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Application of Small Punch Test to Evaluate Sigma-

Phase Embrittlement of Pressure Vessel Cladding
Material
a a b
JooSuk LEE , InSup KIM & Akihiko KIMURA
a
Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science
and Technology, 373-1, Guseong-Dong, Yuseong-Gu, Daejeon, 305-701, Korea
b
Institute of Advanced Energy, Kyoto University, Gokasho, Uji-shi, Kyoto, 611-0011
Published online: 07 Feb 2012.

To cite this article: JooSuk LEE , InSup KIM & Akihiko KIMURA (2003) Application of Small Punch Test to Evaluate Sigma-
Phase Embrittlement of Pressure Vessel Cladding Material, Journal of Nuclear Science and Technology, 40:9, 664-671

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 Journal of NUCLEAR SCIENCE and TECHNOLOGY, Vol. 40, No. 9, p. 664671 (September 2003)

ORIGINAL PAPER

Application of Small Punch Test to Evaluate Sigma-Phase Embrittlement of

Pressure Vessel Cladding Material
JooSuk LEE1 , InSup KIM1,* and Akihiko KIMURA2
1
Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology,
373-1, Guseong-Dong, Yuseong-Gu, Daejeon, 305-701, Korea
2
Institute of Advanced Energy, Kyoto University, Gokasho, Uji-shi, Kyoto 611-0011
(Received May 27, 2003 and accepted in revised form July 11, 2003)

The influence of -phase on mechanical properties in type ER309L stainless steel has been investigated by small
punch test. The SA508 cl.3 reactor pressure vessel steel plates were overlay-cladded with the type ER309L welding
consumable with different heat input rates. The microstructure of the clad was composed of fcc -austenite, a few
percent of bcc -ferrite and bct -phase. Area fraction of -phase was ranging approximately 28% depending on the
welding condition. Ductile to brittle transition behavior was observed in the clad, and it was strongly affected by the
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amount of brittle -phase. When the -phase content was about 8 percent, the transition behavior almost disappeared
due to severe cracking. Fracture appearance gradually changed from circumferential to radial cracking not only as
test temperature became low but as the volume fraction of -phase increased. The results are manifested in terms of
fracture stress of -phase and -ferrite combined with the roles of radial and circumferential stress by means of the
stress analysis of deformed specimen using finite element method.
KEYWORDS: sigma phase, cladding, delta ferrite, small punch test, finite element method, stress analysis

I. Introduction as an effective method to determine the degree of thermal ag-

The inner wall of reactor pressure vessel (RPV) was
overlay-cladded with 300 grade austenitic stainless steels of
a few millimeter thickness to prevent general corrosion at-
tack and the resultant radioactive contamination problems in
main coolant system. The microstructure of the clad is usually
composed of face-centered cubic (fcc) -austenite and small
amount of body-centered cubic (bcc) -ferrite. Small amount
of primary -ferrite is desirable in the welded austenitic stain-
less steels, because the ferrite phase absorbs phosphorous and
sulfur and thereby prevents hot cracking or tearing.1) On the
other hand, it is likely to decompose to brittle -phase and
newly created austenite when the steel was exposed to in the
range of 873 to 1,173 K for a long time. The crystal structure
of -phase is body-centered tetragonal (bct) with 30 atoms
per unit cell and its hardness value is approximately 68 con-
ventional Rockwell (HRC).2)
The presence of -phase in an austenitic stainless steel re-
sulted in the dramatic loss of ductility and toughness.35) A
study on the influence of -phase in a type 310 stainless steel
showed that the toughness reduction was about 85% by aging
at 973 K for 2 h.5) However, as for the nuclear RPV cladding
materials, although a few researches have been done to mea-
sure the changes in mechanical properties induced by thermal
aging and neutron irradiation,69) it is still insufficient to ex-
plain the changes of mechanical properties related with the
microstructural characteristics even at unirradiated condition,
particularly concerned with the role of -phase.
In this study, the changes in mechanical properties in ac-
cordance with the variation of -phase in the RPV cladding
were manifested by small punch (SP) test. The SP test proved
Corresponding author, Tel. +82-42-869-3815, Fax. +82-42-869-
3810, E-mail: iskim@kaist.ac.kr
ing embrittlement of a duplex stainless steel.10) Stress analysis
was also carried out to evaluate the cracking criteria of small
punch specimen with the aid of finite element method (FEM).
II. Experimental Procedures
1. Fabrication of Clad and Microstructure Observations
The weld consumable of strip ER309L stainless steel
(0.5t mm90w mm) was overlay-cladded with submerged-arc
welding (SAW) on SA508 cl.3 plates. The chemical com-
position of ER309L is given in Table 1. Three kinds of
clad were fabricated with varying maximum heat input rates
from 164.4 (K001 clad) to 188.5 kJ/cm (K002J clad) by con-
trolling the welding parameters such as current (A), voltage
(V), and welding speed (cm/min). The thickness of single-
layered cladding was approximately 6 mm. The heat treat-
ment of the clads during overlay welding process included
a preheat temperature of 394 K min., an interpass tempera-
ture of 449 K max., and a post heating at 483583 K for 2 h.
The claded plates were then postweld heat treated (PWHT) at
893901 K for 41 h. The microstructure of the clad was ex-
amined using scanning electron microscope (SEM) after elec-
trolytic etching in a solution of 50 g NaOH in 100 ml water at
2 V for 5 s. The ferrite content and the area fraction of -
phase were measured using a Ferrite Content Meter and an
image analyzer after electrolytic etching, respectively. The
results are given in Table 2.
2. Small Punch Test
Transmission Electron Microscopy (TEM) disk (30.28t
mm) type SP specimens were sampled from the portions of
2 mm away from the weld fusion line to avoid a dilution ef-
fects. SP test was performed with an Instron 4204 at a cross-
head speed of 0.2 mm/min at temperatures from 77 to 293 K.

