LarsonMiller correlation for the effect of thermal ageing on the yield

strength of a cold worked 15Cr15NiTi modied austenitic stainless steel

K.G. Samuel
*
, S.K. Ray
Materials Technology Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, India
Received 11 November 2005; received in revised form 16 February 2006; accepted 20 February 2006
Abstract
For 20% cold worked 15Cr15NiTi modied austenitic stainless steel (Alloy D9), the LarsonMiller parameter can be used to describe the
effects of prior thermal exposures to different timetemperature combinations on the 0.2% yield stress s
YS
, ultimate strength and total elongation
in subsequent tensile tests at 300, 723 and 923 K. A single master plot for all the tensile test temperatures was obtained by plotting the Larson
Miller parameter against the ratio S
YS
Z(s
YS
of thermally aged material)/(s
YS
of un-aged material) at identical tensile testing temperature.
q 2006 Elsevier Ltd. All rights reserved.
Keywords: Ti modied austenitic stainless steel; Cold work; Thermal ageing; LarsonMiller parameter
1. Introduction
The LarsonMiller parameter, PZT(log
10
tCC), where T is
the absolute temperature, t the time and C a constant, had its
origin in the tempering studies of Hollomon and Jaffe [1]. This
parameter continues to be widely used for correlation of stress
rupture data of various engineering materials [2,3]. The
LarsonMiller parametric correlation has also been used for
hardness and notch toughness of 2.25Cr1Mo steel [4], the
inuence of ageing on the hardness of cold-worked austenitic
stainless steel [5] and carbon concentration proles in Alloy
800H/2.25Cr1Mo steel joints welded with Inconel 82
consumables [6].
Titanium modied 15Cr15Ni austenitic stainless steel
(Alloy D9) is chosen for the hexagonal wrapper for fuel
subassemblies of fast breeder reactors [7]. This material is
generally used in a 20% prior cold worked condition, and there
is an interest in assessing the inuence of elevated temperature
service exposure on the tensile deformation behaviour,
specically the 0.2% yield stress s
YS
, ultimate strength and
total elongation. Vasudevan et al. [8] have extensively studied
the recovery and recrystallization behaviour on static thermal
ageing 20% cold worked 15Cr15Ni2.2MoTi modied
austenitic steel with various Ti/C ratios, using optical
metallography, and room temperature hardness measurements
and tension tests. They showed that recrystallization during
prior static ageing leads to drastic decreases in hardness and
strength values with corresponding increase in the elongation.
The recrystallization temperature was found to be w973 K,
considerably accelerated as ageing temperature increased, and
depended on the Ti/C ratio. Metallographic observations [8]
indicated the presence of grain boundary precipitates in the
thermally aged alloys. In cold worked and thermally aged steel
of this type, grain boundary precipitates of the type M
23
C
6
and
MC have been reported [9,10]. In this paper, it is shown that the
LarsonMiller parameter can be used to describe the effects of
static thermal exposure of 20% cold worked Alloy D9 on the
subsequent tensile properties at 300, 723 and 923 K.
2. Experimental
The dimensions of the hexagonal wrapper tube are
131.3 mm wide across at faces and 3.2 mm thickness. The
chemical composition (wt%) of the material investigated was
C: 0.045, Cr: 13.88, Ni: 15.24, Mo: 2.12, Ti: 0.23, B: 12 ppm,
Mn: 2.12, Si: 0.64, Cu: 0.017, As: 0.0019, N: 0.0021, Al: 0.01,
Co: 0.007, S:!0.005, P:!0.005, Nb:!0.005, V:!0.01,
Ta:!0.01. The tubes were procured in the 20G4% cold
worked condition. Tensile specimen blanks were cut from the
at faces of the wrapper tube in the axial direction and given an
isothermal ageing treatment at a temperature in the range
