Scripta Materialia 51 (2004) 683 – 688

www.actamat-journals.com

Microstructural study of weld fusion zone of TIG welded

IN 738LC nickel-based superalloy
O.A. Ojo, N.L. Richards, M.C. Chaturvedi *

Department of Mechanical and Industrial Engineering, University of Manitoba, Room 356, Engineering Building, Winnipeg, MB, Canada R3T 5V6

Received 22 April 2004; received in revised form 12 June 2004; accepted 15 June 2004
Available online 8 July 2004

Abstract

The weld fusion zone microstructure of a commercial aerospace superalloy IN 738 was examined. Elemental segregation induced
interdendritic microconstituents were identified to include terminal solidification product M3B2 and Ni7Zr2 in association with c – c 0
eutectic constituent, which require proper consideration during the development of optimum post weld heat treatment.

2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Nickel alloys; Welding; Solidification; Microstructure

1. Introduction heat treatment (PWHT) is usually applied as a remedy

The weldability of heat resistant nickel base superal-
loys has gained importance because of the wide use of
welding to fabricate and repair hot section components
of aero and industrial gas turbine engines that are made
from these materials. Microstructural development in
superalloy welds, which invariably controls properties
and reliability of the weldments, can be significantly
influenced due to microsegregation and non-equilibrium
phase transformation that occur during solidification.
Dendritic microsegregation is known to often result in
formation of intermetallic secondary solidification con-
stituents along dendrite interstices as well as inhomoge-
neous distribution of second phase precipitate particles
[1 – 4]. In some cases important strengthening elements
may be tied up in the resultant non-equilibrium interme-
tallic particles, which could also exhibit other damaging
effects on high temperature performance [1]. Post weld
*
Corresponding author. Tel.: +1-204-474-6675; fax: +1-204-261-
6735.
E-mail address: mchat@cc.umanitoba.ca (M.C. Chaturvedi).
to most superalloy weldments to modify the as-weld
microstructure and relax residual welding stresses in
order to impart optimum reliable properties. It has been,
however, recognized [1] that the response of superalloy
welds to PWHT is controlled primarily by the as-weld
microstructure of the weldment.
Inconel 738 is a c 0 -(Ni3Al,Ti) precipitation hardened
nickel base superalloy which, like other superalloys con-
taining high Al and Ti concentration, is highly suscepti-
ble to microfissuring during welding and PWHT [5].
Cracking during welding of this alloy has been attrib-
uted mostly to large shrinkage stresses occurring as a re-
sult of rapid c 0 precipitation during weld cooling [6].
Nevertheless, Ojo et al. [7] have recently reported that
besides this factor, c 0 particles contribute to microfissur-
ing during welding of IN 738 in a significant way by con-
stitutionally liquating in the heat affected zone (HAZ).
However, very limited information is available in the lit-
erature about the as-weld fusion zone microstructures of
IN 738, which is considered fundamental to its response
to PWHT. Therefore, the present work was initiated
with the objective of studying microstructures that de-
velop in the weld-metal zone of tungsten inert gas

1359-6462/$ - see front matter
2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2004.06.013
684 O.A. Ojo et al. / Scripta Materialia 51 (2004) 683 – 688

