Materials Science and Engineering A 477 (2008) 250–258

Effect of microstructure on properties of friction

stir welded Inconel Alloy 600
Y.S. Sato a,∗ , P. Arkom a , H. Kokawa a , T.W. Nelson b , R.J. Steel c
aDepartment of Materials Processing, Graduate School of Engineering, Tohoku University,
6-6-02 Aramaki-aza-Aoba, Sendai 980-8579, Japan
b Mechanical Engineering Department, Brigham Young University, 435 CTB, Provo, UT 84602, USA
c MegaStir Technologies, 275 West 2230 North, Provo, UT 84604, USA

Received 13 December 2006; received in revised form 7 May 2007; accepted 3 July 2007

Abstract
Friction stir welding (FSW) has been widely used to metals with moderate melting temperatures, primarily Al alloys. Recently, tool materials
that withstand high stresses and temperatures necessary for FSW of materials with high melting temperatures have been developed. In the present
study, polycrystalline cubic boron nitride (PCBN) tool was used for partially penetrated FSW of Inconel Alloy 600, and a defect-free weld was
successfully produced. Microstructural characteristics, mechanical and corrosion properties in the weld were examined. The weld had better
mechanical properties than the base material due to formation of fine grain structure in the stir zone, but exhibited slightly the lower corrosion
resistance in a part of the stir zone and heat-affected zone (HAZ).
© 2007 Elsevier B.V. All rights reserved.

Keywords: Inconel Alloy 600; Friction stir welding; Mechanical properties; Corrosion properties; Microstructure

1. Introduction the corrosion resistance and ductility in the HAZ, respectively.

Inconel Alloy 600 is a solid solution nickel-base alloy with
major element composition Ni–16Cr–9Fe [1]. This alloy has
face centred cubic (FCC) structure up to its melting temperature,
and exhibits excellent mechanical properties, good corrosion and
oxidation resistance at high temperatures. Taking advantages of
these positive factors, this alloy has been mainly used in heat
exchanger tube in nuclear power plant [1–3].
In many commercial applications, welding is inevitable.
However, fusion welding processes often result in some prob-
lems in this alloy [4]. Major problem is hot-cracking in fusion
zone due to segregation of alloying elements during solidifica-
tion. To alleviate the hot-cracking, careful control of the weld
metal composition and temperature are often required during
welding. Even if hot-cracking was suppressed, an as-cast coarse
microstructure remains in the fusion zone. Additionally, the
heat-affected zone (HAZ) often experiences Cr-rich carbide pre-
cipitation and grain growth during fusion welding, which reduce
∗ Corresponding author. Tel.: +81 22 795 7353; fax: +81 22 795 7352.
E-mail address: ytksato@material.tohoku.ac.jp (Y.S. Sato).
When these problems occur, a decrease in heat-input is required.
Most of the abovementioned problems occurring in this alloy
during fusion welding are attributed to solidification or high
heat-input. Therefore, a solid-state joining process having low
heat-input would be better for this alloy. Friction stir weld-
ing (FSW) is an available candidate to effectively alleviate the
problems caused by fusion welding.
FSW is a solid-state joining process and patented by the weld-
ing institute (TWI) in UK in 1991 [5,6]. It has enabled us to
butt-weld Al alloys, which are often difficult to be fusion welded,
without voids, cracking and distortion. This process reduces
the manufacturing costs due to elimination of any defects, filler
materials, and costly weld preparation. Furthermore, friction stir
(FS) welds of Al alloys exhibit better mechanical properties than
fusion welds. Therefore, this process has already been applied
to the construction of Al structures [6–8].
Since inception, FSW had been restricted to moderate melt-
ing temperature materials, such as Al, Mg and Cu alloys [9–13],
due to a lack of available FSW tools for the high melting temper-
ature materials. Recently, several welding tools for high melting
temperature materials, having high temperature strength and
wear resistance, have been developed [14]. Tool development

