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WELDING RESEARCH

SUPPLEMENT TO THE WELDING JOURNAL, FEBRUARY 2003


Sponsored by the American Welding Society and the Welding Research Council

The Mechanism of Stress-Relief Cracking


in a Ferritic Alloy Steel
A novel stress-relaxation technique and extensive microstructural characterization
of the carbide precipitation, elemental segregation, and fracture modes were used
to investigate stress-relief cracking in a ferritic alloy steel

BY J. G. NAWROCKI, J. N. DUPONT, C. V. ROBINO, J. D. PUSKAR, AND A. R. MARDER

ABSTRACT. Stress-relief cracking is a to be individually analyzed by using EDS welded during repairs. In such applica-
major cause of weld failures in creep- and elemental EDS traces taken across tions, preheat and/or postweld heat treat-
resistant, precipitation-strengthened ma- prior austenite grain boundaries. In addi- ments (PWHT) are often required to im-
terials such as ferritic alloy steels, stainless tion, SE STEM imaging with the VG603 prove heat-affected zone (HAZ)
steels, and Ni-based superalloys. Stress- FEG STEM was able to resolve small pre- mechanical properties and reduce suscep-
relief cracking occurs primarily in the cipitates that were previously unobserv- tibility to hydrogen cracking. These pre-
coarse-grained heat-affected zone of able using conventional TEM and STEM heat and PWHT steps represent a signifi-
weldments. Although the general causes techniques. The results of this study form cant fraction of the overall fabrication/
of stress-relief cracking are known, the un- a basis for heat treatment and welding repair costs.
derlying mechanisms are very much a process variables for HCM2S to avoid Recently, a new ferritic steel, denoted
topic of debate. The mechanism of stress- stress-relief cracking. In addition, these as HCM2S, was developed. HCM2S has
relief cracking in the coarse-grained heat- procedures and analytical results can be been reported to exhibit improved me-
affected zone (CGHAZ) of a new ferritic applied to other materials to avoid mi- chanical properties and resistance to hy-
alloy steel (HCM2S) was investigated crostructures that are susceptible to drogen cracking compared to 2.25Cr-1Mo
through stress-relaxation testing and de- stress-relief cracking. steel (Refs. 1, 2). Table 1 compares the al-
tailed microstructural characterization. lowable composition ranges of both
The CGHAZ simulation and stress-relax- Introduction 2.25Cr-1Mo steel and HCM2S. Although
ation testing was performed using Gleeble the carbon content of HCM2S and
techniques. The time to failure exhibited Ferritic alloy steels such as 2.25Cr-1Mo 2.25Cr-1Mo can be identical, HCM2S is
C-curve behavior as a function of temper- steel are commonly used for high-temper- typically produced with a carbon content
ature. A balance of intergranular and in- ature applications in steam generators of ~0.06 wt-%, which is much lower than
tragranular carbide precipitation con- and pressure vessels for chemical and fos- the typical carbon content of 2.25Cr-1Mo
trolled the stress-relief cracking sil power plants. Many components in steel (Refs. 1–5). In addition, the maxi-
susceptibility. Cracking initiated at prior these power plants operate at tempera- mum allowable C content is 0.1 and 0.15
austenite grain boundaries by cavity nu- tures of approximately 300–700°C. wt-% for HCM2S and 2.25Cr-1Mo steel,
cleation on incoherent, Fe-rich M3C car- New components fabricated from respectively. The lowered carbon content
bides. The grain interiors were resistant to 2.25Cr-1Mo steel may require welding at of HCM2S relative to 2.25Cr-1Mo steel
plastic deformation due to precipitation both the installation and fabrication improves weldability by reducing harden-
strengthening by small (5–40 nm) alloy stages, and in-service material may be ability and, therefore, the as-welded hard-
carbides. Elemental segregation played ness of the HAZ. The creep rupture
no detectable role in the stress-relief strength is improved by the substitution of
cracking failures. Much of the microstruc- Mo with W as a solid solution strength-
tural characterization was performed KEY WORDS ener. Vanadium and niobium are added to
using a VG603 FEG STEM having a improve creep strength by way of carbide
probe size of about 1.5 nm. The small Stress-Relief Cracking precipitation strengthening. Boron is also
probe size allowed nano-sized precipitates Carbide Precipitation added to improve creep strength. It has re-
Coarse-Grained HAZ cently been suggested that the improved
J. G. NAWROCKI, A. R. MARDER, and J. N. weldability from these composition modi-
Heat-Affected Zone
DUPONT are with Department of Materials Sci- fications may permit elimination of costly
ence and Engineering, Lehigh University, Bethle- Ferritic Alloy Steel
High Temperature preheat and/or PWHT requirements
hem, Pa. C. V. ROBINO and J. D. PUSKAR are
with Joining and Coating Department, Sandia
(Ref. 1). However, even if no PWHT is
National Laboratories, Albuquerque, N.Mex. necessary, HCM2S will be exposed to
comparable temperatures in service

