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Journal of Alloys and Compounds: Xixue Xing, Xinjie Di, Baosen Wang
Journal of Alloys and Compounds: Xixue Xing, Xinjie Di, Baosen Wang
a r t i c l e i n f o a b s t r a c t
Article history: The effect of post-weld heat treatment (PWHT) temperatures on the microstructure of Inconel 625 depos-
Received 19 August 2013 ited metal (DM) was examined using an optical microscope (OM), scanning electron microscopy (SEM)
Received in revised form 27 November 2013 and transmission electron microscopy (TEM). The transformation mechanism of the c00 ? d phase and
Accepted 27 December 2013
the grain growth kinetics of the c0 phase during PWHT were revealed. The results indicate that the micro-
Available online 9 January 2014
structure of as-welded DM is composed of columnar grains of different sizes, of which the average grain
size is approximately 160 lm. Certain precipitates, such as the dispersed c0 phase, blocky MC-type car-
Keywords:
bide and irregular shape Laves phase, precipitate in the microstructure of the as-welded DM. Compared
Inconel 625 deposited metal
Post-weld heat treatment
with as-welded DM, the microstructure of DM after PWHT at 650 °C for 4 h shows minimal variation.
Segregation With an increase in PWHT temperature, a large number of body-centered tetragonal c00 phases precipitate
Phase transformation at interdendrite regions in the microstructure of DM after PWHT at 750 °C for 4 h. When the PWHT tem-
Coarsening perature increases to 850 °C, the metastable c00 phase directly transforms into a stable d phase in shear
mode, which exhibits a similar chemical composition but a different crystal structure than the c00 phase.
At 950 °C, the c00 phase and the d phase disappear, whereas certain M6C-type carbides precipitate at the
grain boundaries. Alloying elements such as Nb, Mo, Si, Al and Fe in the microstructure of as-welded DM
exhibit segregation behavior. Due to an increasing PWHT temperature, the segregation behavior con-
stantly weakens with minimal evolution to the temperature of 750 °C. Above this temperature, partition
coefficients tend toward 1, and composition heterogeneity disappears at 950 °C. During PWHT, the c0
phase continuously coarsens with an increase in PWHT temperature. The dynamic analysis shows that
the coarsening behavior of the c0 phase corresponds with the formula: d 3 d
3 ¼ A eQ =RT =T t with an
0
activation energy of 253 kJ/mol.
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http://dx.doi.org/10.1016/j.jallcom.2013.12.224
X. Xing et al. / Journal of Alloys and Compounds 593 (2014) 110–116 111
Fig. 2. OM images of as-welded Inconel 625 deposited metal: (a) etched with mixed
2. Material and methods
acid and (b) etched with aqua regia.
A DM sample was GTA overlay welded with Inconel 625 (ERNiCrMo-3) filler
wire on a low-alloy steel plate using a current of 110 A DC and a voltage of 13 V.
The interpass temperature was controlled at 100 °C or less, and a welding speed cellular–dendritic. The two types of cellular–dendritic microstruc-
of 25 mm/min was maintained. The chemical composition of the superalloy DM ture exhibit identical growth directions and appear alternately. The
in this study consisted of (wt.%) 22.66 Cr, 8.71 Mo, 3.53 Nb, 0.01 C, 0.09 Mn, 0.32 arm spacing of continuous cellular–dendritic microstructure
Fe, 0.08 Si, 0.01 Cu, 0.14 Al, 0.21 Ti, and margin Ni. The as-welded DM sample
ranges from 80 – 130 lm. This result is consistent with the litera-
was evenly divided into 5 sections that were transversely oriented in the welding
direction (Fig. 1). One of the Sections (I) was selected as the as-welded sample. ture and with observations by Xu et al. [23].