0921-5093/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2007.07.002
 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258
has enabled investigators to effectively study the FSW of high
melting temperature materials. Some papers on FSW of car-
bon steels [15,16], C–Mn steels [17,18], pipeline steels [19],
stainless steels [20–24] and Ti alloy [25] have been reported.
FSW is a solid-state joining process leading to formation of
fine grains, low distortion and no segregation, preventing many
of the problems arising from fusion welding in Inconel Alloy
600. Ye et al. [26] have examined the feasibility of FSW for
Inconel Alloy 600, and reported that the FSW made the defect-
free stir zone having the finer grains and better mechanical
properties than the base material. However, corrosion properties
of the FS weld remains unclear, and microstructure associated
with properties in the FS weld has not been clarified yet.
This study produced a partial penetration FS weld in Inconel
Alloy 600 using polycrystalline cubic boron nitride (PCBN)
tool successfully. The microstructure and several properties,
including mechanical and corrosion properties, of the weld were
examined. The objective of the present paper is to clarify effect
of microstructure on several properties in the FS-welded Inconel
Alloy 600.
2. Experimental procedures
The base material used in this study was a mill-annealed
Inconel Alloy 600, 4.8 mm in thickness. Light sanding of the
top surfaces and adjoining surfaces to remove oxide and con-
taminants prior to welding was performed using 80 grid emery
cloth. Before FSW, each coupon was degreased with methanol
solvent.
An MS100 graded PCBN tool [14], consisting of about 90%
CBN, with a 25 mm shoulder diameter, and a 3 mm pin length
was used in this study. The PCBN tool had three flats on the pin
column surface instead of threads. A locking collar was used
to hold the PCBN and transfer torque to the tungsten carbide
shank. Since the pin length was shorter than the plate thickness,
the present study made only a partial penetration weld in this
alloy.
FSW was completed on a vertical milling machine fitted with
servomotors and automated control system. Since the machine
and tool were exposed to high temperatures during FSW, a liquid
cool tool holder equipped with telemetry system to broadcast
tool temperature was used for the weld trial. An argon atmo-
sphere was introduced through a gas cup around the tool at a flow
rate of 2.8 × 105 mm3 /s (1 m3 /h) to minimize surface oxidation.
A 3.5◦ tilt was applied to the tool during FSW. The welding
direction was parallel to the rolling direction of the plate. The
welding parameters used were a rotational speed of 600 rpm and
a travel speed of about 1 mm/s.
Microstructures in the weld were examined by optical
microscopy (OM), scanning electron microscopy (SEM), ori-
entation imaging microscopy (OIM) and transmission electron
microscopy (TEM). OM was used for observation of grain struc-
ture distribution in the weld. Sample for OM was electrolytically
etched in a 10 wt.% oxalic acid solution at 30 V for 20 s. Inclu-
sions observed in the weld were identified by energy-dispersive
X-ray spectroscopy (EDS) analysis system on an SEM. OIM
was used to examine details of the grain structure in the weld.
251
Fig. 1. Configuration of transverse tensile specimen used in this study.
The sample for OIM was prepared by electrolytical polishing
with a 30 ml HClO4 + 170 ml C2 H5 OH solution at 30 V for 60 s.
Each observation area was 400 ␮m × 400 ␮m. Crystallographic
data were expressed as grain boundary (GB) maps. Average
grain sizes were estimated by the mean linear intercept method
for high angle boundaries including twin boundaries in the GB
maps.
For the thin-foil disk specimens, 3 mm in diameter, were
cut from various locations using an electrical discharge
machine (EDM) and were prepared by jet eletropolishing in
a 50 ml HClO4 + 450 ml C2 H5 OH solution at 248 K (−25 ◦ C).
These thin foils were observed at 200 kV using a JEOL-
2000EXII transmission electron microscope (TEM). A Phillips
CM200FEG TEM equipped with an EDS analysis system was
employed for measurement of Cr depleted zone around the grain
boundary using an electron probe with a spatial resolution of
1.2 nm.
Mechanical properties of the weld were examined by Vick-
ers hardness and transverse tensile tests. Hardness profiles across
the stir zone were measured on transverse cross-sections of the
weld using a Vickers indenter with a 9.8 N load for 15 s. Trans-
verse tensile specimens were cut perpendicular to the welding
direction, as shown in Fig. 1(a). Configuration of the tensile spec-
imen is presented in Fig. 1(b). Gauge part of the tensile specimen
extends from the stir zone to the unaffected base material region.
Tensile tests were carried out at room temperature on a screw-
driven test machine at a crosshead speed of 1.67 × 10−2 mm/s.
Corrosion property of the weld was qualitatively examined
by ferric sulfate–sulfuric acid test [27]. Since the speci-
men for ferric sulfate–sulfuric acid test had dimension of
10 mm × 60 mm × 4.8 mm, two cross-sections perpendicular to
the welding direction, the top surface and the bottom sur-
face of the weld were exposed to the test solution for 86.4 ks
(24 h) during the test. Tested specimens were observed by SEM.
Moreover, double-loop electrochemical potentiokinetic reacti-
vation (DL-EPR) test [28] was also employed in a 0.01 M
H2 SO4 + 0.00002 M KSCN solution to quantitatively evaluate
distribution of the corrosion resistance in the weld. Output of
the DL-EPR test is reactivation current ratio which is deter-
mined by the ratio of the maximum current in the reactivation
loop to that in the anodic loop. Higher current ratio means the
larger degree of sensitisation in the material [29]. Since current
ratio increases with grain boundary area, the obtained current
