Optics & Laser Technology 43 (2011) 208–213

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Optics & Laser Technology

journal homepage: www.elsevier.com/locate/optlastec

Microstructure and residual stress of laser rapid formed

Inconel 718 nickel-base superalloy
Fencheng Liu, Xin Lin, Gaolin Yang, Menghua Song, Jing Chen, Weidong Huang n
State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi’an 710072, PR China

a r t i c l e in f o a b s t r a c t

Article history: The microstructure and residual stress of laser rapid formed (LRFed) nickel-base superalloy Inconel 718
Received 14 March 2010 was investigated. The as-deposited microstructure of an LRFed Inconel 718 alloy is composed of
Received in revised form columnar dendrites growing epitaxially along the deposition direction, and the columnar dendrites
30 May 2010
transformed to unevenly distributed equiaxed grains after annealing treatment at high temperature.
Accepted 23 June 2010
Available online 14 July 2010
Residual stress evaluation in microstructure scale by Vickers micro-indentation method indicates that
the residual thermal stress is unevenly distributed in the LRFed sample, and it has a significant effect on
Keywords: the recrystallization during solution annealing treatment. The residual stress is introduced by rapid
Residual stress heating and cooling during laser rapid forming. There is an alternative distribution between high
Laser rapid forming
residual stress regions and low residual stress regions, within a single deposited layer, resulting in a
Inconel 718
similar distribution of recrystallized grain size.
& 2010 Elsevier Ltd. All rights reserved.

1. Introduction 2. Experimental

Laser rapid forming (LRF), which combines laser cladding with
rapid prototyping, is a promising technology for manufacturing
compact metallic parts with high performance [1]. It can
manufacture complex components without using dies, tooling
and only needs little machining. Meanwhile, fine microstructure
without macro-segregation can be obtained due to the rapid
solidification process of the molten pool during laser rapid
forming [2]. The repeated rapid heating and rapid cooling will
also result in the residual thermal stress in the LRFed parts, which
has a remarkable influence on the finish machining and the
geometric resolution of the LRFed parts. To date, the distribution
of residual thermal stress during an LRF has been studied by many
researchers in the sight of the crack control by means of neutron
diffraction [3] and hole drilling [4,5], etc. Many of these methods
are complicated, expensive or time consuming, and they cannot
measure residual stress at microstructure scale interested.
Comparatively, the residual stress measurement by Vickers
micro-indentation [6,7] is possibly an appropriate method for
the rapid evaluation of residual stress in microstructure scale.
In the present study, Inconel 718 samples were prepared by an
LRF. The microstructure and residual stress in microstructure
scale of the LRFed samples were investigated. The effect of
residual stress on the grain size distribution during the solution
annealing treatment was also discussed.
n
Corresponding author. Tel./fax: + 86 29 88494001.
E-mail address: huang@nwpu.edu.cn (W. Huang).
The forming of Inconel 718 alloy samples were carried out on a
LRF-II system, which consists of a PRC2000 continuous wave CO2
laser, a controlled atmosphere chamber and a powder feeding
system with a coaxial nozzle. The powder of Inconel 718 alloy
with the size of  150 mm and spherical shape, produced by
plasma rotation electrode process (PREP), was laser deposited on
a 1Cr18Ni9Ti stainless steel sheet substrate. The dimension of the
deposited sample is 80  24  10 mm3 (length  width  height).
The average chemical composition of LRFed Inconel 718 alloy was
(wt%) 19.3 Cr, 18.4 Fe, 0.9 Ti, 0.3 Al, 3.7 Mo, 5.8 Nd, 0.031 C and
balance Ni. The LRF processing parameters were listed in Table 1.
Parts of the LRFed Inconel 718 alloy samples were subjected to
subsequent heat treatment. In order to observe the microstruc-
ture changes of LRFed samples when exposured at a temperature,
these samples were solution annealed at temperatures ranging
950–1250 1C for 1 h, followed by water quench. The metallo-
graphic investigations of an LRFed Inconel 718 alloy were
performed on the as-deposited and the solution annealed
samples. Microstructural characteristic was observed using an
OLYMPUS optical microscope on the polished sections etched
with a mixture of 100 ml CH3CH2OH+ 20 ml HCl+ 5 g FeCl3.
Residual stress of the as-deposited sample was measured by
regular Vickers micro-indentation method. The measured position
was just in the middle of a cross section of the as-deposited
sample. The microhardness of corresponding position was
measured by a HXP-1000TM numerical microhardness tester
with a load of 200 N and a dwell time of 20 s. The stress–strain
curve of LRFed Inconel 718 alloy, which is needed in the residual