WELDING JOURNAL 25 -S
WELDING RESEARCH
work has shown martensite start and finish temperatures.
HCM2S to be suscepti- Carbides begin to precipitate when the
ble to stress-relief CGHAZ is exposed to elevated tempera-
cracking, but the un- tures during postweld heat treatment for
derlying mechanisms stress-relief and/or during service. Eventu-
are largely undeter- ally, stable carbides such as those based on
mined (Ref. 6). V, Mo, Nb, and W nucleate on the many
Stress-relief crack- dislocations present in the grain interiors.
ing is a common cause The result is a fine, uniform dispersion,
of weld failures in producing significant precipitation
many creep-resistant, strengthening and even secondary harden-
precipitation-strength- ing. These alloy carbides are mainly coher-
ened alloys such as fer- ent or semicoherent with the ferrite matrix
ritic alloy steels (Refs. and stable at relatively high temperatures
7–9), stainless steels for long times (Refs. 7, 8, 14). The precip-
(Refs. 10, 11), and Ni- itates retard dislocation movement and re-
Fig. 1 — Time to failure during stress-relaxation testing for various test tem- based superalloys strict relaxation of residual stresses during
peratures. The numbers within the graph represent the average of four to (Refs. 12, 13). The gen- postweld heat treatment. Carbides will
six tests at temperature. eral definition of also form on the energetically favorable
stress-relief cracking is prior austenite grain boundaries. These
intergranular cracking carbides are typically Fe3C, M23C6, and
in a welded assembly M6C and, at later stages of coarsening, are
Table 1 — Allowable Composition Ranges of that occurs during exposure to elevated mainly incoherent with the matrix. They
HCM2S (wt-%) temperatures produced by post-weld heat coarsen easily due to the incoherency and
treatments (PWHT) or high-temperature the fact they are located along high diffu-
Element HCM2S 2.25Cr-1Mo service (Ref. 14). Residual stresses are sivity paths. The matrix adjacent to the
(Ref. 1) (Ref. 3) typically relieved during a PWHT through boundaries can then become devoid of al-
C 0.04–0.10 ≤0.15
plastic deformation of the material. loying elements, and a precipitate-free or
Cr 1.90–2.60 2.00–2.50 Therefore, a susceptible microstructure is denuded zone is thereby formed along the
Mo ≤0.30 0.90–1.10 one with strong grain interiors that resist prior austenite grain boundary (Refs. 9,
W 1.45–1.75 — plastic deformation and weak grain 11). This region is soft and ductile relative
V 0.20–0.30 — boundaries. Failure can occur in the heat- to the remaining precipitation-strength-
Nb 0.02–0.08 — affected zone or fusion zone, but the ened grain interior.
B ≤0.006 — coarse-grained heat-affected zone Elemental segregation is also known to
Al ≤0.03 —
Si ≤0.50 0.20–0.50
(CGHAZ) is the most susceptible region cause stress-relief cracking (Refs. 14, 15).
Mn 0.30–0.60 0.30–0.60 of a steel weldment. Tramp elements (S, P, Sn, Sb, As) and in-
P ≤0.030 ≤0.035 Although the details of stress-relief tentionally added elements (Al, B, Mn)
S ≤0.010 ≤0.035 cracking mechanisms are not totally un- can segregate to prior austenite grain
derstood, general knowledge of the causes boundaries causing decohesion and weak-
of stress-relief cracking for ferritic alloy ening of the boundaries. In addition, sul-
Table 2 — Chemical Composition of HCM2S steels has been well developed (Refs. 8, fides are thought to precipitate at prior
Used in this Research 14–17). During a typical arc welding austenite grain boundaries, act as cavity
process, the unmelted base metal directly nucleation sites, and promote crack prop-
Element Wt-% adjacent to the fusion zone reaches tem- agation through stress-driven diffusion
peratures close to the melting point of the (Ref. 18).
C 0.061 material, high in the austenite phase field The result of the above microstructural
Cr 2.52
Mo 0.11 of the Fe-C phase diagram. During the features is a precipitation-strengthened
W 1.50 time spent in the austenite phase field, pre matrix with comparatively weak grain
V 0.24 existing carbides, nitrides, carbonitrides, boundary areas caused by one or more of
Nb 0.05 and even some inclusions dissolve into the the following: coarse, incoherent precipi-
B 0.0036 austenite matrix. Since dissolution of the tates; a soft denuded zone; and/or ele-
Al 0.013 precipitates is diffusion-controlled, the mental segregation. Therefore, stress
Si 0.30 degree of dissolution is dependent on the (residual or applied) will not be relieved
Mn 0.33
Ni 0.07
welding parameters that influence the through the intended macroscopic plastic
N 0.007 thermal profile (time and temperature). deformation of the grains, but rather by
P 0.0013 However, if sufficient dissolution occurs, cracking along prior austenite grain
S 0.006 austenite grains grow essentially unim- boundaries culminating in catastrophic,
Ar 0.0029 peded, resulting in a large austenite grain stress-relief cracking failure.
Sb 0.0001 size. Due to the fast cooling rates associ- As described above, numerous theo-
Sn 0.007 ated with arc welding, dissolved alloying ries exist on the causes of stress-relief
Cu 0.022
elements remain trapped in solution and cracking and these theories may all be
the austenite transforms to low-ductility valid under certain circumstances. The
martensite or bainite depending on the general reasons for stress-relief cracking
where stress-relief cracking can occur dur- hardenability and thermal cycle. Another are known, but the underlying mecha-
ing operation (Refs. 1, 2). In addition, possibility is that the newly formed nisms are still a source of debate. Many
HCM2S may be welded to existing 2.25Cr- martensite may auto-temper during cool- studies explore only one mechanism and
1Mo steel that requires a PWHT. Previous ing, which is favored in systems with high disregard others. In addition, various

