MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5

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Transient liquid phase bonding of FSX-414 superalloy at the

standard heat treatment condition

R. Bakhtiari⁎, A. Ekrami
Department of Materials Science and Engineering, Sharif University of Technology, Tehran, 11115-9466, Iran

AR TIC LE D ATA ABSTR ACT

Article history: The as-cast samples of FSX-414 Co-based superalloy were heat treated at the standard
Received 26 August 2011 solution and aging heat treatment cycles. Specimens for joining were cut from the as-cast
Received in revised form ingot. Transient liquid phase (TLP) bonding was carried out at the standard solution cycle,
1 February 2012 using MBF-30 interlayer. Also, bonded specimens were homogenized at the standard aging
Accepted 3 February 2012 condition.
The microstructure of the as-cast, heat treated and TLP bonded specimens were studied.
Keywords: These studies showed that the non-uniform distributed carbides of the as-cast specimen
TLP bonding were replaced by uniform ones during the heat treatment. Eutectic M23C6 carbides were
FSX-414 superalloy observed in all specimens. Due to the complete isothermal solidification, no eutectic
Solution structure was observed in the bond region of bonded specimens. In the diffusion affected
Aging zone (DAZ) of these specimens, some intermetallics of the Co\B system were seen. Line
scan EDS analysis across the bonding zone of the homogenized joint showed more uniform
distribution of alloying elements in comparison with the unhomogenized joint.
Hardness profiling across the bonding zone showed that isothermal solidification zone's
(ISZ) hardness in the homogenized specimen is closer to the base metal (BM) hardness in
comparison with the unhomogenized specimen. A hardness peak was observed in the
DAZ region of the both homogenized and unhomogenized joints. Shear strength and
shear fracture energy of the homogenized joint were about 93% and 82% those of the base
metal, respectively. More fibrous zones and smaller dimples were observed at the homogenized
joint's fracture surface, in comparison with the unhomogenized one.
© 2012 Elsevier Inc. All rights reserved.

1. Introduction FSX-414, a GE-patented Co-based alloy, is the current alloy

Nozzles of gas turbines are stationary airfoils that direct the
hot gas path flow onto the rotating buckets. They must be
able to withstand high temperatures. The first stage nozzles
of gas turbines are subjected to the highest gas path tempera-
ture but to lower mechanical stresses in comparison with the
rotating buckets. As a result, the first stage nozzles must have
excellent resistance to thermal fatigue, as well as to high tem-
perature oxidation and corrosion [1,2].
used for production of first stage nozzles and some later-stage
nozzles. Co-based alloys generally possess superior strength at
very high temperatures, compared with the Ni-based alloys
[3]. In addition, the oxidation resistance of FSX-414 is such
that it is currently used with no protective oxidation coating [1].
After 24,000 hour service interval of a segment of FSX-414
nozzles, extensive cracking has been reported, especially
around the leading and trailing edges as well as between the
two airfoils. Low cycle thermomechanical fatigue caused the

⁎ Corresponding author at: PhD candidate at Sharif University of Technology and Visiting Researcher at University of Calgary. Tel.: +98 912
2720166; fax: +98 21 66005717.
E-mail addresses: r_bakhtiari@mehr.sharif.edu (R. Bakhtiari), ekrami@sharif.edu (A. Ekrami).