ratios were normalized by grain boundary unit area [30].
252 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258
Fig. 2. Cross-section perpendicular to the welding direction of the weld.
3. Results and discussion
3.1. Microstructural characteristics in the weld
Macroscopic overview of the cross-section perpendicular to
the welding direction is shown in Fig. 2. The weld centre is
defined as centre of the weld at the top surface which was swept
by the shoulder, as shown in Fig. 2. The stir zone is observed
around the weld centre. No defects are observed in the stir zone,
except for remnant of initial butt surface. The stir zone is clas-
sified into two typical zones: black region which is observed
in the middle of the advancing side and light gray region which
occupies the most part. The black and gray regions are expressed
as the “BZ (black zone)” and “GZ (gray zone)” throughout this
paper, respectively.
Optical micrographs of the base material (BM), GZ, BZ and
thermo-mechanically affected zone (TMAZ) shown in Fig. 2 are
presented in Fig. 3. The BM has coarse grain structure. Besides
Fig. 3. Optical micrographs of the BM, GZ, BZ and TMAZ shown in Fig. 2.
the distinct grain boundaries, many twin boundaries are faintly
observed in the BM. FSW produces fine equiaxed grain structure
in the GZ. It seems that the BZ also has fine grains, but grain
boundaries in this region are not clearly observed due to presence
of many pits in the grain interiors. The TMAZ has a slightly
smaller grain structure than the BM. Slip bands are observed in
some grains in this region.
Grain boundary maps obtained from the BM, GZ and BZ by
OIM are shown in Fig. 4. In these maps, thick black lines cor-
respond to high angle boundaries having misorientation over
15◦ , and gray lines correspond to 3 twin boundaries. Low
angle boundaries having misorientation between 3◦ and 15◦ are
coloured by thin black lines, but they are hardly observed in
all regions. The BM has coarse grains including a high density
of twin boundaries. Frequency of twin boundaries and average
grain size in the BM was about 60% and 23 ␮m, respectively.
On the other hand, both the GZ and BZ have the finer equiaxed
grain structure. It is found that the frequency of twin bound-
aries in these regions is lower than those in the BM. In the GZ
and BZ regions, average grain sizes were approximately 16 and
14 ␮m, and the frequency of twin boundaries was about 24 and
6%, respectively. It seems that the grain sizes in Figs. 3 and 4
are much larger than the calculated values, which is due to the
calculation of the grain size including twin boundaries. Average
grain sizes excluding twin boundaries were about 61, 22 and
15 ␮m in the BM, GZ and BZ, respectively.
Microstructural evolution of the stir zone during FSW could
be explained as follows. FSW introduces frictional heat and
 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258
Fig. 4. Grain boundary maps obtained from the BM, GZ and BZ by OIM.
severe plastic deformation arising from the rotation of the
welding tool into the materials. Continuous [12,31–33], discon-
tinuous [33] and/or geometric dynamic recrystallisation [34,35]
occurs in the stir zone during stirring of FSW, which produces
the fine recrystallised grain structure. Since stirring of the mate-
rials destroys the initial microstructure of the BM, both the GZ
and BZ existing in the stir zone of the present weld have the finer
grain structure having the lower density of twin boundaries than
the BM.
The BZ had much lower frequency of twin boundaries than
the GZ. Since both the GZ and BZ are located within the stir
zone, it would be expected that they receive similar thermal and
mechanical effects from the rotating tool during FSW. After for-
mation of tiny recrystallised grains during stirring, the grains
would experience recovery, recrystallisation and static grain
growth during the weld cooling cycle of FSW [35,36].
Additionally, it is likely that annealing twins would be formed
in the stir zone of Inconel Alloy 600 during the cooling cycle,
because this alloy has relatively low stacking fault energy [37].
It is known that annealing twins are formed during grain growth
following recrystallisation [38]. The BZ had the smaller grain
structure with much lower density of twin boundaries, as shown
in Fig. 4. This suggests that annealing twin formation would be
suppressed with grain boundary migration in the BZ. As will be
253
shown later, the BZ contains a high density of CBN particles,
which may be a reason for suppression of the grain boundary
migration in the BZ.
SEM images of the BM, GZ and BZ in the weld lightly
electro-etched in a 10 wt.% oxalic acid solution for 5 s are shown
in Fig. 5(a). Shorter etching times were used to minimize the
large number of deep pits that were observed in this region when
the longer etching was applied. All regions contain some blocky-
shaped inclusions at grain boundaries and in the grain interiors.
EDS analysis revealed that the blocky-shaped inclusion was TiN,
which is often observed in commercial Inconel Alloy 600 [1,39].
Size of TiN inclusion is smaller in the GZ and BZ than in the
BM, which would be due to fragmentation of TiN during stirring
of FSW.
Besides the TiN inclusions, a lot of flaky-shaped pits and
inclusions are also observed at grain boundaries and in the grain
interiors in the BZ. They are indicated by black arrows in a
magnified SEM image of the BZ. Since the pits have similar
shape to the inclusions, they would be formed by exfoliation of
the inclusions during etching. An example of EDS spectrums
obtained from flaky-shaped inclusion and grain boundary are
shown in Fig. 5(b). The EDS spectrum of the grain bound-
ary consists of the Ni, Cr and Fe peaks, while the B, N, Ni,
Cr and Fe peaks are found in the EDS spectrum of the flaky-
254 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258

