Engineering Fracture Mechanics xxx (2017) xxx–xxx

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Engineering Fracture Mechanics

journal homepage: www.elsevier.com/locate/engfracmech

Effects of long-time service at high temperature on the material

strength and J-R curve of Grade 91 steel
Hyeong-Yeon Lee ⇑, Dong-Won Lim, Ji-Young Jeong
Korea Atomic Energy Research Institute, 989-111 Daedeok-daero, Yuseong-gu, Daejeon 34057, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history: The effects of long-time service at high temperature on the material strength, ductility, and
Received 6 July 2016 J-Resistance behavior of Mod.9Cr-1Mo (ASME Grade 91) steel were investigated based on
Received in revised form 27 January 2017 tensile and J-R tests with virgin and service-exposed Gr.91 steel specimens. The service-
Accepted 24 February 2017
exposed Gr.91 steel specimens were sampled from a tee junction in a reheat steam piping
Available online xxxx
system of an ultra-supercritical (USC) plant in Korea with an accumulated operation time
of 73,716 h. Comparisons of the test data were made not only between the test results of
Keywords:
the virgin materials and service-exposed materials but also between the test results and
Long-time service
Grade 91 steel
the material properties in the elevated temperature design (ETD) codes. These test data
Yield strength of yield strength (YS) and tensile strength (TS) for the virgin and service-exposed Gr.91
Tensile strength steel were compared with those of the ETD code, which showed that the current ETD code
Ductility overestimates the YS and TS properties for long-time service in a non-conservative manner
J-R curve for Gr.91 steel. J-R test data currently not available in ETD codes were produced over a
Thermal aging range of temperatures for virgin and service-exposed Gr.91 steel. The effects of long-
time service in J-R curve were investigated.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction

The influence of long-time service at high temperature has recently been an important issue in high-temperature com-
ponents of Generation IV (hereafter Gen IV) nuclear reactor systems [1,2] and ultra-supercritical (USC) plants operating
under a creep regime because the degree of actual degradation in service-exposed materials has been found to be more sev-
ere than generally anticipated, especially for Grade 91 steel [2–4].
The target design lifetime of a Gen IV reactor system is 60 years or more. It is generally known that the material strength
and fracture toughness in such systems tend to degrade as the operation time accumulates. However, the elevated temper-
ature design (ETD) codes [5–8] do not fully address the material degradation issues. Currently, ASME Section III Subsection
NH [5] (ASME-NH) takes long-time service effects into account only regarding yield strength and tensile strength, while RCC-
MRx considers thermal aging with thermal aging coefficients but most of the coefficients are left blank.

Abbreviations: ASME-NH, ASME Section III Division 1 Subsection NH; CCG, creep crack growth; DHX, decay heat exchanger; ETD, elevated temperature
design; FHX, forced-draft sodium-to-air heat exchanger; Gen IV, generation IV; Gr.91, Grade 91; J-R, J-integral Resistance; LBB, Leak Before Break; SFR,
Sodium-cooled Fast Reactor; SG, Steam Generator; TS, Tensile Strength; USC, Ultra Super Critical; YS, Yield Strength.
⇑ Corresponding author.
E-mail address: hylee@kaeri.re.kr (H.-Y. Lee).

http://dx.doi.org/10.1016/j.engfracmech.2017.02.022
0013-7944/Ó 2017 Elsevier Ltd. All rights reserved.

Please cite this article in press as: Lee H-Y et al. Effects of long-time service at high temperature on the material strength and J-R curve of
Grade 91 steel. Engng Fract Mech (2017), http://dx.doi.org/10.1016/j.engfracmech.2017.02.022
2 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx

The effects of long-time service on the yield strength (YS), tensile strength (TS), ductility, and fracture behavior of Gr. 91
steel were investigated in this study to quantify the degradation of the material in terms of material strength and J-R prop-
erties based on a series of material test results from virgin and service-exposed Gr.91 steel. Service-exposed Gr.91 steel
materials sampled from a reheat steam piping system of an ultra-supercritical plant with an accumulated operation of
73,716 h were used for the material testing. The test results of the service-exposed Gr.91 steel were compared with those
of virgin Gr.91 steel, and the test data were compared with those of the ETD codes [5,7–9].