0030-3992/$ - see front matter & 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.optlastec.2010.06.015
 F. Liu et al. / Optics & Laser Technology 43 (2011) 208–213
stress evaluation, was obtained by testing an as-deposited sample
and a full solution annealing treated sample which was exposured
at 1100 1C for 3 h and followed by water quenching. Uniaxial
tensile was carried out at room temperature on an INSTRON11-96
universal material testing machine and with a tensile rate of
2 mm/min. The heat treatment used here is to achieve the
homogenization of alloy elements and release the residual stress
completely prior to the test of stress–strain curve.
3. Results and discussion
3.1. Microstructure of an LRFed Inconel 718 superalloy
Fig. 1 shows the typical microstructure of the as-deposited
LRFed Inconel 718 alloy. As shown in Fig. 1(a), columnar dendrites
grow epitaxially along the deposition direction, and some
dendrites even traverse several layers. During an LRF, the heat is
mainly dissipated from the substrate or the pre-deposited layers.
Similar to the welding process [1], the heat flow direction during
the solidification of molten pool is about perpendicular to the
surface of substrate or the pre-deposited layers, leading to the
directional columnar dendrites growth in the LRFed specimen
from the bottom up. Moreover due to the rapid solidification of
molten pool, the primary arm spacing of the dendrites is much
smaller than that of the castings, as shown in Fig. 1(b) and (c).
Layer band structure, which characters a single deposited layer
and an individual laser scanning pass, also can be seen in the form
Table 1
Processing parameters of an LRF route.
Laser power (W) Scanning velocity (mm/s) Powder feeding rate (g/min)
1200 6 8–12
Fig. 1. Microstructure images of an LRFed Inconel 718 superalloy in an as-deposited condition: (a) low magnification image of the cross section, (b) high magnification
image of the cross section, (c) high magnification of the section vertical to the deposition direction.
209
of arcs in Fig. 1(a). The overlapping regions of two adjacent passes
were marked out as ‘‘A’’ in Fig. 1(a).
After solution annealing at a higher temperature, recrystallization
occurred and the grain structure changed simultaneously. Recrys-
tallization is found to occur only when the solution temperature is
higher than 1100 1C, and uneven distribution of equiaxed grain
structure was formed. Fig. 2(a) and (b) shows the typical
recrystallized microstructure of an LRFed Inconel 718 samples
after solution annealed at 1170 and 1250 1C for 1 h, respectively, and
followed by water quench. The grain size is smaller than 100 mm in
fine grain regions, but is larger than 500 mm in coarse grain regions.
Meanwhile, the alternative distribution of fine and coarse grain
zones is observed in the recrystallized samples as shown, and their
interval is similar with the spacing between the adjacent laser
scanning passes, which is 1.6 mm during an LRF. It is obvious that
the grain size distribution after recrystallization has a corresponding
relationship with its position, which is the overlapping region or the
interior region of a single pass. It can be deduced that fine grain
regions are located in the overlapping regions between two adjacent
laser scanning passes, while the coarse grain regions are located in
the interior regions of single pass, approximately. Fig. 2(c) gives the
schematic representation of the relationship between grain size
distribution and its position during LRF process.
It was reported that the static recrystallization temperature of
wrought Inconel 718 alloy is 1020 1C [8], which means that when
sample was exposured at a temperature over 1020 1C for enough
time, recrystallization will occur and the deformed and elongated
grains will transform into finer equiaxed grains. In the present
Shielding gas flux (L/min) Spot diameter (mm) Overlap (%) Increment of Z (mm)
4–8 2.5 25 0.3
210 F. Liu et al. / Optics & Laser Technology 43 (2011) 208–213