26 -S FEBRUARY 2003
WELDING RESEARCH

Fig. 2 — Representative LOM photomicrographs of failed samples viewed in cross section. Arrows indicate areas of void formation.

Fig. 3 — Representative SEM photomicrographs of the fracture surface of a sample that failed during testing at 575°C. IG = region of intergranular fracture;
DT = region of ductile tearing.

mechanisms can operate simultaneously Experimental Procedure and heated to the desired PWHT temper-
and the mechanism can change as a func- ature at a rate of 200°C/s. The simulated
tion of temperature. The chemical composition of the CGHAZs were tensile tested at tempera-
The alloy HCM2S may be susceptible HCM2S used in this work, as determined tures of 575, 625, 675, and 725°C to obtain
to stress-relief cracking from a composi- using optical emission spectroscopy and the necessary data for the stress-relax-
tional standpoint because it contains many wet chemical analysis, is shown in Table 2. ation tests. The 0.2% offset yield point was
strong carbide-forming elements and ele- Constant displacement, stress-relaxation determined from the tensile tests using a
ments known to embrittle grain bound- tests were conducted to assess the stress- dilatometer, which allowed only the
aries. Previous studies have confirmed relief cracking susceptibility of the CGHAZ to be monitored during tensile
HCM2S can be susceptible to stress-relief CGHAZ of HCM2S using round samples testing. The corresponding lengthwise dis-
cracking (Ref. 6). Therefore, the objective with a length of approximately 105 mm placement at the 0.2% yield point was de-
of this research was to gain a fundamental and a diameter of 10 mm with threaded termined from the acquired data and then
understanding of the mechanism(s) of ends. The samples had a reduced gauge- used for the constant displacement stress-
stress-relief cracking using HCM2S as the section approximately 10 mm in length relaxation tests because the Gleeble could
model system. Although HCM2S is a com- and 5 mm in diameter. The CGHAZ was not be programmed to pull the sample to
plicated system, such an alloy is necessary simulated and all testing was done using a the required cross-wise displacement.
to explore each of the possible mecha- Gleeble 1000 thermomechanical simula- Further details of the stress-relaxation test
nisms of stress-relief cracking. Conclu- tor. The thermal cycle to produce the procedure can be found in (Ref. 21).
sions of this research will form a basis for CGHAZ was representative of the follow- The stress-relaxation tests were done as
heat treatment and welding processing ing weld parameters: 2 kJ/mm energy follows: The CGHAZ was simulated as de-
variables necessary to avoid a microstruc- input, 93°C preheat temperature, and a scribed above, cooled to room tempera-
ture susceptible to stress-relief cracking in peak temperature of 1350°C for a 12.7- ture and heated to a programmed PWHT
ferritic alloy steels and other susceptible mm steel plate (Refs. 19, 20). The samples temperature of 575, 625, 675, or 725°C.
alloys. were then cooled to room temperature The samples were loaded in tension to the