2. Grade 91 steel before and after long-time service

2.1. Virgin Gr. 91 steel

Mod.9Cr-1Mo (ASME Grade 91) steel is a promising material candidate for the main components in sodium-cooled fast
reactors [1]. Gr.91 steel is a ferritic-martensitic heat resistant steel and one of the two main materials with austenitic stain-
less steel 316 to be used in Korean Gen IV SFRs [1].
Gr.91 steel has a lower thermal expansion coefficient and higher thermal conductivity than austenitic stainless steel 316.
The thermal conductivity of Gr.91 steel is higher by a maximum of 36.9% at 100 °C and 21.2% at 550 °C, while the thermal
expansion coefficient of Gr.91 steel is lower by a maximum of 51.3% at 250 °C and 48.8% at 550 °C in comparison with those
of austenitic 316 stainless steel [4] so that less thermal stress and more efficient heat transfer can be expected when Gr.91
steel is used in heat exchangers. However, there is a concern about the so-called Type IV cracking at welded joints in Gr.91
steel and careful post weld heat treatment at the welded joint is required [10–14]. The microstructures of Gr.91 steel are
relatively unstable.
The chemical compositions of Gr.91 steels in the ETD codes [15,16] for Gr.91 steel plate, forged Gr.91(F91) steel in the
ASME code, unexposed original Gr.91 steel, and the KAERI virgin plate used for fabrication of the material specimens in
the present study are given in Table 1. As shown in Table 1, the RCC-MRx code restricts the carbon range more strictly,
and a higher carbon from 0.06 to 0.08 would improve the creep strength, and decreasing the upper limit from 0.15 to
0.12 would increase the microstructure stability by the suppression of carbide coarsening and undesirable phase formation
[17]. The service-exposed Gr.91 steel was sampled from a tee fitting of forged Gr.91 (F91) steel in a USC plant. The chemical
compositions were within the range of ASME F91 as shown in Table 1.
In the present study, virgin Gr.91 steel material specimens were made with the ‘KAERI virgin plate’ rather than the ‘un-
exposed original’ Gr.91 steel in Table 1, which is not from the same heat of the service-exposed Gr.91 steel. It should be ideal
to use the same heat material with the unexposed original Gr.91 steel in material testing. In reality, however, it is hard to
secure the original material and even the mill sheet because it is either confidential or impossible to obtain. It is expected
that the differences in the chemical compositions of the original batch and KAERI’s batch might not result in big differences
in the tensile strengths and J-R curves.
In previous study [18], ductility of Gr.91 steel has been reported minimum at 400 °C in a range of temperatures from
room temperature to 700 °C. Since ductility minimum at a certain temperature may result in weak fracture toughness, J-
R tests over a range of temperatures from room temperature to 600 °C were carried out to investigate the J-R behavior
around 400 °C in this study.

2.2. Long-time service-exposed Gr.91 steel

It is known that Gr.91 steel degrades more severely under long-time service at high temperature compared with auste-
nitic stainless steel 316 [2]. Thus, the effects of thermal aging were investigated, and a comparison was made regarding the
strength reduction factors from long-time service in the ASME-NH [5].

Table 1
Chemical compositions of Grade 91 steel (wt.%).

Code/test C Mn P S Si Ni Cr Mo V Al Others
ASME 0.06–0.15 0.25– 0.025 0.012 0.18– 0.43 7.90– 0.80– 0.025– 0.02
(Gr.91 plate) 0.66 0.56 9.60 1.10 0.08
RCC-MRx 0.08– 0.30–0.60 0.02 0.005 0.20–0.50 0.20 8.00– 0.85– 0.03–0.07 0.04 Nb 0.06–0.10
(Gr.91 plate) 0.120 9.50 1.05
ASME (F91) 0.08–0.12 0.3–0.6 0.025 0.025 0.2–0.5 0.4 8.0–9.5 0.85– 0.18–0.25 Al 0.02 Nb 0.03–0.07
max max max 1.05
Ti 0.01
Zr 0.01
Unexposed, 0.08 0.38 0.018 0.003 0.34 0.29 8.75 0.875 0.242 0.014 Nb 0.079
original (Gr.91)
KAERI Virgin 0.115 0.415 0.012 0.0014 0.23 0.22 8.9 0.869 0.0513 0.014 Nb 0.079
plate (Gr.91)
N 0.038

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 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx 3

Thermally aged Gr.91 steel was used to investigate the long-time service effects and to quantify the conservatism of the
material strength properties in the ETD codes. The service-exposed Gr.91 steel was sampled from a tee junction in the reheat
steam piping system of a USC thermal power plant in Korea with an accumulated operation time of 73,716 h (8.4 years).
The images of the tee fitting and sampled plate are shown in Fig. 1. The forged tee fitting had an inner diameter of 760 mm
and a thickness of 27 mm. The design temperature and pressure of the piping system were 574 °C and 0.54 MPa, respec-
tively, while the operating temperature and operating pressure were 569 °C and 4.67 MPa, respectively.