(TIG) welded IN 738 alloy, to help develop a more suit- 3. Results

able PWHT schedule that would result in minimal
microfissuring and reliable microstructure and 3.1. Optical metallography and electron microprobe
properties. This communication reports and discusses analysis
microsegregation pattern and the ensuing microconstit-
uents in the weld metal zone upon solidification and Fig. 1 shows optical micrograph of the fusion zone
cooling. consisting of cellular-dendritic microstructure. The
chemical composition of at least 15 points in the central
dendrite core regions was determined by EPMA/WDS
and is given in Table 1. The distribution/partition coef-
2. Experimental procedures ficient k of the alloying elements, which describes the
direction and extent of microsegregation during solidifi-
The as-received Inconel 738LC superalloy was in the cation, was determined from this data. Under equilib-
form of 2.5 · 0.5 · 0.6 cm cast plates and its compositions rium conditions and by neglecting undercooling at the
was (wt%) 0.11C, 15.84Cr, 8.5Co, 2.48W, 1.88Mo, dendrite tips, the first solid to form from the liquid,
0.92Nb, 0.07Fe, 3.46Al, 3.47T, 1.69Ta, 0.04Zr, 0.012B which is the dendrite core will have a composition of
balance nickel. 7.6 · 2.5 · 0.3 cm rectangular plates, kC0, where C0 is the nominal composition of the alloy
with a 0.13-cm deep V-groove were machined from the and k is the equilibrium partition coefficient [8]. There-
as-received material. They were given the standard solu- fore, the ratio between dendrite core composition and
tion treatment of 2 h at 1120 C followed by argon the nominal composition will yield the partition coeffi-
quenching. The heat-treated samples were tungsten gas cient at the beginning of solidification process. Another
arc (TIG) welded with IN 738 filler wire, using a current implicit assumption of this approach is that the solute
of 60 A DC and 10 V. The welding torch and wire elements exhibit negligible diffusion in the solid during
speeds were maintained at 76 and 304 mm/min, respec- solidification. The extent of solid-state diffusion during
tively. Welded samples were sectioned transversely to solidification would depend on the cooling rate and
the weld and polished using standard metallographic interdendritic arm spacing. The secondary dendrite
techniques. The fusion zone microstructure was ex- arm spacing along fusion zone centerline in the present
amined and analyzed by optical microscope, JEOL
5900 scanning electron microscope (SEM), JEOL
2000FX transmission electron microscope (TEM), both
equipped with an ultra thin window Oxford energy dis-
persive spectrometer (EDS), and a Cameca MBX elec-
tron probe microanalyser (EPMA) equipped with /
(p,z) correction algorithm. X-ray microanalysis using
theoretical Cliff – Lorimer k factors and selected area
diffraction analyses were performed in TEM on inter-
dendritic constituents extracted on carbon extraction
replicas, and on those present in thin foils prepared from
the weld fusion zone. Extraction replicas were prepared
through standard technique with a solution of 10 ml
HCL and 1 g of tartaric acid in 90 ml of methanol at
3 V. Thin foils were produced by twinjet polishing with
25% perchloric acid in 75% methyl alcohol at
20 to

