. Similarly, grain size will not be
discussed, although previous studies [lo] have shown
that grain size has little effect in ferritic steels. Since
we are not at present able to distinguish between co-
herent and noncoherent precipitates, we will discuss
the precipitation kinetics in terms of precipitate for-
mation, growth, and subsequent ripening and over-
aging.
In addition to our electron microscopy results [l]
that showed the formation of precipitates during tem-
pering, we also collected indirect evidence of precipi-
tation reactions 1121. When the low- and medium-
carbon steels were tempered for times longer than 1 h
at 704C, hardness peaks were observed - generally
between 1 and 10 h {longer times at lower tempera-
tures). For the ~~-carbon rod and commercial plate,
however, a continuous decrease in hardness was noted
(a hardness peak is noted during the first hour of tem-
pering at 593C). Such secondary hardness peaks are
indicative of precipitation reactions, and since the low-
and medium-carbon materials are primarily ferrite, the
reactions must be occurring in this phase.
As in every precipitation strengthening process, we
would expect an optimum precipitate size and density
for maximum strengthening, followed by Ostwald
ripening, which leads to overaging and subsequent loss
of the strengthe~ng effect. The lower the temperature,
MO steel (II)
the longer is the time before overaging, and in this
discussion, we will consider that overaging begins when
the strength has peaked. Furthermore, the precipitate
density and particle size before overaging will depend
on carbon content; that is, the greater the amount of
precipitate formed, the greater the precipitate density
at the optimum size. Our tempering results indicated
that the low- and medium-carbon normalized-and-
tempered steels are being strengthened during test,
while the high-carbon rod and commercial plate have
already passed their strength peaks 1121 as a result of
the 704C temper.
Of further interest for this discussion are the actual
precipitation reactions. It is known [9] in commercial
2.25 Cr-1 MO steel that the difference between the
reactions in bainite and ferrite gives rise to the type of
kinetic differences noted in our hardness studies [ 121.
Baker and Nutting [9] did tempering studies to ex-
plain the unexpected greater creep strength for nor-
malized-and-tempered over quenched-and-tempered
2.25 Cr-1 MO steel. Their normalized-and-tempered
material contained considerable proeutectoid ferrite
(large section sizes were normalized), while their
quenched-and-tempered steel was primarily bainite.
~~0~~ M6C finally formed in each constituent,
Baker and Nutting f9] found different carbide reac-
tions (with different kinetics) intermediate to its for-
mation. In the bainite, the first carbide to form on
tempering was cementite, which subsequently changed
to Mo,C and Cr7C3, followed by changes to MZ3C6
and M6C. They wrote the following reactions to de-
scribe their observations:
Cementite -+ Cementite - Cr 7 C 3
+ \ 4 (1)
Mo,C i -j M,,C, + M,C.
In ferrite, on the other hand, the first precipitate to
form was Mo2C, which subsequently transformed to
Me C without the various intermediate carbides:
Mo2C-+M6C. (2)
According to Baker and Nutting [9], only the Mo,C
greatly enhances the creep strength of 2.25 Cr-1 MO
steel. In the bait&e, however, globular MZ3C6 forms
at the expense of the Mo,C and has little effect on
strength. As a result of the rapidity of this intermediate
reaction, the Mo,C in the bainite disappears much
 R.L. Klueh, Effect of carbon on 2.25 0-I IWOsteel (II) 61

sooner than it does in the ferrite. Hence, Baker and T (R) (20 + log 1) x to-3
Nutting [9] concluded that the differences in the rates 28 30 32 34 36
ioo
of reactions in the two constituents explained the
more rapid loss of strength for the quenched-and- 80

tempered (primarily bainite) steel and eventual

strength advantage for the normalized-and-tempered
(primarily proeutectoid ferrite) steel.
With the above general discussion in mind, we shall
examine some of our experimental observations on
creep-rupture strength and attempt to relate these to
the precipitation reactions known to occur in these
materials. The strength advantage for the medium-
carbon steel over the low-carbon steel at 454 and
5 10C is evidently a reflection of the larger amount of
carbide precipitate capable of being formed in this
steel (this assumes that the 15 to 20% bainite in the
microstructure is not contributing significantly to the
strength). At all temperatures, the curves should even-
tually approach one another. Since the rate of precip-
itate growth increases with temperature, the merging
of strengths proceeds more rapidly the higher the tem-
perature. As pointed out previously, the curves for
these two steels do approach each other at 565C.