2.3. Stress analysis results for the reheat steam piping

Piping stress analysis was conducted for the USC reheat steam piping system to check the stress level at the tee junction
part that was sampled for the present study. The maximum stress intensity at the tee fitting under pressure and thermal
loading under normal operating conditions was 79.1 MPa according to finite element analysis, which is not a high stress level
under combined thermal and mechanical loads.

2.4. Microstructural analysis

Investigation of microstructural evolution was conducted for virgin Gr.91 steel and service-exposed Gr.91 steel to quan-
tify microstructural changes during long-term service at high temperature.
Fig. 2 shows microstructural images obtained by transmission electron microscope (TEM) of virgin Gr.91 and service-
exposed Gr.91 steel that was subject to operating conditions of 569 °C and 46.7 bar. The images in Fig. 2 show that the grain
boundary carbides in the service-exposed Gr.91 steel coarsened, and the lath width increased compared to those of the virgin
Gr.91 steel. The TEM investigation of the service-exposed Gr.91 steel showed that the fraction of the lath boundaries
decreased from 38.1% to 34.2%, and the lath width increased from 1.34 lm to 2.07 lm in comparison with those of virgin
Gr.91 steel. In addition, matrix recovery and coarsening of the precipitates were observed for the service-exposed specimens.
The Gr.91 steel was initially martensitic steel, but as it was exposed to high temperature and high pressure, the density of
dislocation decreased, and the grain boundary carbides coarsened.

Fig. 1. Gr.91 tee junction and sampled part after 73,716 h of service at a USC plant.

Virgin Gr.91 Service-exposed Gr.91

1 1

Fig. 2. Microstructure of Gr.91 steel before and after service (73,716 h @569 °C, 46.7 bar).

Please cite this article in press as: Lee H-Y et al. Effects of long-time service at high temperature on the material strength and J-R curve of
Grade 91 steel. Engng Fract Mech (2017), http://dx.doi.org/10.1016/j.engfracmech.2017.02.022
4 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx

Fig. 3. Microstructure of service-exposed Gr.91 steel (73,716 h @569 °C, 46.7 bar).

Laves phase with 1–2 lm size was intermittently observed for the service-exposed specimens as shown in Fig. 3, but Z-
phase was not observed at this stage of service. Due to the characteristics of Laves phase, the observed Laves phase would
cause service-exposed Gr.91 steel to be more prone to crack initiation, and its fracture toughness might decrease corre-
spondingly. Exposure of Gr.91 steel for 73,716 h to a temperature of 569 °C and a pressure of 46.7 bar produced Laves phase
precipitation and substructure recovery. The TEM images in Fig. 3 show that all precipitates, including Laves phase and
M23C6, were coarsened due to long-time service, which contributes to reduction of material strengths. M23C6 carbide coars-
ening was reported to contribute to reducing creep rupture strength [3].
Based on the analysis of substructural changes in Gr.91 steel aged 50,000 h, Brinkman et al. [19] reported that a general
coarsening of substructure, reduction of dislocation density, sharpening of subgrain boundaries, coarsening of precipitates,
and precipitation of Laves phase. In addition, Swindeman et al. [3] reported from their investigation on the samples service-
exposed 130,000 h that significant recovery occurred relative to the fine lath substructure in the as-tempered material. Our
TEM observation results were in general agreement with the results of previous research [3,19,20].
In the present study, the effects of long-time service at high temperature on material strengths (YS, TS), ductility, and
fracture toughness were conducted.