1044-5803/$ – see front matter © 2012 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2012.02.002
 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5
primarily cracking. Some oxidative erosion and associated
cracking has also occurred [4]. Repair of these nozzle seg-
ments is important due to their high price. Prior to 2003,
cracks on these nozzle segments were repaired with the gas
tungsten arc welding process. The large amount of welding
required resulted in considerable distortion of the nozzle
segments. This distortion required significant rework
and dimensional correction [5]. In 2004, GE's energy team
reviewed the activated diffusion healing (ADH) technology.
After that, a liquid phase diffusion sintering process was
developed to successfully repair wide and deep cracks as
well as the craze-cracks [6].
Transient liquid phase (TLP) bonding is considered the pre-
ferred repairing/joining process for superalloys. This hybrid
process combines beneficial features of both liquid-phase
bonding and solid-state bonding. This process differs from
diffusion bonding in that the formation of the liquid interlayer
eliminates the need for a high bonding pressure. In TLP an
interlayer, which contains melting point depressant elements
such as B, P, and Si, is inserted between two surfaces to be
joined. The assembly is then heated to above the interlayer
melting point. The bonding time should be sufficient to
cause isothermal solidification of the joint due to the compo-
sitional change between the joint and the base metal (BM).
Post-bond heat treatment can be used to homogenize the
joint region and brings about its compositional and micro-
structural homogeneity with the base metal [7–9].
The microstructure of as-cast FSX-414 contains non-
uniform distributed carbides within the austenitic matrix. So-
lution and aging heat treatment is common to redistribute the
carbides and change their morphology in order to enhance the
properties [10,11]. From an industrial perspective, performing
the TLP bonding and heat treatment of nozzles simultaneous-
ly is desirable as it reduces the cost.
TLP bonding of the FSX-414 Co-based superalloy at the stan-
dard solution cycle and homogenizing the bonded specimens
at the standard aging cycle are the aims of this research. The re-
lated application is manufacturing the nozzles of this superalloy
in multi parts and then bonding the parts using TLP. In this way,
the design of castings and the cores will be more simple. To eval-
uate the industrial application of this research, microstructural
studies and mechanical tests were conducted.
2. Materials and Experimental Procedures
An ingot of FSX-414 superalloy, with the chemical composi-
tion given in Table 1, was used in this investigation. For TLP
bonding, 10 × 10 × 5 mm coupons were sectioned using an
electro-discharge machine. Contacting surfaces were ground
using 600 grade SiC papers and then were ultrasonically
cleaned in an acetone bath. An MBF-30 interlayer, with chem-
ical composition shown in Table 1, was then inserted between
Table 1 – Chemical composition of the FSX-414 superalloy and MBF-30 interlayer (wt.%).
Co Cr Ni W Fe
FSX-414 Bal 30.25 10.32 6.76 0.52
MBF-30 – – Bal – –
39
two coupons of the base metal. The interlayer was in the form
of an amorphous foil with thickness of 75 μm. Selection of the
Ni-based interlayer was due to the possible strengthening
mechanisms of a Ni substrate at the joint. High temperature
steel fixture was used to fix the coupons. This fixture also re-
duced metal flow during the TLP bonding. Specimens were
bonded at the standard solution cycle (at 1150 °C for 4 h) and
some of the bonded specimens were homogenized at the
standard aging cycle (980 °C for 4 h). These cycles are the stan-
dard homogenizing and aging heat treatment for the FSX-414
superalloy. The interlayer liquidus and solidus temperatures
are 1054 and 894 °C [12], respectively, which bracket the bond-
ing temperature.
Microstructure of the as-cast and heat treated base metal
was investigated. Also, the bonded specimens' microstructure
at sections perpendicular to the bond line was studied, using
an optical microscope and a scanning electron microscope
(SEM). Murakami and Kalling's etchants were used for the mi-
crostructural studies. Semi-quantitative chemical analysis of
the observed phases was conducted on a SEM, equipped
with a beryllium window energy dispersive spectrometer
(EDS) system. The software used in this system was INCA.
The X-ray diffraction (XRD) patterns were recorded in a
Guinier–Hägg camera using monochromatic Cukα1 radiation
of a Rigaku Multiflex X-ray diffractometer. The characterization
was conducted using JADE 6.5 software.
Vickers hardness tests were carried out for all specimens
using a 98 N load. Microhardness across the joint of bonded
specimens was measured using a 0.5 N load on a Buehler
microhardness tester.