8231123 K for various durations up to 10,000 h, and then
quenched in water to retain the microstructure developed
International Journal of Pressure Vessels and Piping 83 (2006) 405408
www.elsevier.com/locate/ijpvp
0308-0161/$ - see front matter q 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijpvp.2006.02.032
* Corresponding author.
E-mail address: samuel@igcar.gov.in (K.G. Samuel).
during ageing. In all, 32 ageing conditions (Table 1) were used
in this study. Flat tensile specimens having 25 mm gauge
length and 4 mm gauge width were machined from the unaged
as well as aged blanks.
Isothermal tensile tests were carried out in a universal
testing machine at a constant cross head speed of 2 mm/min
(nominal strain rateZ1.33!10
K3
s
K1
). The load and elonga-
tion were recorded using the chart drive attached
to the machine. The elevated temperature was controlled
within G2 K over the gauge length using a three zone
resistance-heating furnace. Prior cold worked (PCW) and prior
cold worked and aged (PCWA) specimens were tested at 300,
723 and 923 K.
3. Results and discussion
The typical true stress strain curves for the aged materials
are compared with that of the as received material in Fig. 1. It is
observed that particularly higher ageing temperatures and
longer durations lead to substantial changes in strength and
ductility, reecting changes in microstructure during static
thermal ageing. The average values (from a minimum of two
tests) of s
YS
of the cold worked material as a function of ageing
conditions and test temperature are shown in Table 1. The
combined effects of thermal ageing is sought to be expressed
using the LarsonMiller parameter
P ZT
A
log
10
t
a
CC (1)
where T
A
(in K) and t
a
(in h), are, respectively, ageing
temperature and duration and C, a constant to be determined.
Using this parameter, the dependence of s
YS
(in MPa) on prior
thermal ageing could be expressed using a polynomial of
degree 3:
s
YS
Za
0
Ca
1
PCa
2
P
2
Ca
3
P
3
(2)
The degree of the polynomial was xed as optimal by trial
and error. For a xed value of C, the polynomial coefcients in
Eq. (2) were determined from a least squares t. The value of
the constant C was varied to identify the polynomial t that
gave the highest correlation coefcient R. The variations of the
correlation coefcient R with the LarsonMiller parameter
constant C are shown in Fig. 2. The C value corresponding to
the highest correlation coefcient was found to be 13,
independent of the tensile test temperature. The optimal values
for the constants in Eq. (2) thus determined are shown in
Table 2.
The variation of s
YS
with P for the three tensile test
temperatures is shown in Fig. 3; the rm lines in this gure
represent the optimal ts to Eq. (2). As this gure shows, a
separate correlation is obtained for each of the tensile test
temperatures, although with very similar trends in variation of
s
YS
with P: initially a slight increase, followed by a rapid
decrease, followed by a trend to saturation at large P values.
Table 1
Yield strength s
YS
a
of 20% prior cold worked Alloy D9 after thermal ageing
Ageing
time (h)
Aged at 823 K Aged at 923 K Aged at 1023 K Aged at 1123 K
300 K 723 K 923 K 300 K 723 K 923 K 300 K 723 K 923 K 300 K 723 K 923 K
10 651 623 520 646 553 517 614 473 445 508 402 384
50 707 563 525 720 574 510 588 494 425 399 323 307
100 666 588 491 727 560 545 565 443 416 390 235 197
500 685 543 474 663 517 473 471 368 357 257 200 167
1000 722 547 473 614 473 445 524 401 376 236 163 141
2000 718 562 485 588 494 425 429 323 302 237 161 142
5000 659 529 469 534 422 369 353 290 277 231 179 149
10,000 648 496 469 501 397 370 321 267 235 224 159 142
a
s
YS
values in MPa.
8 10 12 14 16 18 20 22 24 26
0.90
0.91
0.92
0.93
0.94
0.95
0.96
0.97
0.98
TEST
TEMPERATURE
923 K
723 K
300 K
C
O
R
R
E
L
A
T
I
O
N