3. Treatment of long-time service effect in design codes

The effects of long-term service or thermal aging are not taken into account in ASME Section III Subsection NB [21] which
is the design code for light water reactor components operating in the subcreep region.
However, in case of elevated temperature design codes, the current ETD codes of ASME-NH and RCC-MRx explicitly con-
sider long-time service or thermal aging, although they are not in complete status yet. In the case of the ASME-NH, the effect
of long-time service at high temperature has been taken into account in YS and TS with the introduction of strength reduc-
tion factors [5]. In this study, the conservatism of the reduction factor has been investigated.
In the case of the RCC-MRx [7], thermal aging is taken into account with the introduction of thermal aging coefficients,
although all the thermal aging coefficients are still left blank except the case of J-resistance curve for austenitic stainless steel
[22]. Thermally aged material data are not available yet for the material strength data (YS and TS). However, thermal aging is
explicitly considered for 316LN, while no data are provided for Gr.91 steel yet in RCC-MRx [8,22]. J-R curves for ‘moderate
thermal aging’ and ‘advanced aging’ in 316LN are provided separately, according to the degree of thermal aging as a function
of temperature and time, as shown in Table 2 and Fig. 4, for austenitic stainless steel 316LN. In Table 2 and Fig. 4, no thermal
aging is included in ‘moderate thermal aging’. In the case of 550 °C, thermal aging of 316LN components are classified as
‘moderate thermal aging’ if the elapsed time does not exceed 25,000 h and as ‘advanced thermal aging’ if the elapsed time
does not exceed 110,000 h as shown in Table 2.
Thermal aging is reported to have an impact on ductile-brittle transition temperature (DBTT) for Gr.91 steel [2]. There-
fore, care should be taken not only for DBTT but also reduction of J-R properties in Gr.91 components for long-time service at
high temperature.

Table 2
Classification of thermal aging in the RCC-MRx for 316LN stainless steel [22].

500 °C 525 °C 550 °C 600 °C 650 °C

Moderate thermal aging 175,000 h 64,000 h 25,000 h 4,000 h 950 h
Advanced aging – 280,000 h 110,000 h 19,000 h 4,000 h

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 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx 5

350

300

250

2
J-Integral, kJ/m
200

150

100
o
moderate TA (550 C, 316LN)
o
advanced TA (550 C, 316LN)
50

0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
Crack Extension, mm

Fig. 4. Comparison of the J-R curves under moderate and advanced thermal aging for 316LN.

4. Material strength tests of the virgin and service-exposed Gr.91 steels

4.1. Material specimens

Material specimens were fabricated with plates of virgin Gr.91 steel and service-exposed Gr.91 steel plate as shown in
Fig. 1. The tension test specimen was a conventional ASTM standard specimen with a radius of 9 mm at the central gauge
part and a total length of 130.2 mm. The virgin Gr.91 steel specimens were sampled from a virgin Gr.91 steel plate, while
the service-exposed Gr.91 steel specimens were sampled from a service-exposed Gr.91 steel tee fitting far from the welded
joint, farther than three times the thickness from the welded joint as shown in Fig. 1.

4.2. Material strength tests

A number of tensile tests were conducted for the virgin Gr.91 steel specimens and serviced-exposed Gr.91 steel speci-
mens based on the test matrix in Table 3. As shown in the test matrix, tensile tests at 11 temperatures from room-
temperature to 650 °C were conducted both for the virgin and service-exposed Gr.91 steel specimens. The strain rate of
the test was set as 1 mm/min at the cross head, which is equivalent to a strain rate of 6.67  10 4 (1/s) at the gauge part
of the specimen.
All tensile tests at a specific case in Table 3 were conducted with only one specimen but duplicate tests were conducted
over the temperatures of 500 °C, 550 °C and 600 °C to investigate the data scatter. The duplicate test results showed very
similar behavior with the maximum data scatter 1.51% for 500 °C, 3.88% for 500 °C and 0.61% for 600 °C as shown in
Fig. 5. The stress and strain in Fig. 5 are engineering values. The discrepancies in the duplicate tests were reasonably small,
so other tests were conducted with one specimen each.

4.3. Analysis of tension test results

The tensile test results for virgin Gr.91 steel over a range of temperatures are shown in Fig. 6, and those for service-
exposed Gr.91 steel are shown in Fig. 7. A comparison of the two test results shows that the tensile curve of virgin Gr.91
steel dropped as much as 29.2% at room temperature, 22.8% at 300 °C, 33.0% at 500 °C, and 36.2% at 600 °C as shown in Fig. 8.
The test results of the YS and TS for the virgin and service-exposed Gr.91 steel specimens were compared with those of
the ETD codes [6,8] as shown in Fig. 9. It should be noted in Fig. 9 that the YS of the service-exposed Gr.91 steel dropped
partly below the code properties of the ASME-NH and RCC-MRx at 250 °C, 350 °C and 400 °C. The YS dropped as much as
35.8% at 500 °C, and 33.4% at 550 °C from point A to point B in Fig. 9 over a service period of only 73,716 h.

Table 3
Test matrix of the tension tests.