664
 Application of Small Punch Test to Evaluate Sigma-Phase Embrittlement 665

Table 1 The chemical composition of AWS Class ER309L weld metal (wt%)

C Si Mn P S Cr Ni Mo Co V Ti Cu Nb N
0.011 0.36 1.60 0.013 0.001 23.77 13.19 0.06 0.026 0.052 0.09 0.039 0.01 0.045

Table 2 The phase fractions of each RPV clad

Index Austenite (area %) -ferrite (FNa) ) (before PWHT) -ferrite (FN) -phaseb) (area %)
K001 90 9.1 6.6 1.9
K002 90 10.4 6.0 3.7
K002J 90 10.2 2.5 7.9
a) FN: Ferrite number was measured by Ferrite Content Meter, which almost equals to the volumetric percentage.
b) The phase fractions in the clad were measured after applying postweld heat treatment (PWHT).
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Fig. 1 Schematic drawing of the small punch (SP) test cell and specimen holder

Figure 1 shows the schematic drawing of the SP test cell.
Temperature was controlled by injection of liquid nitrogen
into a nitrogen tank with argon gas environment. Steel balls
of 1 mm diameter of which hardness values were over HRC
60 were employed to apply a load to specimens. Displace-
ments were measured using linear variable differential trans-
ducer (LVDT) that was placed to touch the bottom surface of
the specimen. As shown in Fig. 1, the specimen holder con-
sisted of a die with a central hole of 1.6 mm in diameter and a
clamping screw with a hole of 1 mm in diameter for guiding
the ball and loading pin. Scanning electron microscope was
used to observe the fracture surface and cracking appearance
of SP specimens. Figure 2 presents a typical load-deflection
curve at room temperature with definitions of SP properties.
The SP energy was defined as the area under load-deflection
curve per unit thickness of the given specimen. In general, SP
ductile to brittle transition temperature (SP-DBTT) is defined
to be the temperature where the specific SP energy is the aver-
age of maximum and lower shelf SP energy. However, since
the lower shelf energy was not observed in this work, it was
replaced with the SP energy attained at 77 K.
3. Finite Element Stress Analysis
The ABAQUS 6.3-1 standard finite element analysis soft-
ware was used to simulate the small punch test results. Simu-
lation system of SP test was comprised with three main com-