The remaining Sections (II, III, IV, and V) underwent PWHT under the following con- Certain secondary phases precipitate in grains and at the grain
ditions: they were heated in 200 °C increments per hour with a four-hour hold time boundaries of the microstructure of the as-welded DM (Fig. 2a).
at 650 °C, 750 °C, 850 °C and 950 °C, respectively, and slow-cooled in a furnace. The results of the TEM analysis showed that these secondary
The as-welded samples and DM samples subjected to PWHT were polished
phases were dispersed throughout the c0 phase, the blocky MC-
using standard metallographic techniques. The microstructure of the DM that cor-
responded to all thermal states was examined and analyzed by OLYMPUS GX51 OM, type carbide and the irregular shape Laves phase (Fig. 3). The
JEOL JSM-6360LV SEM and PHILIPS CM200 TEM, which were equipped with an chemical compositions of these precipitates, which were deter-
ultra-thin window Oxford energy dispersive spectrometer (EDS). Using TEM, se- mined by TEM/EDS, are listed in Table 1. A small granular-like c0
lected-area electron diffraction (SAED) analysis of the precipitates in thin foils,
phase is dispersedly distributed throughout the c -matrix
which were prepared from the Inconel 625 DM, was performed. Using a current
of 75 V, the thin foils were produced by twinjet polishing with 5% perchloric acid
(Fig. 3a). The c0 phase and the c -matrix possess similar lattice con-
and 95% ethanol at temperatures that ranged from 25 °C to 29 °C. stants and a small lattice misfit [24]; thus, their electron diffraction
patterns are coincident. With the aid of the EDS spectrum of this
dispersed phase, it can be concluded that this precipitate is in
3. Results
the c0 phase. The Laves phase exhibits a hexagonal close-packed
(hcp) crystal structure with lattice parameters of a = b = 0.46 nm,
3.1. Microstructure characterization of as-welded DM
c = 0.73 nm, and c/a = 1.59. In this study, the particle sizes of the
Laves phase range from 20–150 nm. The MC-type carbide (M de-
Fig. 2 shows OM images of the as-welded DM, which was
notes Nb, Ti) exhibits a face-centered cubic (fcc) crystal structure
etched with mixed acid (hydrochloric acid:nitric acid:acetic
with a lattice parameter of 0.43 nm and an average grain size of
acid = 1:1:1) or aqua regia. The microstructure of as-welded DM
approximately 0.2 lm.
is composed of columnar grains, as shown in Fig. 2. The columnar
grain sizes in this study ranged between 100 lm and 200 lm, with
an average value of 160 lm. Two different types of cellular-den- 3.2. Microstructure characterization of DM after PWHT
dritic microstructures were observed in the OM image of the
as-welded DM: the first microstructure is continuous cellular–den- Fig. 4 shows SEM images of DM after a PWHT of 4 h at 650 °C,
dritic, and the second microstructure is discontinuous 750 °C, 850 °C and 950 °C. The TEM images and chemical composi-
tions of new precipitates in the microstructure of DM after PWHT
are displayed in Fig. 5 and Table 2, respectively. Compared with the
as-welded DM, the microstructure of DM after PWHT at 650 °C for
4 h varies insignificantly, with the exception of a small increase in
the size and content of the secondary phases (Fig. 4a). With an in-
crease in PWHT temperature, the amount of Laves phase decreases,
and a large number of rectangular secondary phases precipitate in
the interdendrite regions in the microstructure of DM after PWHT
at 750 °C for 4 h (Fig. 4b). The results of the TEM analysis showed
that these rectangular precipitates, which occur in the intermetal-
Fig. 1. The schematic diagram of overlay welding sample. lic c00 phase, exhibit a body-centered tetragonal structure with
112 X. Xing et al. / Journal of Alloys and Compounds 593 (2014) 110–116
Table 1
Chemical composition of precipitates in the microstructure of as-welded Inconel 625
deposited metal (wt.%).
Phases Ni Cr Nb Fe Al Ti Si
c0 53.9 7.5 16.5 0.6 19.3 2.2 –
MC 5.2 3.8 76.3 – – 10.1 4.6
Laves 42.9 18.0 10.1 13.7 – 15.0 0.3
Fig. 4. SEM images of Inconel 625 deposited metal after post-weld heat treatment
at different temperatures for 4 h: (a) 650 °C, (b) 750 °C, (c) 850 °C and (d) 950 °C.
lattice parameters of a = b = 0.37 nm and c = 0.73 nm and an aver-
age grain size of approximately 70 nm (Fig. 5a).