Test temperature (°C) Strain rate (1/s)

4
Virgin Gr.91 RT, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650 6.67  10
Service exposed Gr.91 RT, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650

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6 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx

600

500

400

Stress, MPa
300
virgin Gr.91
500oC-1
200 500oC-2
550oC-1
100 550oC-2
600oC-1
600oC-2
0
0.00 0.05 0.10
Strain, mm/mm

Fig. 5. Tension test results with two test specimens at 500 °C, 550 °C and 600 °C.

800

700

600
Stress (MPa)

500 RT
200oC
400 250oC
300oC
350oC
300
400oC
450oC
200 500oC
550oC
100 Strain rate = 6.67x10-4 (1/s) 600oC
650oC
0
0.00 0.05 0.10
Strain (mm/mm)

Fig. 6. Tension test results for virgin Gr.91 steel over a range of temperatures.

800

700

600
Stress (MPa)

RT
500 200oC
250oC
400 300oC
350oC
300 400oC
450oC
200 500oC
550oC
600oC
100 Strain rate = 6.67x10-4 (1/s) 650oC

0
0.00 0.02 0.04 0.06 0.08 0.10 0.12
Strain (mm/mm)

Fig. 7. Tension test results for service-exposed Gr.91 steel (73,716 h @569 °C, 46.7 bar).

It is very likely that the YS of the service-exposed Gr.91 steel in Fig. 9 would drop far below the YS of the ETD codes of the
ASME-NH and RCC-MRx as the plant operation time accumulates further, say, up to 60 years which is the target design life of
Gen IV nuclear components.
Long-time service effects are taken into account in the ASME-NH in terms of the YS and TS through the introduction of the
reduction factor shown in Table 4. In the case of Gr.91 steel, the reduction factor for the YS is specified as 1.0, which means

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 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx 7

800 800

700 700 o
virgin_600 C
o
600 600 exposed (73,716h)_600 C
stress (MPa)

stress (MPa)
500 virgin_RT
exposed (73,716h)_RT 500

400 400

300 300

200 200

100 100

0 0
0.00 0.05 0.10 0.15 0.00 0.05 0.10 0.15
strain strain
(a) RT (b) 600 C
Fig. 8. Comparison of the tensile test results of the virgin and service-exposed Gr.91 steels at RT and 600 °C.

600

500
Yield Strength (MPa)

400

300
B
KAERI_Gr.91(virgin)
ASME-NH_Gr.91
200 RCC-MRx_Gr.91_min
KAERI_Gr.91 (73,716 h service)

100
0 100 200 300 400 500 600 700
o
Temperature ( C)

Fig. 9. Comparison of the yield strengths in the design codes and test results for the virgin and service-exposed Gr.91 steels.

Table 4
Tensile and yield strength reduction factor from long-time prior elevated temperature service [5].

Material Service temp. (°C) YS reduction factor TS reduction factor

304SS 480 1.0 0.8
316SS 480 1.0 0.8
Alloy 800H 730 0.9 0.9
Grade 91 480 1.0 [Note 1]

[Note 1]: see Table 5.

no reduction in the YS needs to be considered, while reduction factors for the TS are given in relation to the temperature and
service time shown in Table 5. The interpolated TS reduction factor after 73,716 h service at 569 °C was calculated as 0.89.
In addition, changes in the tensile strength of the service-exposed Gr.91 steel due to long-time service at high tempera-
ture are shown in Fig. 10, which are similar to those in the case of YS shown in Fig. 9. The TS of the service-exposed Gr.91
steel dropped a lot from that of the virgin Gr.91 steel, and it dropped below the TS values of the ASME code at temperatures
higher than 150 °C, while they approached the TS of the RCC-MRx code as the temperature increased, and the TS value
(338 MPa) at 550 °C dropped below the RCC-MRx value (340 MPa) shown in Fig. 10. The TS of the aged Gr.91 specimen
dropped 22.3% at 500 °C, 27.0% at 550 °C and 25.9% at 575 °C from C to D in Fig. 10. It should be noted that the ASME_RF
curve in Fig. 10, which is a curve taking the reduction factor in Table 5 into consideration, dropped below the KAERI_Gr.91
curve after 73,716 h in Fig. 10, which means that the current RF of ASME-NH is non-conservative even for the present case
with 73,716 h service.

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8 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx

Table 5
Tensile strength reduction factors for Gr.91 steel in the ASME-NH.