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WELDING RESEARCH

Fig. 4 — Representative SEM photomicrographs of the fracture surface of a sample that failed during testing at 675°C.

fracture surfaces were Results and Discussion


examined using a JEOL
6300f SEM operated at Stress-Relaxation Tests
10 kV. Thin foils were
prepared by mechani- The stress-relief cracking susceptibility
cally grinding 3-mm-di- was measured by the time to failure dur-
ameter disks to ~50 µm ing stress-relaxation testing. The time to
followed by ion beam failure as a function of temperature ex-
thinning to electron hibited C-curve behavior as shown in Fig.
transparency. Elemen- 1. The nose of the C-curve, or shortest
tal segregation was ex- time to failure, occurred at 675°C. Typical
amined in thin foils by light optical micrographs (cross-sectional
performing EDS lines- view) of failed samples are shown in Fig.
cans across prior 2A and B. Many cracks are present behind
austenite grain bound- the fracture edge. These cracks always oc-
aries with a VG603 curred along prior austenite grain bound-
FEG STEM. The aries approximately normal to the tensile
VG603 FEG STEM is a axis. Away from the fracture surface,
very unique instrument cracks were never observed transgranu-
due to the very high larly or along packet boundaries. Cavities
Fig. 5 — Amount of intergranular failure as a function of temperature. beam current produced were also observed along the prior austen-
in a small area. The ite grain boundaries, as illustrated in Fig.
beam size is only ~1.5 2B. Thus, the general failure characteris-
nm and the accelerating tics of the stress-relief cracking simula-
voltage is 300 kV. These tions are similar to those encountered in
displacement value corresponding to the features allow very small areas of a sample actual weldments.
0.2% offset yield strength of the CGHAZ to be analyzed without long counting times The microscopic failure mode was fur-
determined from tensile testing at temper- or sacrificing resolution. In addition, the ther investigated using scanning electron
ature. The displacement was then held small beam size allows the boundary to be microscopy to examine the fracture sur-
constant and the load was monitored as a analyzed with minimum interference from faces. The failure mode was strongly a
function of time. This test method effec- the matrix on either size of the boundary. function of test temperature. Figures 3
tively simulates the residual stresses pre- Carbide precipitation was analyzed using and 4 are representative scanning electron
sent in an actual weldment because the carbon extraction replicas. The carbides micrographs of the fracture surfaces of
maximum residual stress that can be pre- were analyzed using EDS and convergent samples that failed during testing at 575
sent is the yield strength (Ref. 22). Four to beam electron diffraction using both a and 675°C, respectively. The samples
six stress-relaxation tests were performed JEOL 2000FX TEM operating at 200 kV tested at 575°C exhibited both intergranu-
per temperature and the times to failure and the previously mentioned VG603 FEG lar failure (IG) and conventional macro-
obtained from the acquired data. STEM. Secondary electron (SE) STEM scopic ductile tearing (DT), as shown in
Failed samples were examined using imaging in the VG603 FEG STEM was Fig. 3A. Examination of the areas of in-
light optical microscopy (LOM), scanning used to resolve small precipitates on the car- tergranular failure at higher magnification
electron microscopy (SEM), and transmis- bon extraction replicas. These precipitates shows significant microductility (localized
sion electron microscopy (TEM). Samples were unresolvable using conventional TEM ductile failure comprised of microvoids) is
were prepared using standard metallo- and STEM techniques. Similar work, espe- present on the grain faces and possibly
graphic techniques and viewed in cross- cially with regard to stress-relief cracking, some small particles are also present on
section using light optical microscopy. The had not been performed prior to this study. the grain faces — Fig. 3B. In contrast, the

28 -S FEBRUARY 2003
WELDING RESEARCH
samples tested at 675°C failed almost
completely intergranularly — Fig. 4A. A
The exposed grain surfaces were covered
with microductility and small particles
similar to the samples tested at 575°C —
Fig. 4B. The amount of intergranular fail-
ure was measured from scanning electron
photomicrographs using an image analysis
system. In general, the amount of inter-
granular failure increased with increasing
test temperature, as illustrated in Fig. 5.
Samples tested at 575 and 625°C had only
40–60% intergranular failure, while those
samples tested at 675 and 725°C exhibited
80–100% intergranular failure. These re-
sults imply the prior austenite grain
boundary characteristics change with tem-
perature and, therefore, further analysis
of the grain boundaries was conducted.