With a further increase in temperature to 850 °C, along with 3.3. Segregation behavior of alloying elements in DM
declining c00 phase, MC-type carbide and Laves phase, a substantial
number of needle-like secondary phases were observed in the Table 3 displays the average chemical compositions for a mini-
microstructure of DM (Fig. 4c). The results of the TEM analysis re- mum of 12 points in the dendrite core and interdendrite regions in
veal that this phase consists of an orthorhombic stable intermetal- as-welded DM, which were determined by an electron microprobe.
lic d phase, which exhibits a similar chemical composition but The results show that the elements Mo, Al, Si and Nb diffuse from
different lattice parameters (a = 0.51 nm, b = 0.43 nm, and the dendrite region and the element Fe diffuses to the dendrite re-
c = 0.46 nm) than the c00 phase. The d phase exhibits only three dif- gion during the solidification process of DM. The segregation
ferent orientations, and some poor c00 phase regions appear near behavior does not appear in Cr. This finding is attributed to the dif-
the d phase (Fig. 5b). Fig. 5b reveals the following orientation rela- ference among the partition coefficient K of Mo, Al, Si, Nb, Fe and
tionship between the d phase and the c00 phase: ð0 2 0Þd ==ð0 1 0Þc00 ; Cr. The K value, which is defined by K = Cs/Cl (Cs is the solid compo-
=½0 0 3 00 : At 950 °C, the c00 phase and the d phase disappear,
½2 0 4 sition and Cl is the liquid composition at a particular temperature),
d c
and small amounts of blocky secondary phases appear at the grain describes how strongly an alloying element partitions in the liquid
boundaries (Fig. 4d). The results of the TEM analysis showed that and solid phases during solidification. Assuming that the equilib-
these new blocky precipitates comprise M6C-type carbide, which rium partition coefficient K is a constant, the dendritic core compo-
has a face-centered cubic (fcc) structure, a lattice parameter of sitions are determined by KCl. Therefore, the ratio between the
1.12 nm and an average grain size of approximately 10 lm. These dendritic core composition and the interdendritic composition
blocky M6C-type carbides develop concurrently along the grain can be used as an approximate partition coefficient in this study.
boundaries (Fig. 5c). The approximate partition coefficients of the alloying elements
X. Xing et al. / Journal of Alloys and Compounds 593 (2014) 110–116 113
Fig. 6. The relationship between the partition coefficient and post-weld heat
treatment temperature.
Table 2
Based on the experimental results, secondary phases, such as
Chemical composition of precipitates in the microstructure of Inconel 625 deposited
metal after post-weld heat treatment (wt.%). the dispersed c0 phase, blocky MC-type carbide and irregular shape
Laves phase, precipitate in the microstructure of the as-welded
Phases Ni Cr Nb Fe Al Ti Si
DM, in addition to the c-matrix. According to the literature
c00 65.2 6.1 26.6 0.5 – 1.6 – [2,25], the equilibrium solidification process of as-deposited Inco-
d 65.9 2.9 28.1 1.2 – 1.0 0.9
nel 625 superalloy is as follows:
M6C 31.3 12.2 – 8.3 0.9 0.8 46.5
L ! L þ c ! L þ c þ NbC ! c þ NbC þ Laves:
In the GTA overlay welding process, the solidification in DM of
Table 3 Inconel 625 wire begins with the reaction L ! c; which causes the
Chemical composition of dendrite core and interdendrite in as-welded Inconel 625
deposited metal (wt.%).
accumulation of Nb, Ti and C elements in intergranular spaces and
liquid along the grain boundaries. Thus, MC-type carbide (M de-
Analyzed areas Ni Cr Mo Nb Fe Al Si notes Nb, Ti) precipitates in these regions via the eutectic type
Cores 64.01 23.47 8.50 1.17 0.48 0.70 0.33 reaction L ! ðc þ NbCÞ, which consumes the majority of the avail-
Spaces 60.65 23.48 9.59 2.68 0.39 1.31 0.56 able carbon. Alloying elements, such as Nb, Cr, and Fe, accumulate
K 1.06 1.00 0.89 0.44 1.23 0.53 0.59
in the intergranular spaces and liquid along the grain boundaries.