Temp (°C) Time (h)

1 3  103 104 3  104 105 3  105
450 1 1 1 1 1 1
475 1 1 1 1 1 0.98
500 1 1 1 1 0.97 0.97
525 1 1 1 1 0.94 0.91
550 1 1 1 0.94 0.92 0.89
575 1 1 0.95 0.92 0.88 0.83
600 1 0.96 0.92 0.89 0.85 0.84

800

700
Tensile strength (MPa)

600

500

C
400 KAERI_Gr.91(virgin)
ASME_Gr.91
ASME_RF(73,716h)
300 KAERI_Gr.91(73,716h service) D
RCC-MRx_Gr.91

200
0 100 200 300 400 500 600
o
temperature ( C)

Fig. 10. Comparison of the tensile strengths in the design codes and test results for the virgin and service-exposed Gr.91 steels.

Considering the fact that the stress level at the tee junction was not high (maximum stress intensity of 79.1 MPa), the
degree of material degradation in terms of strengths (YS, TS) was higher than expected, and the YS degradation was more
severe than that seen in a previous study [3].
The above findings of the long-time service effects on the YS and TS raise important issues, such as the possibility of over-
estimation of Gr.91 steel material strengths in the ASME-NH code [5]. Therefore, it seems necessary for the ASME-NH to
address these issues based on more validation material tests.
In addition, the elongation behavior of the Gr.91 steel before and after long-time service was investigated over a range of
the temperatures. The results show that elongation increased as much as 17.8–23%, as shown in Fig. 11, due to long-time
service at high temperature.
Ferritic-martensitic steels, such as Gr.91 steel, owe their creep resistance to the effects of a fine precipitation-stabilized
dislocation network formed during the tempering of martensite [3]. The strength reduction of the service-exposed Gr.91

45

40 virgin
Service exposed 73,716 h
Elongation (%)

35

30

25

20

15
0 100 200 300 400 500 600 700
o
Temperature ( C)

Fig. 11. Comparison of elongation between the virgin Gr.91 and service-exposed Gr.91.

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 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx 9

steel is linked with increase in the lath width and the reduction in the dislocation density due to the recovery and coarsening
of the grain boundary carbides under long-time service.
However, ductility increased due to thermal aging at high temperature. Elongation properties are provided in the RCC-
MRx only for austenitic stainless steel of 316LN and 316L but not for Gr.91 steel [8].

5. J-R curve behavior

Fracture toughness is an important factor along with material strength in maintaining the integrity of high-temperature
components. The fracture properties for austenitic stainless steel are provided relatively well in the RCC-MRx [8] compared
with those of Gr.91 steel [9]. It was reported that there are issues on non-conservatism on the property of creep crack growth
(CCG) for Gr.91 steel in the RCC-MRx Tome 6 [9] based on CCG tests [23].
The other important issue for Gr.91 steel is that the J-R properties are not provided in A9 [8,9] of the RCC-MRx which are
required for leak before break (LBB) analysis. This study was intended to provide the J-R properties of Gr.91 steel for a range
of temperatures. In addition, the effect of long-time service on the J-R behavior in Gr.91 steel was investigated.

5.1. J-R test

The J-R fracture specimens for the virgin Gr.91 and service-exposed Gr.91 steels were standard ASTM compact tension
specimens with a thickness of 25.4 mm and a chevron notch.
The J-R fracture tests were conducted according to the procedure of ASTM E1820 with a fatigue pre-crack larger than
1.3 mm at the notch tip and longer than 0.05 times the notch length.
As part of investigating the fracture toughness of Gr.91 steel, the J-R fracture curves for the virgin and service-exposed
Gr.91 steel specimens were obtained for a range of temperatures, and their J-R behavior was investigated independently
and compared to quantify the effect of long-time service at high temperature.
As shown in the J-R test matrix of Table 6, the tests were performed at 7 temperatures from 300 °C to 600 °C, and the
strain rate of the J-R test at cross-head was 1 mm/min.

5.2. Analysis of J-R test results

The J-R fracture curves obtained for the virgin Gr.91 steel for the eight temperatures are shown in Fig. 12. The J-R curve
has the minimum J value at 400 °C up to a crack extension of 5 mm, which is a unique behavior in that each J resistance at
500 °C, 550 °C and 600 °C is greater than that at 400 °C for the virgin Gr.91 steel shown in Fig. 12.
In the case of the service-exposed Gr.91 steel, the J-R curve for 425 °C was the lowest, which means that the fracture
toughness minimum temperature changed from 400 °C (virgin Gr.91) to 425 °C (service-exposed Gr.91) as shown in

Table 6
Test matrix of the J-R fracture tests.