C
O
E
F
F
I
C
I
E
N
T
,

R
L-M PARAMETER CONSTANT, C
Fig. 2. Variation of correlation coefcient for t with Eq. (1) as a function of
LarsonMiller parameter constant C at various test temperatures.
0.00 0.05 0.10 0.15 0.20 0.25
100
200
300
400
500
600
700
800
900
1000
Test
Temperature
Ageing Condition
Temperature/Time
A 300 K 20% Prior Cold Worked (PCW)
B 300 K PCW + 823 K/10 hours
C 923 K 20% Prior Cold Worked (PCW)
D 923 K PCW + 1123 K/2000 hours
D
C
B
A
T
R
U
E

S
T
R
E
S
S
,

M
P
a
TRUE PLASTIC STRAIN
Fig. 1. Typical stressstrain curves of Ti modied austenitic stainless steel in
cold worked and subsequent thermal ageing conditions at 300 and 923 K.
K.G. Samuel, S.K. Ray / International Journal of Pressure Vessels and Piping 83 (2006) 405408 406
A similar trend has been observed by Vasudevan et al. [5] in
their study on the dependence of hardness of prior cold worked
D9 alloy subjected to prior thermal ageing using the Larson
Miller parametric approach. The slight initial increase in s
YS
with P might be attributed to precipitation of TiC during
ageing. Kesternich and Meertens [11] have reported that ne
homogenous dispersions of TiC were obtained in a 20% cold
worked Ti stabilized 15Cr15Ni austenitic stainless steel on
ageing at 923 K. The decrease in s
YS
at higher P values reects
the recovery and possibly recrystallization of the initial cold
worked structure during thermal ageing.
s
YS
depends both upon the microstructure developed during
the prior thermal ageing, and also the temperature (and strain
rate) for the tensile test. However, it may be possible to index
the microstructure variation using a structure sensitive yield
strength ratio S
YS
dened as
S
YS
Zs
YS
for aged material=s
YS
for unaged material (3)
at an identical tensile test temperature (and strain rate). For a
Type 316 stainless steel Samuel et al. [12] showed the viability
of this yield strength ratio, and also the ratio of tensile ductility
dened in an analogous manner, for indexing the effects of
prior cold work in various modes of deformation.
Fig. 4 shows the plots of S
YS
with P, which follows the same
three-stage pattern observed for each tensile test temperature in
Fig. 3. The optimal correlation between S
YS
and P was
determined in the manner described above, as:
S
YS
ZK14:636C0:0031PK2:615!10
K7
P
2
C4:096!10
K12
P
3
(4)
Here too, the optimal value for C was determined to be 13.
The possibility of generating master curves such as Eq. (4)
for ultimate tensile strength ratio, S
UTS
and total elongation
ratio, S
TE
dened in analogous ways to Eq. (3) was explored.
The results for these analyses are shown in Figs. 5 and 6,
respectively. Clearly, T
A
and t
a
can be combined using the
LarsonMiller parametric approach to describe the effects of
prior thermal ageing on ultimate tensile strength s
UTS
and total
elongation TE. The optimal values for the corresponding
10000 11000 12000 13000 14000 15000 16000 17000 18000 19000 20000
100
200
300
400
500
600
700
800
Y
I
E
L
D

S
T
R
E
N
G
T
H
,

M
P
a
P = T
A
[log
10
(t
a
/h) + 13]
Tension Test Temperature
300 K
723 K
923 K
Fig. 3. Variation of yield strength with LarsonMiller parameter at various test
temperatures.
11000 12000 13000 14000 15000 16000 17000 18000 19000 20000
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
1.1
1.2 Tension Test Temperature
300 K
723 K
923 K
Y
I
E
L
D

S
T
R
E
N
G
T
H

R
A
T
I
O
,

S
Y
S
P = T
A
[Log(t
a
/h) + 13]
Fig. 4. Variation of yield strength ratio with LarsonMiller parameter at various
test temperatures.
10000 12000 14000 16000 18000 20000 22000 24000 26000 28000 30000
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
2.6
2.8
3.0
3.2
Test Temperature C
300 K 18
723 K 22
923 K 12
T
E
N
S
I
L
E

D
U
C
T
I
L
I
T
Y

R
A
T
I
O
,

S
T
E
P = T
A
[Log(t
a
/h) + C]
Fig. 6. Variation of tensile ductility ratio with LarsonMiller parameter at
various test temperatures.
10000 12000 14000 16000 18000 20000 22000 24000 26000
0.55
0.60
0.65
0.70
0.75
0.80
0.85
0.90
0.95
1.00
1.05
1.10
1.15
1.20
Test Temperature C
300 K 18
723 K 12
923 K 12
T
E
N
S
I
L
E