We previously noted that, with the exception of
the high-carbon rod and the commercial plate at
565C no correlation between the curvilinearity of
the creep-rupture curves and the fracture mode could
be made. Such cu~~inearity could be the result of
precipitate formation and growth. That is, strength
drops off more rapidly with time than a linear extra-
polation because of precipitate growth and overaging.
Such an explanation agrees with the observed change
in curvature with temperature. The curves for the low-
carbon steel, which forms the least amount of precipi-
tate and thus overages most rapidly, shows curvature
at all temperatures. On the other hand, the higher
carbon materials form a larger density of precipitates
that require a longer growth period before overaging;
thus, they do not show curvature at 454C over the
time period of our tests, but do at the higher tempera-
tures.
Possibly the most interesting observation is the in-
tersection of the creep-rupture curves for the medium-
and high-carbon steels at 5 10 and 454C (extrapolated).
For these results an explanation similar to that pro-
posed by Baker and Nutting [9] is possible. In the me-
dium-carbon steel, which is primarily ferrite, the Mo,C
precipitate provides strength over a longer period of
60
8
6
*C
2
21
15 t6 17 (8 19 20
P=7-(K) (20 + log ,) X to-
Fig. 5. Comparison of Larson-MiUer diagrams determined in
this study with those in other studies, Curves for annealed
material are from Smith [ 81, Sponseiler et al. [ 21,and Seeley
and Zeisloft [4].
time [the difference is in the rates of reactions (1) and
(2)]. Since we would eventually expect the medium-
carbon steel to overage, the creep-rupture curves may
once again deviate (before finally merging at equilibri-
um), When (and if) this deviation occurs cannot be
predicted without more long-time tests.
In fig_5, the average Larson-Miller curve for an-
nealed commercial 2.25 Cr-1 MOsteel, taken from
Smith f8], was added to the curves of fig. 4 (since the
curve for the 0.120 wt % C steel was similar to that for
the 0.135 wt % C steel, only the latter is shown).
Smith [8] has no Larson-Miller curve for normalized-
and-tempered commercial 2.25 Cr-1 MOsteel, but
since the 0.135 wt % C steel agreed quite well with
Smiths limited data, this curve should suffice for re-
presenting this material. Also shown in fig. 5 are curves
taken from Sponseller et al. [2] for 0.01 and 0.042
62 R.L. Klueh, Efyect of carbon on 2.25 0-f
wt % C, and from Seeley and Zeisloft [4] for 0.02 wt
% C, all three materials in the annealed condition. At
low parameter values our curve for the 0.009 wt % C
steel and the three curves taken from the other studies
are about the same as the average of the annealed com-
mercial steel; our curve for the 0.030 wt % C steei is
significantly above the average.
During the furnace cool (the anneal), the times
involved are probably not sufficient to allow signifi-
cant amounts of diffusion by substitutional atoms
(molybdenum and chromium). Therefore, the globular
carbides precipitated in the ferrite (independent of the
pearlite) during the anneal are mainly cementite
(M3C), which contains chromium and molybdenum
in proportions similar to those in the steel. On pro-
longed exposure at the test temperatures, however,
substitutions diffusion becomes possible and the pre-
cipitation of the more stable MozC within the ferrite
ensues and leads to the same sequence of events ob-
served for the normalized-and-tempered steel:
strengthening, overaging, then disappearing by eventu-
al conversion to Me C.
Assuming that this sequence of events occurs, then
the relative placement and trends of the curves in fig.
5 follow. Since the large amounts of initially formed
globular or pearlitic carbides in the commercial ma-
terial add little to the creep strength, the small differ-
ence at low parameter values between our low-carbon
rod, the annealed low-carbon steels from the other
studies [2,4], and Smiths average curve results be-
cause the strength is primarily determined by the
strength of ferrite. At these temperatures, the precipi-
tation is relatively slow; thus, precipitation strength-
ening by MoZC plays no role. Only for long-time tests
at these temperatures will the differences caused by
precipitation become evident (greater than the several
thousand hours of the tests under discussion) [2,4].