Test temperature (°C) Cross head speed (mm/min)

Virgin Gr.91 steel 300, 370, 400, 425, 500, 550, 600 1.0
Service exposed Gr.91 steel 300, 370, 400, 425, 500, 550, 600

1750

1500

1250
2
J-Integral, kJ/m

1000

750

Gr.91
500 RT-1 300-1
370-1 400-1
250 425-1 500-1
550-1 600-1

0
0 1 2 3 4 5 6 7 8
Crack Extension, mm

Fig. 12. J-R curve of virgin Gr.91 steel.

Please cite this article in press as: Lee H-Y et al. Effects of long-time service at high temperature on the material strength and J-R curve of
Grade 91 steel. Engng Fract Mech (2017), http://dx.doi.org/10.1016/j.engfracmech.2017.02.022
10 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx

Fig. 13. In addition, the magnitude of the J-integral decreased due to long-time service. The J value dropped as much as 51%
for 425 °C and 16% for 400 °C due to long-time service, which are significant reductions in fracture resistance.
In RCC-MRx [8] thermally aged material data are not available yet for the material strength data (YS and TS) for Gr.91
steel. Considering the steep drop of 50% at 550 °C for 316LN stainless steel, as shown in Fig. 13, in RCC-MRx over the design
lifetime, the decrease of the J values for Gr.91 steel is significantly steeper than those for the 316LN steel case.
The J-R curves before and after service are compared in Figs. 14 and 15 to see the effects of long-time service on Gr.91
steel. As shown in the figures, the J-R curve dropped as much as 25.5% at room temperature, 38.1% at 370 °C, 17.7% at
400 °C, 52.9% at 425 °C, and 38.5% at 600 °C.
A peculiar behavior in the J-R curves was observed at 400 °C in Fig. 14 because the two J-R curves before and after service
are almost the same up to around the 3.2 mm crack increment. In addition, the J-R behavior at 425 °C is important as well
because the J value after long-time service was the minimum.
For the J-R curve of virgin Gr.91 steel, care should be taken at a temperature of 400 °C because that is the temperature of
the ductility minimum in Fig. 11 and pre-study [18]. The coincidence of the temperature (400 °C) for the ductility minimum
and J-R minimum is reported to be correlated with dynamic strain aging [24].
The reduction in fracture toughness was found to be influenced by reduction of strength due to long-term service as well
as association with the Laves phase precipitation observed in the service-exposed Gr.91 steel as mentioned in Section 2.4.
Laves phase with 1–2 lm size was intermittently observed for the service-exposed specimens. The observed Laves phase
with brittle characteristics seems to contribute to the degradation of fracture toughness.
It is important to note that due to long-time service at the USC plant, the Gr.91 steel material strength decreased (26.07%
@400 °C), and the ductility increased (max 23% at 200 °C), while the fracture toughness decreased (52.9% at 425 °C). Ductility
is generally inversely proportional to strength. Toughness is a sort of energy associated with ductility and strength that is
required to fracture a material. The J-R behavior shows that the reduction in the toughness of the service-exposed Gr.91 steel
was more influenced by the reduction in strength rather than the increase in elongation due to long-time service.

1750
Aged Gr.91
1500 RT-1
300-1
370-1
1250 400-1
J-Integral, kJ/m 2

425-1
500-1
1000 550-1
600-1
750

500

250

0
0 1 2 3 4 5 6 7 8
Crack Extension, mm

Fig. 13. J-R curve of service-exposed (73,716 h) Gr.91 steel.

1750 1750

o
1500 1500 400 C (Virgin)
o o
370 C (Virgin) 400 C (73,716h Service)
o
2

370 C (73,716h Service)

J-Integral, kJ/m

1250 1250
2
J-Integral, kJ/m

1000 1000

750 750

500 500

250 250

0 0
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
Crack Extension, mm Crack Extension, mm

Fig. 14. Comparison of the J-R curves for the virgin and service-exposed Gr.91 steels at 370 °C and 400 °C.