Elemental Segregation

EDS linescans were done across prior


austenite grain boundaries on thin foils
prepared from samples that failed during
stress-relaxation testing to determine if el-
emental segregation, in particular if
known embrittling elements (S, P, Sn, As,
Sb, and Mn), contributed to stress-relief
cracking. Multiple boundaries (at least
three) were analyzed in each sample and
multiple linescans (at least two) were per-
formed at different locations across a
given boundary. Linescans were done by
“stepping” the beam across prior austen- B
ite grain boundaries. Approximately 64
steps were done per linescan in incre-
ments of approximately 1 nm. The bound-
ary could be analyzed with minimal inter-
ference from the matrix on either side of
the boundary because the beam size was
only ~1.5 nm. In addition, the beam cur-
rent was high enough that a sufficient
number of counts could be collected in a
small amount of time, which minimized
specimen drift. The results from typical
EDS linescans are shown in Fig. 6, al-
though not every element analyzed is
shown. The STEM photomicrographs
show the boundaries analyzed. The arrow
on the photomicrograph indicates the di-
rection of the EDS linescan (left to right
on the graphs below the photomicro-
graphs), and the “dotted” line to the left
of the arrow on the photomicrograph
shows, by virtue of the intense beam cur-
rent, the path along which the beam trav-
eled — Fig. 6A only. The graphs shown
below the photomicrograph represent the
number of X-ray counts as a function of
distance or position for a given element.
The prior austenite boundary position is

Fig. 6 — Typical EDS line scans done across prior


austenite grain boundaries. Dotted line on W1 rep-
resents boundary position. A — Sample tested at
675°C; B — sample tested at 725°C.

WELDING JOURNAL 29 -S
WELDING RESEARCH
A B C

Fig. 7 — TEM photomicrographs of extraction replicas of typical prior austenite grain boundaries in a sample failed after testing. A — 575°; B — 675°C; C —
725°C.

stress-relief cracking in
HCM2S. However, it
should be noted boron
segregation, which has
been linked to stress-re-
lief cracking in some al-
loys (Refs. 14, 15),
couldn’t be reliably de-
tected by the analytical
methods used here.

Carbide Precipitation

Transmission electron
microscopy was used to
further analyze the prior
austenite grain bound-
aries. Carbides were
identified using conver-
gent beam electron dif-
fraction patterns and
from their characteristic
Fig. 9 — TEM photomicrographs of extraction EDS spectra (Refs.
replicas of a typical prior austenite grain boundary 25–27). Typical TEM ex-
Fig. 8 — Representative EDS spectrum of Fe-rich M3C found along prior triple point containing many coarse, incoherent
traction replica pho-
austenite grain boundaries in the CGHAZ of failed stress relief cracking M C carbides. Sample tested at 675°C.
3 tomicrographs of prior
samples. Sample tested at 675°C.
austenite grain bound-
aries observed in samples
tested at 575, 675, and
indicated by the dotted line in the first boundary. Again, it appears P is enriched 725°C are shown in Fig. 7. Carbides are
graph of tungsten (W1). The only element at the prior austenite grain boundary, but visible along the prior austenite grain
enriched at the prior austenite grain the peak is statistically insignificant. boundaries. These carbides ranged in size
boundary is W. Although it may appear an Tungsten has been shown to segregate from about 50 to a few hundred nanome-
element such as Cr is also enriched at the to prior austenite grain boundaries in fer- ters and were identified as Fe-rich M3C
prior austenite grain boundary (Fig. 6A), ritic alloy steels (Ref. 24), but was found to carbides with a representative EDS spec-
a calculation to indicate statistical signifi- de-embrittle the grain boundaries. In ad- trum shown in Fig. 8. The samples tested
cance (Ref. 23) shows W is the only statis- dition, much microductility was found on at 575°C did not contain carbides at each
tically significant element enriched at the the areas of intergranular failure on the prior austenite grain boundary — Fig. 7A.
prior austenite grain boundary. Tungsten fracture surfaces. This characteristic frac- In contrast, the prior austenite grain
enrichment was found at almost every ture surface is not typical of failure due to boundaries of the samples tested at 675°C
prior austenite grain boundary at each test tramp element segregation where the are more fully covered by the M3C car-
temperature. Chromium and V segrega- areas of intergranular failure have smooth bides (Fig. 7B), and the boundaries in Fig.
tion were occasionally observed, such as in and featureless fracture surfaces. It can be 7C (725°C) are almost completely cov-
Fig. 6B, but no tramp element segregation concluded from these results that elemen- ered. The amount of grain boundary cov-
was detected at any prior austenite grain tal segregation did not contribute to erage as a function of temperature could