40 C using a current of 1.8 – 3.5 A. Fig. 1. Optical micrograph of the fusion zone.

Table 1
Chemical composition of dendritic core and various phases present in weld fusion zone
Elements Ni Cr Co Al Ti Ta Nb Mo W Zr C B
Dendrite core (wt%) 63.16 15.52 9.28 3.19 2.43 1.24 0.48 1.64 2.81 0.005 – –
k 1.03 0.98 1.09 0.92 0.69 0.74 0.52 0.87 1.13 0.13 0.3 [10] 0.008 [10]
MC carbide (at%) 2.4 9.1 0.6 – 40.9 17.8 18.2 4.8 6.2 – – –
M3B2 boride (at%) 4.2 63.9 2.3 – 1.3 – 3.4 18.9 4.3 1.7 – –
Ni7Zr2 (at%) 63.1 2.6 5.4 – 1.6 4.0 2.3 – – 21 – –
 O.A. Ojo et al. / Scripta Materialia 51 (2004) 683 – 688
work was between 3.3 and 4.5 lm, with an average value
of 3.75 lm. The cooling rate within the fusion zone was
estimated to be about 550 C/s by using the empirical
data obtained for IN 738 on the relationship between
cooling rate and secondary dendrite arm spacing [9].
Such rapid cooling rate could appreciably limit the ex-
tent of solute back-diffusion. The initial partition coeffi-
cients at the start of solidification of the metallic
alloying elements were calculated and are listed in Table
1. The result indicates that W and Co with k > 1 segre-
gate to the dendrite core while Mo, Ta, Ti, Nb, Zr
and Al with k < 1 enrich the interdendritic regions. Ni
and Cr having k values approximately equal to unity
tend to exhibit uniform distribution between dendrite
core and dendrite interstices. The microsegregation pat-
tern of the alloying elements observed in the present
work are in close agreement with those reported in other
superalloys welds [2,4]. The partition coefficients of B
and C were not determined in the present work due to
difficulty in quantifying these light elements with suffi-
cient accuracy and the fact that effect of back-diffusion
of interstitial elements can be significant during solidifi-
cation. However, values estimated from their Ni – X bin-
ary phase diagram [10] are likewise listed in Table 1. It
should be noted that the partition coefficients are not
necessarily constant during solidification process, but
they explain well the formation of interdendritic micro-
constituent as would be discussed shortly. In addition, in
the case of solute buildup at dendrite tips, the initial so-
lid to form will have a higher composition as compared
to the case of no solute buildup, assumed in the present
approach, and lead to a higher measured value of k.
Hence, the obtained k values reported here provide an
upper bound when k < 1.
3.2. Scanning electron microscopic examination
Fig. 2 shows a typical SEM micrograph of the fusion
zone. No evidence of centerline solidification cracking
Fig. 2. SEM micrograph of the fusion zone.
685
was observed in any of the welded samples, however,
occurrence of microporosity mainly associated with
some eutectic regions was observed at higher magnifica-
tion. The interdendritic region consisted of discrete
second phase particles with blocky, rod-like and Chi-
nese-script like morphologies and isolated c – c 0 eutectic
with its usual characteristic mode of formation consist-
ing of the ‘‘crown’’ region protruding into the last to
solidify liquid [11] (inset of Fig. 2). Preliminary SEM/
EDS microchemical analysis of the interdendritic dis-
crete particles suggested them to be based on MC type
carbides, which was confirmed by TEM analyses. Based
on aerial fraction analysis, the volume fraction of c – c 0
eutectic islands was estimated to be between 2% and 3%
while that of the discrete interdendritic particles was be-
tween 1.5% and 2%. Different second phase particles en-
riched in Ni and Zr and others in Cr and Mo were
observed in front of some of the c – c 0 eutectic (Fig. 2).
In addition, careful SEM examination at higher magni-
fication suggested that the observed variation in contrast
in interdendritic regions, which is most prominent
around the c – c 0 eutectic could be due to precipitation
of closely spaced fine c 0 precipitates which could not
be resolved appropriately by SEM.
3.3. Analytical transmission electron microscopic exam-
ination
TEM/EDS X-ray microanalysis of interdendritic con-
stituents extracted on carbon extraction replicas showed
that most of the particles have a composition similar to
those of MC type carbides in the base metal (Table 1).
Analysis of electron diffraction patterns confirmed them
to be FCC-MC carbides with a lattice parameter of 4.36
Å. TEM examination revealed that some of these car-
bides existed in the form of coarsely lamellar and dendri-
tically shaped particles (Fig. 3). The inset in Fig. 3 shows
the diffraction pattern with [0 0 1] zone axis of the car-
bide particle. Apart from the carbides, the only other
Fig. 3. TEM micrograph of coarsely lamellar and dendritically shaped
MC type carbide with SADP from [0 0 1] zone axis.
686 O.A. Ojo et al. / Scripta Materialia 51 (2004) 683 – 688
Fig. 4. TEM micrograph of M3B2 boride extracted on carbon
extraction replica with SADP from ½1 1 2 zone axis.
phase observed on carbon extraction replicas was
Cr – Mo rich particle mostly in regions which had the
topography of c – c 0 eutectic constituent (Fig. 4). Thin
foil examination likewise showed the presence of a sim-