Room temperature shear tests were carried out for both
the bonded specimens and the base metal, using a fixture
schematically shown in Fig. 1. These tests were performed
on an Instron tensile machine at a cross-head speed of
1.7 × 10− 5 m/s. The shear fracture energy was calculated
from the force–displacement graph. The fracture surfaces
were studied using a stereo microscope, an optical microscope
and the SEM.
The applied stress during the shear test is focused entirely
on the joint, while this stress could be focused on the base
metal during the tensile test. Therefore, the shear test is a
more appropriate test to evaluate the mechanical properties
of the joints, in comparison with the tensile test. Selection of
the shear test in this research was according to this.
3. Results and Discussion
3.1. Superalloy Studies
3.1.1. Microstructural Studies
Fig. 2 shows microstructures of the as-cast and the heat
treated specimens. Distribution of carbides in an austenitic
C Mn Mo Ta B Si
0.15 0.59 0.03 0.14 0.006 0.72
0.06 – – – 3.2 4.5
40 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5
Fig. 1 – Schematic design of shear test fixture.
matrix is visible in this figure. The as-cast microstructure
contains non-uniform distributed carbides (Fig. 2a). These
carbides are M3C2, M7C3 and M23C6, which are the common
carbides of FSX-414 superalloy's microstructure [5,13,14].
These chromium carbides, containing Co, W or Mo in sub-
stitution of Cr, precipitate intragranularly during cooling
from the casting temperature. These coarse and blocky
Fig. 2 – Microstructures of specimens at the (a) as-cast,
(b) solution and (c) solution + aging heat treatment
conditions.
carbides form with a semirounded morphology. The as-
cast carbides such as M3C2 and M7C3 are unstable at high
temperatures and precipitate in the form of finer M23C6 car-
bides [15].
Fig. 2b and c shows more uniform distribution of the car-
bides in the heat treated microstructure in comparison with
the as-cast one. This uniformity is more for specimens heat
treated at solution + aging cycles. M23C6 carbide forms an eu-
tectic structure consisting of alternate sheafs of M23C6 and γ
matrix [10]. Fig. 3a shows this structure in the as-cast micro-
structure. EDS analysis of different phases of Fig. 3a is given
in Table 2. The analysis of the light phase is similar to the ma-
trix. The dark phase composition is consistent with a high
chromium carbide containing Co and W. This phase could be
the M23C6 carbide. Similar results are obtained for the speci-
men heat treated at solution + aging cycles (Fig. 3b). The XRD
pattern of this specimen shows the peaks of Cr23C6 and (Ni,
Co,Cr)23C6 phases (Fig. 4). These results show that M23C6 car-
bides are retained after heat treatment. The reason is that
the eutectic islands are not generally affected during heat
treatment of the superalloy [10].
3.1.2. Hardness
Fig. 5 shows the hardness values of various microstructures.
The hardness of the as-cast specimen is the highest. The
coarse and blocky primary carbides with non-uniform inter-
granular distribution cause the high hardness value. As a re-
sult of solution heat treatment, carbide distribution becomes
uniform and the primary carbides, such as coarse grain
boundary ones, dissolve. This causes partial homogenizing
of the as-cast structure as well as a hardness reduction.
Aging treatment increases the hardness due to the formation
of secondary fine carbides.
3.2. TLP Microstructures
Fig. 6 shows microstructure of the specimens after bonding +
homogenizing. The bond region consists of two distinct
zones which are the isothermally solidified zone (ISZ) and dif-
fusion affected zone (DAZ). There is no eutectic structure
within the ISZ. This means that the bonding time is sufficient
to complete the isothermal solidification.
Some needle-like phases are visible in the DAZ of Fig. 6.
EDS compositional analysis of these phases in the microstruc-
tures of both the bonded and bonded + homogenized speci-
mens shows that they are cobalt-boride intermetallics. The
formation of the intermetallic phases in the DAZ is due to
the diffusion of boron from the interlayer to the base metal
during the bonding. Co2B and CoB are two types of intermetal-
lics of the Co\B system. Their melting points are 1280 and
1460 °C, respectively [16], which are greater than the bonding
and homogenizing temperatures. These brittle intermetallics
can affect the mechanical behavior of the joint. The existence
of intermetallics at DAZ of the homogenized joint indicates
that homogenizing treatment is not able to dissolve these
phases completely.
The homogenizing stage is assumed to follow the comple-
tion of the isothermal solidification stage and is usually done
at a temperature different from the bonding temperature [9].
During the homogenizing treatment, concentration of melting
 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5 41