The greater strength of the normalized-and-tempered
0.030 wt % C steel at the low temperatures (above
that for the 0.042 wt % C steel and the average curve)
is the result of precipitation of Mo,C that began
during tempering.
At high parameter values (fig. 5), we see that the
curves for the normalized-and-tempered 0.030 wt % C
steel and the annealed 0.042 wt % C steel of Sponseller
et al. 123 cross, now giving the strength advantage to
the annealed steel. In this case, the strength advantage
gained at low values as a result of the tempering that
MO steel [II}
started the Mo,C precipitation leads to a more rapid
overage, and thus lower creep-rupture strengths (i.e.
essentially all of the precipitation reaction in the an-
nealed material occurs during test). Also, at high pa-
rameter values the curve for the hip-carbon normal-
ized-and-tempered steel crosses the average curve for
annealed material, a result that agrees with work by
Krisch and Naumann [ 131 and Yukitoskhi and
Nishida [6] who showed that for long-time tests in the
range 500 to 6OOC, the creep-rupture curves for nor-
m~ized-and-tempered and annealed 2.25 Cr- 1 MO
steels cross, with the strength of the annealed steel
becoming greater than that of the normalized-and-
tempered material. The initial 1 h temper, along with
the much slower disappearance of MoZC in ferrite
than in bainite, explains such a crossover.
Regardless of the initial carbon content (above
ferrite saturation) and microstructure (determined by
heat treatment), ultimately the 2.25 Cr-1 MO steels
will approach a microstructure consisting of a carbon-
saturated ferrite matrix containing spheroidized
carbide coarsened to such an extent that it has little
or no effect on the creep strength. When this point is
reached, the strength will be determined almost entire-
ly by the ferrite and, because of the limited solubility
of carbon in ferrite, the strength should not depend
on the original carbon content. When this occurs will
depend greatly on temperature (i.e. if the temperature
is low enough, the strength will change very little) and
the original carbon content. As an indication that the
above conclusion is correct, we cite the work of
Sponseller et al. [2]. An extrapolation of their 649C
creep-rupture data - their highest temperature is
considerably higher. than an LMFBR steam generator
- shows that beyond several thousand hours the
creep-rupture curve for annealed commercial steel
approaches that for an annealed steel with 0.042 wt %
C. Because of the lowered rates, the time scale over
which this occurs at lower temperatures will be ex-
panded .
Finally, a word is in order on the effect of precipi-
tation on solid solution strengthening. As a result of
the formation of the globular M,3C6 and M,C during
long-time exposure at elevated temperatures, large
amounts of Cr and MO may be removed from solid
solution. For binary iron alloys, Austin et al. [ 141
have shown that MO is by far the most effective ele-
ment in its ability to impart solid solution strength-
 R.L. Klueh, Effect of carbon on 2.25 Cr-I MO steel (II)
ening (the effect of Cr above 0.75 wt % is minimal).
In the limit of long times at the elevated temperatures,
therefore, the solid solution strengthening afforded by
MOmay eventually give the strength advantage to the
lower carbon material, since it will lose less MOby
carbide formation.
Acknowledgments
The author gratefully acknowledges C.W. Walker
and J.L. Griffith, Jr., for carrying out the experimen-
tal work; C.E. Zachary for the metallography; J.O.
Stiegler for the electron microscopy; P.L. Rittenhouse,
S. Peterson, D.A. Canonico, and W.R. Martin for re-
viewing the manuscript; and Bette Thomas for pre-
paring the manuscript. Discussions with W.R. Martin
and D.A. Canonico throughout this work were most
helpful and are greatly appreciated.
References
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[ 2) D.L. SponseIIer, M. Semchyshen and P.J. Grobner, in:
63
Low Carbon and Stabilized 2 l/4 Cr-1 MO Steel (Amer-
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[3] A.A. Bauer, ibid.,p. 113.
[4] R.R. Seeley and R,H. ZejsIoft, ibid., p. 37.
[5] T. Yukitoshi and Y. Nishida, Proc. Extension Semin.
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[lo] K.J. Irvine, J.D. Murray and F.B. Pickering, Structural
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[ 121 R.L. Klueh, unpublished research.
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