As a result, the Laves phase precipitates in the microstructure via
the reaction L ! ðc þ LavesÞ. The simultaneous presence of Ni
were calculated and are listed in Table 3. The results indicate that and the c0 phase-forming elements Al, and Ti causes the formation
Ni and Fe with K > 1 segregate to the dendritic core, whereas Mo, of the dispersed c0 phase, which can effectively strengthen the
Nb, Al and Si with K < 1 enrich the interdendritic region. Cr with mechanical properties of Inconel 625 DM through the pinning ef-
K values approximately equal to unity tends to exhibit a uniform fect for dislocation.
distribution between the dendritic core and the cellular-dendrite Compared with as-welded DM, the microstructure of DM after
interstices. PWHT at 650 °C for 4 h shows minimal variation. This finding is
Fig. 6 shows the relationships between the partition coefficients primarily attributed to the slow diffusion velocity of the alloying
K for alloying elements and the PWHT temperature. The solubility elements in DM [13]. Above 650 °C, the Laves phase constantly dis-
of the alloying elements in the c -matrix constantly increase with solves with an increase in solid solubility and diffusion velocity of
an increase in the PWHT temperature. Thus the partition alloying elements in the c -matrix. As a result, numerous Nb atoms
coefficients of Fe, Mo, Si, Nb and Al continuously trend toward 1. were released in the interdendrite regions. A study by Lippold et al.
114 X. Xing et al. / Journal of Alloys and Compounds 593 (2014) 110–116
[2] indicates that the c00 phase will only form during PWHT in 4.3. Grain growth kinetics of the c00 phase during PWHT
which the solid solubility of Nb is exceeded in the temperature
range between 678 °C and 936 °C. Thus, a larger number of rectan- Fig. 9 shows TEM images of the c00 phase in DM. As shown in
gular c00 phases were observed to form in DM after PWHT at 750 °C Fig. 9, the c00 phase significantly coarsens, but its quantity con-
for 4 h. When a PWHT temperature of 850 °C is used, the metasta- stantly decreases as the PWHT temperature increases. Because
ble c00 phase transforms into a stable needle-like d phase, which the shape of the c0 phase is irregular, the size of the c0 phase in this
exhibits a similar chemical composition but a different crystal study is substituted by the average diameter of the circle with the
structure (orthorhombic) than the c00 phase. These needle-like d same projected area as the c0 phase. The relationship between the
phases contain only three different orientations, and some poor average diameter of the c0 phase and the PWHT temperature is
c00 phase regions appear near the d phase (Fig. 5b). Due to a signif- presented in Fig. 10. The c0 phase coarsens slowly at low tempera-
icant increase in the solid solubility and diffusion velocity of Nb in tures, whereas the growth trend increases dramatically with an in-
the c -matrix, the c00 phase and d phase disappeared and the M6C- crease in PWHT temperature.
type carbide formed at the grain boundaries. According to the Gibbs–Thomson theory and the Greenwood
model [29,30], the relationship between the growth rate of the c0
phase and its radius is given as
4.2. Transformation mechanism of the c00 ?d phase during PWHT
dr
¼ D2Sum =RTr ð1= r 1=rÞ; ð1Þ
dt
Fig. 7 shows the transformation process of the c00 ? d phase.
Fig. 7 shows that the rectangular metastable c00 phase initially where r is the average particle radius at time t, nm; r0 is the average
evolves into an irregular short strip c00 phase and subsequently particle radius at t = 0, nm; S is the concentration of solute (c0
Fig. 8. The schematic diagram for the transformation of the c00 ? d phase.
X. Xing et al. / Journal of Alloys and Compounds 593 (2014) 110–116 115
Fig. 10. Relationship between the size of c0 phase and post-weld heat treatment
temperature.
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