Fig. 5. (a) SEM images of the BM, GZ and BZ and (b) EDS spectrum obtained from a flaky-shaped inclusion and grain boundary in the BZ.

shaped inclusion. Size of the inclusions is ∼1 ␮m, so that EDS
spectrum of the inclusion would include signals generated from
both the inclusion and surrounding matrix. Commercial Inconel
Alloy 600 contains minimal B. Since this alloy was FS-welded
using PCBN tool in the present study, the flaky-shaped inclu-
sions are likely CBN debris arising from wear of the PCBN
tool.
3.2. Mechanical properties of the weld
Vickers hardness profiles obtained along the top, middle and
bottom lines on the cross-section shown in Fig. 2 are presented
in Fig. 6. It is noted that the bottom line does not cross the stir
zone. The BM has hardness between 140 and 160 HV. Both the
GZ and BZ exhibit slightly higher levels of hardness than the
BM as a result of the finer grain size. The highest hardness in
the weld was in the BZ. This may be attributed to a high density
of CBN particles.
Transverse tensile properties of the weld and BM are shown in
Fig. 7. The weld has the slightly higher ultimate tensile strength
(UTS) and 0.2% offset yield strength (YS), and lower elonga-
tion than the BM. The tensile specimen of the weld fractured
in the BM region, because the BM had the lowest hardness in
the present weld, as shown in Fig. 6. The strength is roughly
proportional to hardness [40], so that the BM region would
preferentially yield and then fail during transverse tensile test.
The inhomogeneity of deformation in the weld causes the lower
elongation of the weld [40].
 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258 255