30 -S FEBRUARY 2003
WELDING RESEARCH
not be quantified, but, in general, the 675°C were covered
amount of grain-boundary carbides (area with carbides.
fraction or % of grain boundary area cov- Further examina-
ered) increased with increasing tempera- tion of the grain-
ture. The varying coverage along a given boundary carbides ex-
grain boundary is probably due to orienta- plains their role in the
tion mismatch between adjacent grains. In stress-relief cracking
general, increasing the degree of misori- failures. Figure 9 is a
entation (less coincident sites) makes the higher magnification
site more energetically favorable to car- view of a typical prior
bide precipitation because grain-bound- austenite grain bound-
ary energy increases with misorientation ary triple point con-
(Ref. 28). As the temperature (or time) is taining many Fe-rich
increased, the degree of misorientation M3C carbides. Most of
plays less of a role (Ref. 29). The varying these carbides have
degree of misorientation is presumably curved interfaces and
the reason almost every prior austenite are relatively coarse.
grain boundary in the samples tested at In addition, M3C car- Fig. 10 — Intragranular hardness as a function test temperature.

A B

C D

Fig. 11 — STEM photomicrographs of extraction replicas of typical intragranular regions of samples that failed during stress-relief cracking testing and accom-
panying EDS spectra. A — A dense distribution of W/Fe-rich carbides, sample tested at 575°C; B — representative EDS spectrum; C — dense distribution of
W-rich carbides, sample tested at 675°C; D — representative EDS spectrum.

WELDING JOURNAL 31-S


WELDING RESEARCH
A B

stresses. The strength relative strength of the grain interiors.


C
of the prior austenite Carbide precipitation and, to a lesser
grain interiors largely extent, dislocation density, control the
governs the ability to strength of the grain interiors. The mor-
plastically deform phology and coherency are the main fac-
globally. Hardness tors that determine the strengthening po-
measurements were tency of the precipitates. TEM and STEM
taken on samples after techniques were used to examine intra-
stress-relaxation fail- granular precipitation as a function of test
ure. The indents were temperature. Figure 11A is a secondary
placed only within the electron (SE) STEM image of a carbon ex-
prior austenite grain traction replica of a typical intragranular
interiors to minimize region in a sample tested at 575°C. SE
any contribution from STEM imaging allows for the topography
the prior austenite of a sample to be examined, and, there-
grain boundaries and fore, small particles on a film are easily ob-
the results shown in served. These small particles were unob-
Fig. 10. The hardness servable using conventional TEM
(resistance to plastic imaging. A dense distribution of small
Fig. 12 — Example of crack and cavity formation at a prior austenite grain
deformation) is ap- precipitates is visible in Fig. 11A. These
boundary. The cavities have nucleated on incoherent M3C carbides. A —
proximately equal for precipitates were found to be W and/or
LOM photomicrograph; B and C — SEM photomicrographs.
the samples tested at Fe-rich carbides that varied in size from
575, 625, and 675°C, approximately 5–20 nm with a representa-
but is significantly less tive EDS spectrum of an individual pre-
in the sample tested at cipitate shown in Fig. 11B. Individual car-
bide has the orthorhombic crystal struc- 725°C. It should be noted the use of a bides were able to be analyzed using a
ture and, therefore, has little coherency room temperature mechanical test to un- VG603 FEG STEM because the beam
with the bcc/bct ferrite matrix. The derstand elevated temperature deforma- size is only about 1.5 nm. These W/Fe-rich
amount of intergranular failure increased tion is not entirely appropriate. These carbides provided significant precipitation
with increasing temperature due to in- hardness tests were done at room temper- strengthening that resulted in the rela-
creasing amounts of intergranular M3C ature. The deformation mechanisms in tively high hardness shown in Fig. 10. A SE
carbides. However, if only grain- bound- most alloys differ between room tempera- STEM image of a typical intragranular re-
ary carbides controlled stress-relief crack- ture and elevated temperature. For in- gion in a sample tested at 675°C is shown
ing, the time to failure would be expected stance, at elevated temperatures, disloca- in Fig. 11C. A dense distribution of pre-
to decrease with increasing temperature tion climb and slip occur, but at room cipitates about 5–40 nm in size is present.
because the amount of grain-boundary temperature, only slip typically occurs These precipitates were found to be W-
carbides and intergranular failure in- (Ref. 3). In addition, stress-relief cracking rich carbides with a representative EDS
creased with increasing temperature. is a time-dependent failure, but hardness spectrum of an individual precipitate
However, the time to failure did not in- testing is time independent. Nevertheless, shown in Fig. 11D. Some V-rich carbides
crease with temperature but exhibited C- microstructural features such as precipi- were also observed. The carbide distribu-
curve behavior, as shown in Fig. 1. Thus, tates, which provide obstacles to deforma- tion is relatively coarser than the samples
another factor is contributing to the stress- tion, are likely to affect the deformation tested at 575°C, but W and V-rich carbides
relief cracking failures. response in a qualitatively similar manner are typically more coherent with the fer-
Stress-relief cracking is a function of at high and low temperatures. Thus, the rite matrix than W/Fe-rich carbides.
the material’s ability to plastically deform room-temperature hardness test should Therefore, it appears the differences in
to accommodate residual or service provide a reasonable representation of the morphology are offset by the differences