Deposition direction
1600 µm Fine
grain
Coarse Fine Coarse
grain grain grain
Deposition direction

1600 µm

Coarse Fine Coarse Fine

grain grain grain grain

----Fine grain region ----Coarse grain region

n+3

n+2

n+1

Layer:
Scanning spacing
Pass: N+4 N+3 N+2 N+1 N
Fig. 2. Recrystallized microstructure of an LRFed Inconel 718 after heat treatment after solution annealed at 1170 1C for 1 h (a), at 1250 1C for 1 h (b) and its schematic plan (c).

experiment, the recrystallization of an LRFed Inconel 718 alloy
only occurred when the exposure temperature is higher than
1100 1C, which is much higher than the static recrystallization
temperature of wrought Inconel 718 alloy. It should be point out
that one of the samples was solution annealed at a much higher
temperature of 1250 1C, which is very near to the melting point of
1344 1C for Inconel 718 alloy. No grain boundaries or grain
interiors incipient melting was observed here. It is maybe an
attribute to the finer substructure and the absence of low melting
point precipitates at grain boundaries and grain interiors, resulted
from the rapid solidification of molten pool.
3.2. Residual stress of an LRFed Inconel 718 superalloy
In general, it is the residual strain and stress formed during
plastic deformation that drives the recrystallization of deformed
grains; however, the LRFed materials have not been deformed
during LRF. Therefore, the residual thermal stress, which is
accumulated from the repeated rapid heating and rapid cooling
of molten pool during an LRF, is considered to be the driving force
of recrystallization in an LRFed Inconel 718 alloy.
In order to find out the formation mechanism of how the
alternative distribution of fine and coarse grain zones were
formed, the residual stress in as-deposited sample of an LRFed
Inconel 718 alloy was investigated with Vickers micro-indenta-
tion method [6,7]. The series of points measured were in a straight
line, which traversed two laser scanning passes within a single
deposited layer, in a cross section perpendicular to the laser
scanning direction, so that the difference of the residual stress
between the interior region of a single pass and the overlapping
region of two adjacent passes could be detected.
Assuming that, the residual stress is in an equal-biaxial state
and the uniaxial stress–strain curve obeys a power-law function,
e.g. s ¼Kenp MPa (n and K are material constants which can be
obtained from the uniaxial stress–strain curve), Carlsson and
 F. Liu et al. / Optics & Laser Technology 43 (2011) 208–213
Fig. 3. Schematic of the nominal projected contact area Anom.
Larsson [9,10] have found that the residual stress and the residual
strain follow the following relations.
H ¼ C sðerepr þ eres Þ
 