VOL. 40, NO. 9, SEPTEMBER 2003

 666
ponents; the specimen, the ball, the upper and lower die, and
an axis-symmetric mesh was used. Figure 3 presents the brief
sketch of the system. The specimen measures 0.28 mm in
thickness and 3 mm in diameter. The diameter of the ball and
the central hole in lower die is 1.0 mm and 1.6 mm, respec-
tively. In this calculation, it was assumed that the specimen,
which consisted of 660 elements with CAX4R type (4 node
bilinear without twist), was an elastic-plastic body, and both
the ball and the die were rigid ones. The friction coefficient
was selected to be 0.25 for the loading involved in the sys-
tem. The material properties of the specimen were inserted
for evaluating stress components. The elastic properties were
assigned (E=190 GPa, =0.28) and true stress vs. true strain
data for plastic properties were obtained from uniaxial ten-
sile testing. The load was applied to the ball in the vertical
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Fig. 2 Typical SP load-deflection curve of K001 RPV clad at room
temperature with the definition of SP properties
Fig. 3 Brief sketch of the small punch test simulation system and
the mesh of the SP specimen used in the present finite element
analysis
J. LEE et al.
direction (in Y -direction) in a static mode.
III. Results and Discussion
1. Microstructure of RPV Clads
Figure 4 presents the typical microstructure of 309L clad
varying with the heat input rates. The main metallic phase
of the clad was composed of about 90% fcc austenite, a few
percent of bcc -ferrite and brittle bct -phase, regardless of
welding conditions. The -ferrite was mainly formed at the
austenite grain boundaries and sometimes formed inside the
austenite matrix in a skeleton manner. As listed in Table 2,
after applying stress relieving heat treatment, the content of
-ferrite was reduced to about 6.6, 6.0, and 2.5 vol% in K001,
K002, and K002J clad, respectively. At the same time, the
fraction of -phase in each clad was measured approximately
1.9, 3.7, and 7.9 area %. The simultaneous occurrence of re-
duction of -ferrite and formation of phase can be explained
by the following two decomposition mechanisms of -ferrite
during the heat treatment.4, 5, 11) The first is the precipitation
of chromium rich carbides at initial / boundaries by the
eutectoid reaction (M23 C6 +  ) and the second is forma-
tion of -phase and new austenite (  ) ( +  ). On the
other hand, the variation of contents of -phase in each clad
is considered to be related to the total amount of available
chromium atoms which are consumed to form a -phase dur-
ing stress relieving heat treatment.
2. Temperature and Microstructure Dependent SP
Properties
Figure 5 presents experimental and simulation results of
load-deflection curves as a function of test temperature. The
simulation results for the 309L stainless steel in the tempera-
ture range from 293 to 77 K give an almost accurate descrip-
tion of experimental load-deflection curves in the whole test
temperatures. In K001 clad, the maximum SP load continu-
ously increased until the test temperature decreased to 153 K
and the fracture occurred in the plastic instability region, indi-
cating ductile shearing type fracture. Below 153 K, the maxi-
mum SP load suddenly decreased and the specimens fractured
in the plastic membrane stretching region. When the test tem-
perature was 77 K, a continuous small amount of load drop
occurred in the plastic membrane stretching region. This ser-
ration like behavior may be related to the preferential fracture
of brittle ferrite by the high radial stress (load drop) and the
arrest by surrounding ductile austenite (load rise).10) The sim-
ilar behavior was observed in a set of load-deflection curves
of K002 clad, while the onset temperature of the serrations
moved to a higher temperature. However, the final fracture
load and deflection of K002J clad at fracture were very small
compared to the other clads at all test temperatures.
Figure 6 presents the constituents of normalized maximum
SP load, Pm /to2 , and final deflection as a function of test tem-
perature, where, to is the initial specimen thickness in mil-
limeter. As shown in Fig. 2, the maximum SP load, Pm , con-
sists of four components corresponding to each deformation
region,
Pm = Peb + Ppb + Ppms + Ppi ,
JOURNAL OF NUCLEAR SCIENCE AND TECHNOLOGY
 Application of Small Punch Test to Evaluate Sigma-Phase Embrittlement 667

(a) K001 (b) K002J

Fig. 4 Typical microstructural characteristics of the clad materials, gray=austenite, white gray=new austenite (  ),
dark gray=-ferrite, black= phase, Backscattered electron mode
The K001 and K002J clad were fabricated with the heat input rate of 164.4 and 188.5 kJ/cm, respectively.
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(a) K001 clad

Fig. 6 The constituents of normalized maximum SP loads, Pm /to2 ,

and final deflection, t , at fracture as a function of temperature
Peb , Ppb , Ppms and Ppi represent the constituent of max-
imum SP load such a elastic bending, plastic bending, plastic
membrane stretching and plastic instability, respectively.

stituent indicated a strong dependence on test material and

(b) K002J RPV clad
Fig. 5 Experimental and simulation results of SP load-deflection
curves as a function of test temperature
where Peb , Ppb , Ppms and Ppi represent the com-
ponent of maximum SP load such as elastic bending, plas-
tic bending, plastic membrane stretching and plastic instabil-
ity, respectively. From the figure, the variation of normal-
ized (Peb +Ppb ) constituent was slightly dependent on the
test materials and it increased continuously as test tempera-
ture cooled down, while the normalized (Ppms +Ppi ) con-
temperature with decreasing temperature. The K001 material
showed a gradual increase in the normalized (Ppms +Ppi )
until it suddenly decreased at 153 K, and K002 clad showed a
similar strengthening behavior before it decreased at around
223 K. The K002J material, however, displayed the lowest
values compared to the others and it did not show a peak
of maximum SP load in the temperature range tested in this
work. These differences between the materials are consid-
ered to be due to the difference in the volume fraction of -
phase. The -phase tended to fracture rather than plastically
deformed during deformation and its fracture stress which
was estimated by fibre loading model, was 750 MPa.5) As for