Please cite this article in press as: Lee H-Y et al. Effects of long-time service at high temperature on the material strength and J-R curve of
Grade 91 steel. Engng Fract Mech (2017), http://dx.doi.org/10.1016/j.engfracmech.2017.02.022
 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx 11

1750
1750
o
o
500 C (Virgin)
425 C (Virgin) 1500 o
1500 o 500 C (73,716h Service)
425 C (73,716h Service)

1250

2
1250

J-Integral, kJ/m
2
J-Integral, kJ/m

1000 1000

750 750

500 500

250 250

0 0
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
Crack Extension, mm Crack Extension, mm

Fig. 15. Comparison of the J-R curves for the virgin and service-exposed Gr.91 steels at 425 °C and 500 °C.

6. Discussion

The influences of long-time service exposure at high temperature on the strength and fracture toughness of Gr.91 steel
were investigated through tension and J-R fracture tests, and a comparison of the material properties with the elevated tem-
perature design (ETD) codes was made.
An analysis of the long-time service effects on the ASME-NH with a number of relevant material tests showed that the
strength reduction factors in the ASME-NH were non-conservative for the Gr.91 steel considered in this study because
the factors for the YS and TS under long-time service reached nearly the code properties after only 8.4 years of service.
Because the reduction factors of the YS and TS provided in the ASME-NH were shown to be non-conservative for Gr.91 steel
after long-time service, validation of those properties seems to be necessary with relevant material tests.
Based on the present study, the J-R test results for the virgin and service-exposed Gr.91 steels showed that the J-R curves
of the service-exposed specimens dropped by as much as 47.3% at 425 °C from those of the virgin Gr.91 steel specimens. Care
should be taken because the J-R curve drop of Gr.91 steel was larger in the Gr.91 steel than in the austenitic stainless steel of
316LN.
A previous study by Swindeman et al. [3] reported that the yield strengths of T91 superheater tubes after 130,000 h ser-
vice were higher than ASME code properties [6]. However, the present study showed that the YS of F91 tee fitting partly
dropped below design code properties, although the maximum stress intensity under thermal and pressure loading induced
at the tee junction was not high with the value of 79.1 MPa.
Degradation mechanisms can be investigated from a systematic modeling of service-exposed Gr.91 steel in terms of
material strength (YS, TS), creep rupture strength, fatigue strength, and J-R curves.
It is judged that more systematic analysis of thermal aging of Gr.91 steel in terms of material strength, creep rupture
strength, and fatigue strength etc. should be conducted to secure the long-term integrity of the Gr.91 steel components.

7. Conclusion

The effects of long-time service at high temperature on the strength and fracture toughness of virgin and service-exposed
Gr.91 steel were investigated through tension and J-R fracture tests, and the following conclusions were obtained.
The tensile test results of the Gr.91 steels showed that the strength reduction factors in the ASME-NH were non-
conservative for the Gr.91 steel because YS with 73,716 h service dropped significantly by a maximum of 35.8% and dropped
partly below the code properties. Therefore, it seems necessary to validate the strength reduction factors on the YS and TS in
the ASME-NH for Gr.91 steel with more test data.
The J-R properties of Gr.91 steel are currently not available in elevated temperature design codes. Therefore, J-R test data
were produced over a range of temperatures for virgin and service-exposed Gr.91 steel in this study. The J-R test results for
the two Gr.91 steels showed that the J-R curves of the service-exposed specimens dropped as much as 47.3% at 425 °C and
16% at 400 °C from those of the virgin Gr.91 steel specimens. Comparing the amounts of the J-R curve drop, the J-R curves of
the Gr.91 steel were found to have a greater reduction in the Gr.91 steel than in austenitic stainless steel of 316LN.

Acknowledgements

This work was supported by a NRF grant (2013K1A3A7A03078195) and another NRF grant (2012M2A8A2025635) of the
Korea government (MSIP). We would also like to gratefully acknowledge the TEM investigations by Prof. Hyun Uk Hong of

Please cite this article in press as: Lee H-Y et al. Effects of long-time service at high temperature on the material strength and J-R curve of
Grade 91 steel. Engng Fract Mech (2017), http://dx.doi.org/10.1016/j.engfracmech.2017.02.022
12 H.-Y. Lee et al. / Engineering Fracture Mechanics xxx (2017) xxx–xxx

Changwon National University, material tests by Dr. Woo-Gon Kim of KAERI, and Prof. Chang-Sung Seok and Mr. Suk-Woo
Hong of Sungkyunkwan University.

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Please cite this article in press as: Lee H-Y et al. Effects of long-time service at high temperature on the material strength and J-R curve of
Grade 91 steel. Engng Fract Mech (2017), http://dx.doi.org/10.1016/j.engfracmech.2017.02.022