sres
c2 ¼ c02 0:32ln 1 þ
sðeres Þ
where c2 is the area ratio defined as the ratio between the real
projected contact area A (mm2) and the nominal projected contact
area Anom (mm2), c2 ¼A/Anom; H is the microhardness of the tested
point, and here H¼P/A MPa (P is the testing load used, N) which is
different with the definition of micro Vickers hardness, where
HV¼P/Asurf kgf/mm2 (Asurf is the surface area of the sharp
indenter, mm2); C is a constant, which depends on the geometry
of the sharp indenter only; s(erepr + eres) is the flow stress at an
effective plastic strain (erepr + eres), while erepr is a representative
value of the effective plastic strain and eres is the von Mises
effective residual plastic strain in an equi-biaxial situation.
It is known that erepr ¼0.08 and C¼3 [10], when a Vickers
indenter is used, and c20 E1 within a certain accuracy standard.
In the present study, the real projected contact area A was
directly measured with a quantitative analysis of an optical
microscopy and the nominal projected contact area Anom was
calculated with the diagonal lines of the indentation as follows:
Anom ¼[(L1 + L2)/2]2/2 (L1 and L2 are the length of diagonal line of
the sharp indenter, mm). Fig. 3 gives the schematic of the nominal
projected contact area Anom. The experimentally measured stress–
strain curves of an as-deposited and full solution annealing heat
treated LRFed Inconel 718 sample are given in Fig. 4. The stress–
strain curve could be fitted approximately by a power-law
function as sðeres Þ ¼ 1181:21e0:1754
p MPa for the as-deposited
sample and sðeres Þ ¼ 976:33e0:2448p MPa for the full solution
annealing heat treated sample, as shown in Fig. 4(a) and (b),
respectively. So the residual strain and the residual stress could be
calculated from the following Eqs. (3) and (4), when the stress–
strain curve of as-deposited sample was used, or from following
Eqs. (5) and (6) when the stress–strain curve of full solution
211
annealing heat treated sample was used.
 1=0:1754
H
eres1 ¼ 0:08 ð3Þ
3  1181:21
and
  2  
c 1
sres1 ¼ 1181:21  9eres 90:1754  exp 1 ð4Þ
0:32
 1=0:2448
H
eres2 ¼ 0:08 ð5Þ
3  976:33
and
  2  
c 1
sres2 ¼ 976:33  9eres 90:2448  exp 1 ð6Þ
0:32
The indentation group and the corresponding measured
residual stress are shown in Fig. 5. As shown in Fig. 5(a),
positions ‘‘A’’ and ‘‘B’’ are located in the overlapping regions of
two adjacent pass, i.e., the right side of ‘‘B’’ is the pass N, the
interval between ‘‘A’’ and ‘‘B’’ is the pass N+1, and the left side of
‘‘A’’ is the pass N+ 2, in sequence. The measured residual stress as
shown in Fig. 5(b) is given in its absolute value form, because the
determination of the residual stress sign is infeasible in the
present study, and the coarse gray dash line gives the changing
trend of the residual stress along the line composed by the tested
points. It is found that, the high residual stress regions and low
residual stress regions appear alternately, similar to the
recrystallized grains. Positions ‘‘A’’ and ‘‘B’’ as shown in Fig. 5(b)
is corresponding to the positions ‘‘A’’ and ‘‘B’’ as marked out in
ð1Þ Fig. 5(a). From Fig. 5(b), it is also shown that the residual stress in
the overlapping region is higher than that of the interior region of
a single pass. The previous studies [11,12] have shown that micro
or macro cracks often occurred in the overlapping regions
ð2Þ
between two adjacent laser scanning passes, which also means
that a certain extent of high tensile stress was existed in this
region. Correspondingly, in the present study, these regions were
observed to possess high residual stress, which is in a reasonable
agreement with the previous studies.
To be used as the criterion of the calculation of residual stress,
the stress–strain curve should generate from a certain condition
of the as-deposited sample or heat treated sample. In this study,
both conditions are considered and the corresponding calculated
residual stress curves are presented in Fig. 5(b). In despite of the
variation in value, the changing trends of these two curves are
similar. In fact, it is the changing trend of the residual stress which
is more concerned with in this study, rather than the correct
value. Even if two different residual stress curves were obtained,
both of which can be used to evaluate the residual stress
distribution.
Similar as the welding process, residual thermal stress is
formed due to the uneven temperature distribution during an LRF
process. When a new pass is deposited, the pre-deposited pass in
the single layer has already solidified, will have enough strength
to restrain the free expansion of the newly deposited pass, which
leads to the occurrence of plastic compression deformation of the
newly deposited pass at a higher temperature. As the new pass
was cooled, the shrinkage of compression deformed region is
smaller than that under the free compression deformed condition,
due to the resistance to restraint of pre-deposited passes, resulted
in the formation of tensile stress in the new pass. As for
overlapping regions between the adjacent passes, Zhang et al.