ilar phase associated with c – c 0 eutectic regions (Fig. 6).
SADP analysis and TEM/EDS x-ray microanalysis indi-
cate the phase to be tetragonal M3B2 boride with lattice
parameters of a = 5.71 Å and c = 3.05 Å (Fig. 4 and
Table 1). Fig. 5 shows a typical TEM/EDS spectrum
from a boride particle. As can be seen, boron was de-
tected by the ultra thin window EDS detector and the
strong Cr and Mo peaks are characteristic of M3B2 bo-
ride EDS spectra observed in other Ni base superalloys
[12].
In addition to M3B2 boride, the Ni – Zr rich phase ob-
served in SEM was also found in thin foils by TEM
examination (Fig. 6). The chemical composition of this
phase as determined by TEM/EDS is given in Table 1.
This type of Ni – Zr intermetallic phase has not been
previously reported in IN 738 alloy. A review of Ni –
Zr binary phase diagram [13] reveals that two interme-
tallic phases Ni5Zr and Ni7Zr2 form at Ni rich corner
Fig. 5. TEM/EDS spectrum from a M3B2 boride particle.
Fig. 6. TEM micrograph of a thin foil from fusion zone showing M3B2
and Ni7Zr2 associated with c – c 0 eutectic region.
of the Ni – Zr system (Ni5Zr fi 14.85 – 18.4 at% Zr and
Ni7Zr2 fi 22.2 at% Zr). Ni7Zr2 is, however, shown to
melt congruently, suggesting that in the liquid with a
composition close to this, Ni7Zr2 would form first on
solidification. In IN 738 weld metal, severe positive seg-
regation of Zr during solidification could enrich the
interdendritic liquid such that Ni7Zr2 forms during the
terminal stages of solidification. Jayanth et al. [14] in
their study of phase equilibria in the Ni rich portion
of Ni – Al – Zr ternary system reported a dominant pres-
ence of Ni7Zr2 compared to Ni5Zr in the Ni – Al – Zr
phase equilibria. The chemical composition given in
Table 1 suggests the phase to be based on Ni7Zr2. This
was confirmed by TEM selected area diffraction pattern
analysis of the particles, which indicated them to be
based on monoclinic Ni7Zr2 phase with lattice para-
meters of a = 4.82 Å, b = 8.22 Å, c = 11.13 Å and
b = 96.7. Fig. 7 shows SADP from a particle of this
phase at [1 0 1] zone axis. A phase of similar chemical
composition as, determined by EPMA, and considered
to be (Ni,Co)7Zr2 has been reported in a Zr doped Ni
base superalloy IN 100 [15].
Fig. 7. SADP from a Ni7Zr2 particle at [1 0 1] zone axis.
 O.A. Ojo et al. / Scripta Materialia 51 (2004) 683 – 688
Fig. 8. TEM dark field image of c 0 precipitate particles with
superlattice reflections at ½1 1 2 zone axis.
Fig. 9. TEM micrograph showing inhomogeneous c 0 distribution
within interdendritic region.
In addition to those solidification constituents men-
tioned, precipitation of c 0 particles was observed in all
the thin foils from fusion zone. Fig. 8 shows a TEM
dark field micrograph obtained using a superlattice
reflection from c 0 precipitate particles with ½1 1 2 zone
axis. However, the morphology and size of the c 0 phase
were observed to vary depending on their location. Re-
gions around the interdendritic c – c 0 eutectic were
found to contain the coarsest c 0 precipitates (Fig. 9).
4. Discussion
The microstructural development in the fusion zone
of a weld is largely dominated by two interrelated solid-
ification occurrences, dendrite formation and solute par-
titioning. The first solid to form from the weld pool was
in the form of c dendrites. During their continued for-
mation, solute elements with partition coefficient k < 1
were rejected into interdendritic liquid at the dendrite/
liquid interface. Continual solute enrichment of the
687
interdendritic liquid could cause the solubility limit of
the primary solidification phase, c matrix, to be ex-
ceeded, such that secondary solidification constituent
are formed between the dendrites. In nickel base super-
alloys, several secondary solidification constituents are
possible including carbides, borides, eutectic c 0 and a
number of other intermetallic phases. In IN 738 alloy,
substantial positive dendritic microsegregation of strong
carbide forming elements, Ti, Nb, Mo and Ta along
with C, which also exhibits limited solubility in Ni,
would eventually result in the formation of interdendrit-
ic MC carbides. This is most likely to occur via a mono-
variant L fi c + MC eutectic-type transformation, as
supported by the observed coarsely lamellar and dendri-
tically shaped carbide particles (Fig. 3).
On further cooling, supersaturation of remaining
interdendritic liquid with c 0 forming elements Ti, Al,
Nb and Ta due to continual enrichment would eventu-
ally be relieved through the formation of c – c 0 eutectic.
The c
c 0 eutectic formation has been reported to occur
over a range of temperatures in PWA 1480 [2] and IN
738 superalloys [16]. Based on the results of differential
thermal analysis (DTA) experiments, it is generally
believed that solidification of IN 738 is completed by
c – c 0 eutectic transformation at around 1200 C [17].
However, Zhu et al. [18] in their study of solidification
behavior of some Ni base superalloys, reported that in
an alloy, which is close to IN 738 in composition, there
existed a liquid pool ahead of solidified c – c 0 eutectic
which could not complete the solidification process until