32 -S FEBRUARY 2003
WELDING RESEARCH
in composition, coherency, and morphol-
ogy resulting in similar hardness values for
the samples tested at 575 and 675°C. A

Mechanism of Stress-Relief Cracking

The above results show that the stress-


relief cracking response of HCM2S is a
balance between intergranular and intra-
granular carbide precipitation kinetics
and load relaxation. Examination of all
the samples was done postfailure. Sec-
ondary cracks and cavities were present
along the prior austenite grain boundaries
away from the fracture surface in each
sample and the exposed grain surfaces
were covered with microvoids and small
particles. From the microstructural char-
acterization, it is known that large (50 to a
few hundred nm) Fe-rich M3C carbides
are mainly present at the prior austenite
grain boundaries. Therefore, the particles
observed on the exposed grain surfaces
can be assumed to be carbides. The frac- B
ture surfaces revealed varying amounts of
macroscopic ductile tearing in addition to
intergranular failure. It seems logical to
conclude that because both the amount of
grain boundary carbides and percentage
of intergranular failure increased with in-
creasing temperature, the two are directly
related. However, the failure mechanism
cannot be fully explained at this point.
A simple, yet critical experiment was
done to isolate the role of grain boundary
carbides in these stress-relief cracking fail-
ures. Since samples tested at 575°C exhib-
ited significant amounts of both inter-
granular failure and macroscopic ductile
rupture, 575°C was chosen as the test tem-
perature for this experiment. An HCM2S
sample was stress-relief tested as every
previous sample. However, instead of al-
lowing the test to continue until the sam-
ple failed, the test was stopped after 2000 Fig. 13 — Mechanism of stress-relief cracking in the CGHAZ of HCM2S. A — During stress-relief re-
seconds. This time was chosen because the laxation; B — after failure.
average time to failure for HCM2S at
575°C was 2198 seconds. The intent was to
stop the test at a point after cracking had though these particles were not analyzed stress-relief cracking test results and mi-
initiated and close to failure. Although on this sample, knowledge of the size and crostructural characterization, the stress-
many of the cracks after 2000 seconds are distribution of precipitates along prior relief cracking mechanism in the CGHAZ
probably in the propagation stage, exami- austenite grain boundaries from TEM of HCM2S can be explained as schemati-
nation of this sample still provides insight analysis indicates the small particles pre- cally illustrated in Fig. 13. The mechanism
into crack initiation. sent on the exposed grain boundaries of is the same throughout the test tempera-
Examination of the sample using light the fracture surfaces must be Fe-rich M3C ture range, but the types of carbides and
optical microscopy revealed many cracks carbides. No other particles were found at fraction of intergranular failure vary with
along prior austenite grain boundaries, as the prior austenite grain boundaries with temperature. During exposure to a
shown in Fig. 12A, but no evidence of duc- the exception of small W/Fe-rich carbides PWHT temperature, Fe-rich M3C car-
tile rupture. This indicates failure starts by or a random inclusion. These findings bides precipitate along the prior austenite
microcracks along prior austenite grain imply cracking initiates by cavity nucle- grain boundaries and to a much lesser ex-
boundaries, but it does not explain how ation at prior austenite grain boundary tent within the prior austenite grains.
cavities initiate. Scanning electron mi- carbides. These cavities then grow, coa- Some prior austenite grain boundaries are
croscopy was then used to further examine lesce, and form microcracks. Neither cav- almost fully covered with these carbides,
the cracks. Figure 12B and C are SEM ities nor microcracks were observed at others are partially covered, and still oth-
photomicrographs of a prior austenite prior austenite grain boundaries devoid of ers are completely devoid of these car-
grain boundary showing cavities that have carbides. bides. This is presumably due to the vary-
formed in the vicinity of M3C carbides. Al- Combining these results with the ing degree of misorientation from