[13] have studied the variation of temperature and thermal stress
within the overlapping region during laser surface modification
treatment through numerical methods. Zhang has found that,
when an overlap ratio of 20% was used, the central area of
212 F. Liu et al. / Optics & Laser Technology 43 (2011) 208–213
Fig. 4. Tensile stress–strain curves of an LRFed Inconel 718 alloy in an as-deposited condition (a) and after full solution annealing heat treatment (b) and their power-low
fitted curves according to sðeres Þ ¼ K enp MPa.
Fig. 5. Residual stress measurement position (a) and results (b). The residual
stress curves 1# and 2# are calculated from the tensile stress–strain curves of an
as-deposited sample and after full solution annealing treated sample, respectively.
The microhardness curve is also presented in (b).
overlapping region of two adjacent passes underwent a double
quench processes, while the region adjacent to the second pass
underwent an anneal process only. Therefore, when the new pass
is deposited, the interior area of an overlapping region, where it
was remelted and resolidified rapidly again, was quenched during
an LRF, resulted in the high residual stress in the overlapping
region, correspondingly. However, in the interior region of a pre-
deposited pass, the heat input when a new pass is deposited just
has an annealing effect on the pre-deposited pass, which
decreased the residual stress formed when this pass is deposited.
So that the interior regions of a single pass only has a lower
residual stress.
Compared with the recrystallized grain size as shown in
Fig. 2(a) and (b), which show that fine grains distribute in the
overlapping region of two adjacent laser scanning passes and
coarse grains distribute in the interior region of a single pass, the
residual thermal stress shows a similar distribution law as shown
in Fig. 5(b). This indicates that the uneven distribution of grain
size is caused by non-uniform distributed residual thermal stress.
It is well known that the recrystallized grain size depends
primarily on the amount of deformation, and is smaller for large
amounts of deformation [14]. From the standpoint of driving
force, a larger amount of deformation produces higher residual
stress, which can increase the number of nuclei and the
nucleation rate. Therefore, a higher residual stress should provide
more nuclei per unit volume, and hence leads to a smaller final
grain size in the overlapping regions of two adjacent passes.
On comparison with the high strain energy of plastic deformed
wrought materials, the recrystallization of an LRFed Inconel 718
alloy is droved by the lower residual thermal stress, so that the
recrystallized grains size is much larger. To improve the
recrystallization process and refine the grain size of LRFed
materials, post-processing should be applied to further enhance
the residual stress. From the aspect of optimization of LRF
processing parameters, increasing the overlap of two adjacent
passes may be a useful method to obtain high residual stress
regions, if it will not make the surface worse remarkably.
The microhardness for the corresponding measurement points
is also given in Fig. 5(b). Compared with the residual stress, the
distribution of microhardness does not show a similar trend along
the testing route. This is in coincidence with the observation of
Carlsson and Larsson [9,10], who have already indicated that
residual strain fields can be accurately correlated with the
hardness, while residual stresses are related to the size of the
contact area which is sensitive to elastic effects.
 F. Liu et al. / Optics & Laser Technology 43 (2011) 208–213
4. Conclusions
(1) Microstructure of laser rapid formed Inconel 718 alloy was
investigated. The typical microstructure of the as-deposited
LRFed Inconel 718 superalloy is found to be columnar
dendrites growing epitaxially along the deposition direction,
which transform to uneven distributed equiaxed grains after
the recrystallization at high temperature.
(2) Residual stress evaluation in microstructure scale by Vickers
micro-indentation method indicates that the residual thermal
stress, which is introduced by rapid heating and cooling
during laser rapid forming, is high in the overlapping regions
of two adjacent passes and is low in the interior regions of a
single pass.
(3) The unevenly alternative distribution of recrystallized grains
is resulted from the unevenly alternative distribution of high
residual stress regions and low residual stress regions.
Acknowledgements
This work was supported by the program for New Century
Excellent Talents in University of China (Grant no. NCET-06-
0879), the National Natural Science Foundation of China (NSFC)
(Grant no. 50971102), NPU Foundation for Fundamental Research
(Grant no. NPU-FFR-JC200808), and the fund of the State Key
Laboratory of Solidification Processing (NPU) (Nos. 16-TZ-2007
and 39-QZ-2009). The work is also supported by the Program of
Introducing Talents of Discipline to Universities (no. 08040).
213
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