Fig. 3 – SEM micrographs of eutectic carbides at the (a) as-cast and (b) solution + aging heat treated conditions.

point depressant (MPD) element decreases at the bonding
zone while the base metal solute element's concentration in-
creases at this zone. Fig. 7 shows line scan EDS analysis across
the bonding zone of both the homogenized and the unhomo-
genized specimens. Concentrations of the alloying elements
such as Co, Ni and Cr at bonding zone of the homogenized
specimen are closer to those of the base metal, in comparison
with the unhomogenized specimen. This difference shows
that during the homogenizing process, diffusion of solute ele-
ments from the base metal to the bonding zone is consider-
able. For example, Fig. 7 shows the relatively uniform
distribution of Si across the bonding zone of the homogenized
specimen.
specimen. During the homogenizing treatment, diffusion of
the base metal alloying elements into the bonding zone
causes solid solution strengthening as well as an increase in
hardness. In addition to carbide strengthening, solid solution
strengthening is the essential strengthening mechanism of
the FSX-414 superalloy [10].
The hardness peak at the DAZ of Figs. 8 and 9 can be related
to the stable intermetallics, such as Co2B and CoB, at the

3.3. Microhardness

Hardness profiling across the bonding zone is a quantitative

measurement of mechanical property variation. This profile
can be used to assess the degree of homogenization as well
as the effect of secondary precipitates on the mechanical
properties [17]. Figs. 8 and 9 show the hardness profile of the
joints before and after the homogenizing treatment, respec-
tively. These profiles indicate three distinct zones. Interdiffu-
sion of alloying elements between the bonding zone and the Fig. 4 – XRD pattern of the solution + aging heat treated
base metal determines the hardness of ISZ. The hardness uni- specimen.
formity at ISZ shows that there is no eutectic phase in this
zone and the isothermal solidification is complete. The ISZ
hardness of the homogenized specimen is closer to the base
metal hardness, in comparison with the unhomogenized

Table 2 – Chemical composition of different phases of

Fig. 3a (wt.%).
Matrix Light phase Dark phase

C 0.10 0.17 1.78

Cr 28.82 31.34 70.17
W 2.47 4.35 9.97
Co 55.16 50.02 14.65
Fig. 5 – Comparison of the base metal's hardness at the as-cast,
Ni 12.80 11.59 2.88
solution and solution+ aging heat treatment conditions.
42 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5

Fig. 6 – SEM micrograph of the homogenized joint.

bonding and homogenizing temperatures. This is consistent
with the microstructural studies (Fig. 6).
3.4. Shear Strength
Fig. 10 shows the values of shear strength and shear fracture
energy of TLP bonded specimens and the base metal. Shear
strength and shear fracture energy of the homogenized spec-
imen are respectively about 93% and 82% of the base metal
at the same heat treatment condition. Both shear strength
and shear fracture energy of the unhomogenized specimen
are lower than those of the homogenized one. These strength
and energy are about 71% and 51% of the base metal,
respectively. The shear strength difference between the ho-
mogenized and unhomogenized specimens indicates the ef-
fect of homogenizing on strengthening of the bonding zone.
During the homogenizing treatment, diffusion of alloying ele-
ments between the base metal and the bonding zone in-
creases the joint strength. This increase is due to solid
solution strengthening. Fig. 11 shows the fracture path at frac-
ture surfaces of the homogenized specimen. The crack propa-
gates through the carbides of the base metal which are outside
of the bonding zone. This is consistent with the high strength of
the homogenized joint.
It is interesting to note that the first stage nozzles of gas
turbines, which are mostly made of the FSX-414 superalloy,