VOL. 40, NO. 9, SEPTEMBER 2003

 668
the role of ferritic steel, even though the typical ferritic phase
has a brittle nature at low temperature, it has a much higher
fracture stress than that of the -phase.12)
Figure 7 presents the effective stress, eff , developed at disk
bottom surface during testing. The eff is defined by13)
1
1/2
eff = (1 2 )2 + (1 3 )2 + (2 3 )2 . Figure 8 presents the temperature dependence of specific
2 SP energy in each clad. The K001 clad showed a gradual
Here, 1 , 2 , and 3 are principal stress components in the x-,
y-, z-directions, respectively. The results indicate that in the
initial deformation process, the peak-effective stress is devel-
oped at the center regions of the specimen and it gradually
moves toward clamped edge with progressing deformation.
In this situation, cracking of -phase will be started when
the peak stress was equal to the fracture stress of -phase.
This occured at a relatively small deflection (approximately
=0.26 and 0.03 mm at 293 and 87 K, respectively), which
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corresponded to the plastic membrane stretching and plastic
bending regine at 293 and 77 K, respectively. Further, the sus-
ceptibility to cracking might coincide with the amount of -
(a) 293 K
(b) 77 K
Fig. 7 Development of effective stress, eff , with proceeding the
deformation at disk bottom surface in K002J material
Simulated at (a) 293 K and (b) 77 K.
J. LEE et al.
phase in the clad, and, from the microstructure observation,
the content of -phase in K001, K002, and K002J was ap-
proximately 1.9, 3.7, and 7.9%, respectively. Therefore, the
smaller strengthening in K002J material would be unavoid-
able by the creation of many micro-cracks, in the -phase
along the austenite grain boundaries.
increase in specific SP energy with decreasing temperature
until the maximum energy was found at around 183 K. As
the test temperature decreased further, a sudden drop of spe-
cific SP energy was observed. The same trends could be seen
in K002 clad except the maximum SP energy was shifted to
about 223 K. However, the transition behavior almost dis-
appeared in K002J clad. The SP energy of K002J showed
almost ground energy levels irrespective of test temperatures
even at room temperature. The difference in transition behav-
ior among the clads seems to originate from the reduction in
load carrying capability and in final deflection according to
the volume fraction of phase. Since the cracked phase
at an early stage in deformation process acted as a nucleation
site of the fracture,25) the presence of phase is considered
to induce a significant reduction in the SP energy depending
on its amounts.
3. Cracking Appearance
Figure 9 presents the cracking appearances of SP speci-
men tested at different temperatures. Cracking appearance
of K001 specimen was completely circumferential at room
temperature, and they showed the mixed mode of radial and
circumferential cracking below 153 K. Similar trend was also
identified in K002 and in K002J specimens except that domi-
nant radial and complete radial cracking could be seen at 77 K
in K002 and K002J, respectively. The difference in cracking
appearance with test temperature is attributed to the differ-
Fig. 8 The temperature dependence of specific SP energy of each
RPV clad material
The SP-DBTT was 144 and 165 K in K001 and in K002 clad,
respectively. However, the SP-DBTT in K002J clad with a larger
fraction of phase (7.9%) could not be determined because of the
significant embrittlement at the entire test temperature regions.
JOURNAL OF NUCLEAR SCIENCE AND TECHNOLOGY
 Application of Small Punch Test to Evaluate Sigma-Phase Embrittlement 669

Fig. 9 Scanning electron micrographs of cracking appearance of SP specimen

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(a), (b), and (c) represents K001 SP specimen tested at 293, 153, and 77 K, respectively. (d), (e), and (f) is the results
of K002J tested at the same temperature.