the temperature was lowered below 1120 C. Similar
observation was also made by Zou et al. [19] in another
derivative of IN 738 alloy. These results [18,19] thus sug-
gest that contrary to the generally held view that solidi-
fication of IN 738 is completed by L fi c – c 0 eutectic
transformation, a different terminal solidification reac-
tion involving formation of other intermetallic phases
could be occurring in this alloy. During the formation
of c – c 0 eutectic, further solute partitioning, involving
rejection of solute atoms with low solubility in c and
c 0 phases into the residual liquid phase ahead of the
formed c – c 0 eutectic could occur. In such a case, Zr
and B which have limited solubility in c and c 0 phases
(though more Zr can dissolve in c 0 than in c) and exhibit
severe positive segregation in Ni alloys, would preferen-
tially segregate into the liquid phase. Considering the
high affinity of Cr and Mo for B, these elements could
also segregate into the residual liquid in front of c – c 0
eutectic constituent. In addition, Zhu et al. [11] have re-
ported that Cr and Mo exhibit positive segregation into
the residual liquid phase during c – c 0 eutectic transfor-
mation in a Ni base superalloy.
On continuous cooling to the invariant terminal
solidification reaction temperature for the alloy i.e. the
effective solidus temperature, high concentration of sol-
ute elements in the final liquid would invariably result in
688 O.A. Ojo et al. / Scripta Materialia 51 (2004) 683 – 688
the formation of terminal solidification product rich in
these elements. This presumably could explain the pres-
ence of Cr – Mo rich M3B2 boride and Ni7Zr2 based
intermetallic compound associated with interdendritic
c – c 0 eutectic in the fusion zone of this alloy. It is also
possible that the M3B2 boride and Ni7Zr2 formed to-
gether with c – c 0 eutectic by complex terminal eutec-
tic-type transformation as suggested by Babu et al. [3].
c 0 precipitate particles would start forming within the
supersaturated c dendrite when the temperature is suffi-
ciently lower than the c 0 solvus temperature to initiate
nucleation during cooling. Inhomogeneous distribution
of c 0 particles involving fine c 0 precipitates within the
dendrite core compared to coarse eutectic c 0 particles
in the interdendritic regions is likely to cause a deterio-
ration in high temperature performance and is one of
the main factors that normally necessitates the use of
PWHT to homogenize and restore properties of superal-
loy weldments.
A potential cause of problem during PWHT in the
present alloy, particularly during the initial stage of
common PWHT cycle involving rapid heating to solu-
tion heat treatment temperature, is the presence of the
low melting terminal solidification constituent M3B2
and Ni7Zr2 in association with c – c 0 eutectic in the fu-
sion zone. Incipient eutectic melting of these constitu-
ents either during the heating cycle or during solution
treatment could reduce the resistance to PWHT crack-
ing and/or degrade the final properties of the weldment.
A DTA study of nickel base superalloys [20] has shown
the occurrence of eutectic melting of Ni – Zr intermetal-
lic at 1154 – 1184 C. This temperature range is close to
the interdendritic c 0 solvus in IN 738 superalloy (1170 –
1180 C) [16]. A Ni – Zr intermetallic compound of com-
position similar to that observed in the present work has
been reported to cause low temperature incipient melt-
ing and reduction in strengthening efficiency of Zr in
cast Mar-M200 superalloy [21]. In the same context,
rapid heating to temperatures just above c-M3B2 eutec-
tic, which was below the c 0 solvus have been also re-
ported to cause incipient melting in IN 100 superalloy
[22]. Besides, significant amount of Zr and B, which
are grain boundary strengthening elements in IN 738,
might be tied up in the Ni7Zr2 and M3B2 particles,
respectively. It has been reported that heat treatments
at 982 C [15] and 1130 C/3 h [21] would prevent low
temperature incipient eutectic melting of Ni – Zr inter-
metallic in IN 100 and Mar-M200 superalloys, respec-
tively. It is envisaged that similar annealing heat
treatment prior to c 0 solution heat treatment portion
of PWHT might also prevent such incipient melting in
the present alloy. Further work is being planned based
on the result of the present work for the development
of a suitable PWHT for IN 738 alloy.
5. Summary and conclusions
Elemental microsegregation during TIG weld metal
solidification of IN 738 resulted in the formation of
secondary solidification constituents MC type carbides,
c – c 0 eutectic, M3B2 boride and Ni7Zr2 intermetallic
compound within interdendritic regions. Consideration
of the presence of low melting terminal solidification
product consisting M3B2 and Ni7Zr2, is pertinent to the
development of an optimum PWHT cycle for the alloy.
Acknowledgments
The authors would like to thank the consortium of
Manitoba aerospace industries and NSERC for the
financial support. One of the authors (OAO) also
acknowledges gratefully the award of Graduate Fellow-
ship from NSERC and the University of Manitoba.
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