S
T
R
E
N
G
T
H

R
A
T
I
O
,

S
U
T
S
P = T
A
[Log(t
a
/h) + C]
Fig. 5. Variation of tensile strength ratio with LarsonMiller parameter at
various test temperatures.
Table 2
Polynomial constants in Eq. (2) for the ts to s
YS
data in Fig. 3
Test
temperature
(K)
Polynomial constants
a
0
a
1
a
2
a
3
300 K13160.076 2.749 K1.765!10
K4
3.622!10
K9
723 K5796.868 1.303 K8.494!10
K5
1.778!10
K9
923 K6711.446 1.434 K9.133!10
K5
1.830!10
K9
K.G. Samuel, S.K. Ray / International Journal of Pressure Vessels and Piping 83 (2006) 405408 407
constants are given in Tables 3 and 4. However, master plots
using S
UTS
or S
TE
could not be obtained. It may be noted that
the result for S
TE
(Fig. 6) is in contrast to that of Samuel et al.
[12] for cold worked SS 316. It is, however, interesting to note
that the S
UTS
data for 723 and 923 K apparently can be
considered to belong to a single band (Fig. 5), while S
TE
data
for 300 and 723 K seem to belong to a single band (Fig. 6).
These trends could actually be anticipated from the
corresponding optimal values for C, Tables 3 and 4 and
Figs. 5 and 6. The mechanistic reasons for these observations
are not clear. s
YS
depends upon the initial microstructure and
therefore the parameter S
YS
is successful in indexing the
microstructure developed after the static ageing. Tensile
deformation apparently results in signicant modulation
of deformation and damage substructure. These modulations
determine s
UTS
and TE, but are not reected in P, and
therefore S
UTS
and S
TE
cannot be used to index the
microstructure. Differences in the observed dependences of
S
UTS
KP and S
TE
KP relations (Figs. 5 and 6) however suggest
that a single parametric formulation would not succeed for both
S
UTS
and S
TE
. More detailed modelling is needed to sort out
this issue.
4. Conclusions
1. Variation of the 0.2% yield strength of a 20% prior cold
worked Alloy D9 at 300923 K after static thermal
ageing for t
a
hours at temperature of T
A
(t
a
%10
4
h,
823%T
A
%1123 K) could be adequately described by the
LarsonMiller parameter, PZT
A
(log
10
t
a
CC), with the
optimal value of C as 13.
2. For tensile tests at 300, 723 and 923 K, a master curve,
independent of tensile test temperature, is obtained when
the ratio of the yield strengths of the aged and unaged
materials at identical test temperature is plotted against the
LarsonMiller parameter dened. It is concluded that this
ratio quantitatively indexes the microstructure at the start of
the tensile test. For this correlation too, the optimal value of
C is 13.
3. The LarsonMiller parameter correlation adequately
described the effect of prior thermal ageing on both
ultimate strength and total elongation in the subsequent
tensile tests at 300, 723 and 923 K. However, correspond-
ing ratios failed to yield master curves independent of
tensile test temperature.
References
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1

4
Cr1 Mo steel due to
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Table 4
Polynomial constants in Eq. (2) for the ts to T
E
data
Test
temperature
(K)
Polynomial constants
a
0
a
1
a
2
a
3
300 595.962 K0.074 3.032!10
K6
K3.612!10
K11
723 K271.965 0.042 K2.081!10
K6
3.425!10
K11
923 5.898 0.006 K8.498!10
K7
3.668!10
K11
Table 3
Polynomial constants in Eq. (2) for the ts to s
UTS
data
Test
temperature
(K)
Polynomial constants
a
0
a
1
a
2
a
3
300 K7805.158 1.268 K6.065!10
K5
9.308!10
K10
723 K1136.072 0.437 K3.307!10
K5
7.476!10
K10
923 K5534.991 1.342 K9.602!10
K5
2.199!10
K9
K.G. Samuel, S.K. Ray / International Journal of Pressure Vessels and Piping 83 (2006) 405408 408