ence in the critical deflection to induce fracture of -phase

or -ferrite, as well as to the difference in the principle stress
component, namely, radial (rad ) or circumferential (cir ), de-
pending on the deflection.
As shown in Fig. 7, the position of peak-effective stress de-
veloped at the bottom surface moves from the center regions
to the clamped edge with proceeding deformation. In this sit-
uation the contributions of radial and circumferential stress
to the effective stress were depicted in Fig. 10. At initial de-
formation process (0.030.05 mm) near the center regions,
rad was smaller than cir , and this turned to reverse as de-
formation proceeded. In the meantime, the fracture stress of
-phase at the disk bottom surface was able to be attained
as the deflection was approximately 0.26 and 0.03 mm at 293
and 77 K, respectively. And, at that point the principle stress
component, which was responsible to the fracture of -phase, (a) 293 K
was attributed to the radial and circumferential one at 293 and
77 K, respectively. Accordingly, the cracking path will be
formed in circumferential and in radial direction at 293 and
77 K, respectively.
Figure 11 shows the higher magnification of the regions
in (d) and (f) of Fig. 9. In the figure, besides the larger cir-
cumferential cracks near at the clamped edge at 293 K, there
exist many minor circumferential cracks in K002J clad 200
400 m away from the specimen center. On the other hand,
we could also confirm the creation of many micro-cracks by
the fracture of -phase in radial direction at 77 K. The radial
cracks were combined with each other by the tearing of sur-
rounding austenite, and the main cracks were able to propa-
gate to the radial direction. Those observed appearances well
coincide with the predicted cracking paths analyzed by finite
element method.
Some differences of cracking appearance among the clads (b) 77 K
may stem from the difference in the fracture stress between
Fig. 10 Variation of radial, r ad , and circumferential stress, cir ,
-phase and -ferrite. Though the -ferrite became brittle at component with proceeding the deformation at disk bottom sur-
low temperatures,14) -phase is much susceptible than that of face in K002J material
-ferrite, regardless of test temperatures. The fracture stress Simulated at (a) 293 K and (b) 77 K.
of typical ferritic steel is approximately 1,000 MPa (when the

VOL. 40, NO. 9, SEPTEMBER 2003

 670
Fig. 11 Scanning electron micrographs of K002J SP specimen tested at 293 and 77 K
(a) and (b) are higher magnification of the regions indicated in (d) and (f) of Fig. 9, respectively. (c) is the higher
magnification of the regions indicated in (b) of Fig. 11, respectively. Arrows in (a) indicate the formation of circum-
ferential cracks at the center regions of the specimen and arrows in (c) indicate the cracking of phase in the radial
direction.
yield and the tensile strength were approximately 340 and
600 MPa, respectively).12) Thus, to reach the fracture stress
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of ferritic phase, it should be deflected about 0.1 mm even at
77 K (Fig. 7(b)). At that point the radial stress is somewhat
higher than or similar to the circumferential one (Fig. 10(b)),
consequently, the mixed mode cracking was able to be formed
at 77 K in K001 specimen, because it contained about 6.6%
-ferrite, which was more than two times larger -ferrite frac-
tion than that of the K002J.
IV. Summary
The alteration of mechanical properties in accordance with
the volume fraction of phase in the RPV cladding was man-
ifested by SP test. In addition, the changes of the principle
stress component during deformation were correlated with the
cracking appearances of the deformed SP specimen. The re-
sults are summarized as follows:
(1) The microstructure of the clad was composed of fcc
austenite and a few percent of bcc -ferrite, and the
transformation of -ferrite during postweld heat treat-
ment resulted in the formation of brittle bct -phase.
Area fraction of -phase was ranging approximately 2
8% depending on the welding condition.
(2) The ductile to brittle transition behavior of RPV clad was
mainly controlled by the amount of -phase because the
-phase fractured during initial deformation process and
the cracked -phase acted as a nucleation site of the frac-
ture. When the area fraction of -phase was about 8%,
the transition behavior almost disappeared due to the sig-
nificant cracking even at room temperature.
(3) As test temperature was decreased, the fracture stress
of -phase was easily developed at the center region of
SP specimen at initial deformation stage, where the cir-
cumferential stress was higher than the radial stress. For
that reasons, the fracture appearance of SP specimen was
changed from circumferential to radial cracking as the
test temperature decreased.
(4) Small punch test was effective to evaluate the -phase
embrittlement and the FEM analysis to simulate the
stress state in the SP specimen was well interpreted the
crack appearance of the specimen.
J. LEE et al.
Acknowledgments
This work has been carried out as a part of the Core Uni-
versity Program (CUP) between Korea and Japan, supported
by Ministry of Science and Technology (MOST) in Korea and
Japan Society for the Promotion of Science (JSPS). The au-
thors are grateful to DooSan Heavy Industry for supplying
of RPV clad materials as welded state and Dr. J. S. Cheon
in Korea Atomic Energy Research Institute (KAERI) for his
valuable advice on the FEM analysis.
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