WELDING JOURNAL 33 -S
WELDING RESEARCH
boundary to boundary and along a given the high temperature samples (725°C). and failed due to conventional ductile
boundary. Some alloy carbides are also Unfortunately, the shared characteristics tearing. Elemental segregation did not
present along the prior austenite grain were those that increase susceptibility to play a role in the stress-relief cracking fail-
boundaries. These carbides also form a stress-relief cracking. Most of the prior ures. The results of this work provide a
fine, uniform dispersion within the grain austenite grain boundaries were covered fundamental understanding of the under-
interiors both along lath boundaries and with incoherent M3C carbides, thus weak- lying mechanisms of stress-relief cracking.
within laths. These alloy carbides provide ening the grain boundaries, as shown by In addition, this study can serve as a basis
significant precipitation strengthening. Si- the high amount of intergranular failure. for the selection of heat treatment and
multaneously, the sample is held in ten- The amount of intergranular failure in the welding processing variables necessary to
sion at a constant displacement, which re- samples tested at 675°C is only about 15% avoid a microstructure prone to stress-re-
sults in an applied load or stress that less than the samples tested at 725°C. A lief cracking in susceptible alloys.
immediately begins to relax after the max- dense distribution of small intragranular
imum load is reached. Carbide precipita- W and V-rich carbides provided signifi-
tion occurs simultaneously with the stress cant precipitation strengthening at 675°C. Acknowledgments
relaxation, and the rates of these two phe- The intragranular hardness was approxi-
nomena are functions of temperature. mately equal to that of the samples tested The authors would like to gratefully ac-
Creep-like cavities formed during the at 575 and 625°C. Therefore, the weak knowledge Dave Ackland, Adam Pap-
load relaxation at M3C/prior austenite prior austenite grain boundary regions worth, and J. Alwyn Eades of Lehigh Uni-
grain boundary interfaces as illustrated in combined with a strong grain interior re- versity for their contributions to this work.
Figs. 12B and C and 13A. Eventually, sulted in abrupt failure during the initial
these cavities linked to form microcracks stages of stress-relaxation. The bound-
along prior austenite grain boundaries. aries were covered with incoherent car- References
There were some grain boundaries that bides and subsequent cavities because the
did not have any carbides present and grain interiors were precipitation 1. Masuyama, F., Yokoyama, T., Sawaragi,
therefore no cavities formed. Cavities con- strengthened before an appreciable frac- Y., and Iseda, A. 1994. Materials for Advanced
tinued to grow until enough microcracks tion of the load could be relaxed. The load Power Engineering, Part I D. Coutsouradis et al.,
formed and all the remaining stress was could then only relax through localized eds., Netherlands: Kluwer Academic Publish-
concentrated to the areas that were still in- failure at prior austenite grain boundaries ers, pp. 173–181.
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where the remaining uncracked areas and propagation. This proposed mecha- Y., and Iseda, A. 1994. Service Exposure and Re-
could not sustain the stress and the mate- nism explains both the C-curve behavior liability Improvement: Nuclear, Fossil, and Petro-
rial failed as conventional macroscopic displayed in Fig. 1 and fracture character- chemical Plants. PVP, Vol. 288. ASME, pp.
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ductile tearing shown in Fig. 3A. In addi- cence) of the CGHAZs of HCM2S. als Park, Ohio: ASM International.
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covered with carbides experienced both ceedings Maintenance and Repair Welding in
intergranular and macroscopically ductile Conclusions Power Plants V. Orlando, Fla., pp. 16–30.
failure at the same boundary. 5. Creep Rupture Data of HCM2S Steel Tubes,
The samples tested at 725°C experi- The stress-relief cracking of a new fer- Pipes, Forgings, and Plates. 1997. Sumitomo
enced almost total intergranular failure ritic alloy steel was investigated and a Metal Industries, Ltd., and Mitsubishi Heavy
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similar even though the resultant fracture grain interiors were resistant to plastic de- ing Journal 50(6): 247-s to 252-s.
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Miami, Fla.: American Welding Society. gical Transactions A 13A: 557–563.

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WELDING JOURNAL 35 -S