Fig. 6. Hardness profiles obtained along the top, middle and bottom lines on the
cross-section shown in Fig. 2. Fig. 7. Transverse tensile properties of the weld and BM.

3.3. Corrosion properties of the weld
Cross-section and SEM images of several regions of the weld
after ferric sulfate–sulfuric acid test are shown in Fig. 8. Inter-
granular corrosion and loss of grains occurred in the BM and
GZ. The corrosion is most significant in the BZ, i.e. many grains
were removed at the bottom of this region, and a lot of pits are
observed inside the remaining grains. Region where some grains
were removed exists in the HAZ. The region with the greatest
loss of grains in the HAZ is defined as “GLG-region”.
Result of the DL-EPR test obtained from the BM, GZ, BZ
and GLG-region is shown in Fig. 9. The GZ shows the lower
current ratio than the BM. The BZ exhibits the same level of
current ratio as the BM, while the current ratio of the GLG-
region in the HAZ is higher than that of the BM. It is noted
that the deterioration of the corrosion resistance in the BZ is not

Fig. 8. (a) Cross-section and (b) SEM images of several regions in the weld after ferric sulfate–sulfuric acid test for 86.4 ks (24 h).
256 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258
Fig. 9. Reactivation current ratios in the BZ, GZ, BZ and GLG-region.
significant in Fig. 9, although the BZ is severely corroded during
the ferric sulfate–sulfuric acid test (Fig. 8). Since the DL-EPR
test is sensitive to the Cr depletion, this result suggests that the
corrosion of the BZ during the ferric sulfate–sulfuric acid test
is not attributed to the Cr depletion resulting from formation of
the Cr-rich precipitates. The CBN particles may be a reason for
severe corrosion of the BZ during the ferric sulfate–sulfuric acid
test, because they exist in this region, as shown in Fig. 5, but the
exact reason has not been clarified in the present study.
The DL-EPR test (Fig. 9) shows that the GLG-region in the
HAZ exhibits the highest current ratio in the weld. Since precip-
itation of Cr-rich carbides often adversely affects the corrosion
Fig. 10. TEM images of the BM, GZ and GLG-region.
resistance in the HAZ of fusion welded Alloy 600 due to forma-
tion of the Cr depletion around the Cr-rich carbides [4], vicinities
of the grain boundaries in the BM, GZ and GLG-region were
examined by TEM.
TEM images of these regions are shown in Fig. 10. The BM
consists of coarse grain structure having a low density of dis-
locations and large intergranular precipitates. Average size of
the intergranular precipitates was 275 nm, and the precipitates
were observed on random high angle grain boundaries [41].
The GZ consists of the finer grain structure having a higher
density of dislocations than the BM. Precise TEM examina-
tion revealed that the GZ also had small precipitates having the
average size of 80 nm on the grain boundaries. Precipitates are
also observed along the grain boundaries in the GLG-region
in the HAZ. The average size of the precipitate was 170 nm
in this region. Selected area diffraction analyses proved that all
intergranular precipitates observed were the Cr-rich M23 C6 -type
carbides having FCC structure. Additionally, the carbides had
a cube-on-cube crystallographic relationship with the matrix in
all regions, which suggests that the carbides did not undergo
severe stirring during FSW. An example of the diffraction pat-
tern obtained from an intergranular precipitate is also shown in
Fig. 10.
The M23 C6 -type carbide mainly consists of Cr and C. It is
likely that Cr depleted zone is formed in the vicinity of the
grain boundaries. Assuming that the larger M23 C6 -type carbide
makes a deeper Cr depleted zone, the BM should have worse
corrosion resistance than the GLG-region in the HAZ, which