Fig. 7 – Line scan EDS analysis of the alloying elements across the bonding zones of TLP bonded specimens, (a) before and
(b) after homogenizing.
 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5
Fig. 8 – Hardness profile of the joint before homogenizing.
must have excellent resistance to thermal fatigue [2]. There-
fore, regarding the joint performance, thermal fatigue proper-
ties of the joint should be investigated in addition to the
joint's shear strength. The brittle phases are known as the
preferred sites for nucleation and propagation of the thermal
fatigue cracks [18]. The failure during the shear test is also
sensitive to these brittle phases. Therefore, it is expected
that closeness of thermal fatigue properties of the joint to
the base metal's properties could be as the same trend as
the joint's shear strength.
3.4.1. Fractography
Fig. 12 shows images of shear fracture surfaces, which were
taken by a stereo microscope, for both the homogenized and
unhomogenized specimens. Both fracture surfaces show fi-
brous zones and evidences of plastic deformation. In the
void formation mechanism of ductile fracture, microvoid coa-
lescence results in fibrous zones [19]. More fibrous zones and
more marks of plastic deformation are visible at the fracture
surface of the homogenized specimen, in comparison with
the unhomogenized one. This is consistent with the fracture
path of the homogenized specimen which is through the
base metal (Fig. 11). Evidence of brittle needle-like precipitates
is visible on both fracture surfaces. These precipitates form
small proportions of the fracture surfaces. The fracture path
outside of the bonding zone (Fig. 11) shows that these phases
play an insignificant role in crack propagation. SEM micro-
graphs of shear fracture surfaces show that dimples are dom-
inant (Fig. 13). This could be evidence of ductile fracture. The
dimples in the fracture surface of homogenized specimen
are smaller and their number at a constant magnification is
greater, than in the unhomogenized specimen. This is evi-
dence of greater susceptibility to ductile fracture [19]. High
shear strength and ductile fracture of homogenized specimen
are desired properties of TLP bonding.
Fig. 9 – Hardness profile of the joint after homogenizing.
43
Fig. 10 – Comparison of shear strength and shear fracture
energy of the (a) base metal and TLP bonded specimens, (b)
before and (c) after homogenizing.
4. Conclusions
FSX-414 Co-based superalloy was TLP bonded at the standard
solution cycle. The bonded specimens were homogenized at
the standard aging cycle. The results of microstructural stud-
ies and mechanical tests showed that:
• Non-uniform distributed carbides in the austenitic matrix of
the as-cast specimen were replaced by uniform ones in the
microstructure of heat treated specimens. This uniformity
was greater for specimens heat treated at the solution +
aging cycle, in comparison with solution heat treated
specimens. XRD patterns and EDS analysis showed that
M23C6 carbides of both the as-cast and the heat treated
specimens, formed a eutectic structure. This structure
consisted of alternate sheaves of the M23C6 carbides and
the austenitic matrix.
• The solution heat treated specimen's hardness was lower
than that of the as-cast specimen. Aging treatment caused
increased hardness.
• Both before and after homogenization, the bonding region
consisted of two distinct zones including ISZ and DAZ. No
eutectic structure in the ISZ, and needle-like intermetallics
in the DAZ, including Co2B and CoB, were characterized.
• ISZ hardness, shear strength and shear fracture energy of
the homogenized specimen were higher than those of the
unhomogenized one. The homogenized specimen's shear
strength was about 93% of the base metal's shear strength
at the same heat treatment cycle.
• Fractography studies showed more fibrous zones, smaller
dimple size and greater number of dimples at the homoge-
nized specimen's fracture surface, in comparison with the
unhomogenized one.
• Desired joint properties were obtained for sample TLP bond-
ed at the standard solution cycle and homogenized at the
standard aging cycle. These properties included a eutectic-
free joint, relatively uniform distribution of alloying ele-
ments across the joint, joint hardness close to that of the
base metal, joint shear strength about 93% of the base
metal and ductile fracture of shear tested specimens.
44 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5

Fig. 11 – Optical micrographs of different sides of shear fracture surface for the homogenized specimen (a—side I and b—side II
of Fig. 12b).

Fig. 12 – Stereo micrographs of shear fracture surface for the (a) unhomogenized and (b) homogenized specimens
(F: fibrous zone, P:plastic deformation marks, N: needle-like precipitates).

Fig. 13 – SEM micrographs of shear fracture surface for the (a) unhomogenized and (b) homogenized specimens.
 MA TE RI A L S CH A R A CT ER IZ A TI O N 6 6 (2 0 1 2) 3 8–4 5
Acknowledgment
The authors would like to acknowledge Sharif University of
Technology (SUT) and PARTO Company for financial supports
of this research.
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