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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
WELDING JOURNAL 27 -S
WELDING RESEARCH
Fig. 4 — Representative SEM photomicrographs of the fracture surface of a sample that failed during testing at 675°C.
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
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.
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
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
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34 -S FEBRUARY 2003
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2) Introduction. A short statement giving relevant published. Figures should be original line art or glossy
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reader. Do not duplicate the abstract. submitted by electronic means. To receive complete
3) Experimental Procedure, Materials, Equipment. instructions and the manuscript submission form, please
4) Results, Discussion. The facts or data obtained contact the Peer Review Coordinator, Doreen Kubish, at
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remember.
6) Acknowledgment, References and Appendix.
WELDING JOURNAL 35 -S