does not agree with the abovementioned results (Figs. 8 and 9).
Therefore, the Cr profiles across the grain boundaries having the
Cr-rich carbides were measured in the BM, GZ and GLG-region
 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258
Fig. 11. (a) TEM images of the BM, GZ and GLG-region and (b) profiles of Cr contents across the grain boundaries of these regions shown in (a).
by TEM/EDS (Fig. 11). The Cr profiles were obtained along
the dotted lines in the TEM images. The BM and GLG-region
obviously have Cr depletion at the grain boundary. The grain
boundaries in the GZ have the remarkably higher Cr content than
those in the BM and GLG-region, although small Cr depletion
is detected. Minimum Cr contents in the Cr depleted zones were
approximately 11.5, 10.5 and 14 wt.% in the BM, GLG-region
and GZ, respectively, i.e. the GLG-region in the HAZ has slightly
deeper Cr depletion than the BM. The difference in Cr depletion
is not attributed to reasons of grain boundary energy, because
the grain boundaries are all random boundaries with high energy
[41,42].
The present study used a mill-annealed Inconel Alloy 600.
However, Fig. 11 shows that the mill annealing for the present
BM was not completed, because the mill-annealed microstruc-
ture is generally characterized by a high density of large Cr-rich
carbides and healing of the Cr depletion [1].
Formation mechanism of the Cr depletion in the GZ and
GLG-region may be explained as follows. The GZ would be
heated to temperature higher than 1473 K (1200 ◦ C) during
FSW, because previous studies [16,43] have shown that the
temperature, which depends on the workpiece and welding
parameters, exceeds 1473 K (1200 ◦ C) during FSW of steels.
Since solution annealing of the Cr-rich carbides would be gen-
erally performed at 1373 K (1100 ◦ C) in this alloy [1], the
maximum temperature fully dissolves the Cr-rich carbides of the
mill-annealed BM. The full dissolution of the Cr-rich carbides
in the GZ was supported by the cube-on-cube crystallographic
257
relationship between the carbide and matrix. Dissolution of Cr-
rich carbides would achieve replenishment of the Cr depletion.
During cooling cycle of FSW, temperature of the GZ passes
the stable temperature range of the Cr-rich carbides (about
823–1073 K) [39]. Solubility of C in this alloy is very low [44],
so that it is likely that the Cr-rich carbides rapidly re-precipitate
on the grain boundaries. Since the cooling rate of FSW is rapid,
tiny Cr-rich carbides and shallow Cr depletion would be formed
at the grain boundaries in the GZ.
On the other hand, the GLG-region in the HAZ would be
heated to the stable temperature of the Cr-rich carbide. This sit-
uation causes partial dissolution of the Cr-rich carbides. During
cooling cycle of FSW, growth of the remaining Cr-rich carbides,
rather than nucleation, would occur in this region. Additionally,
this region should be exposed to the stable temperature range
of the Cr-rich carbides for a relatively long time. This situation
would produce deeper Cr depletion at the grain boundaries. This
would be a reason why the GLG-region in the HAZ had the rela-
tively smaller Cr-rich carbides and deeper Cr depletion than the
BM.
Deeper Cr depletion causes the higher current ratio in the
DL-EPR test. According to Fig. 11, the GZ should exhibit the
lower current ratio than the BM and the current ratio of the GLG-
region in the HAZ should be slightly higher than that of the BM,
which is in good agreement with the DL-EPR result (Fig. 9).
The present study showed that the FS-welded Inconel Alloy
600 had two corrosive regions, i.e. the BZ and the GLG-region.
Reduction of corrosion resistance is attributed to deepest Cr
258 Y.S. Sato et al. / Materials Science and Engineering A 477 (2008) 250–258

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