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Inuence of Ni content on microstructure of WNi alloy produced by

selective laser melting


D.Q. Zhang
a,
, Z.H. Liu
a
, Q.Z. Cai
b
, J.H. Liu
c
, C.K. Chua
a
a
School of Mechanical & Aerospace Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798, Singapore
b
State Key Laboratory of Material Processing and Die & Mould Technology, Huazhong University of Science and Technology, Wuhan 430074, PR China
c
Heilongjiang Institute of Science and Technology, Harbin 150027, PR China
a b s t r a c t a r t i c l e i n f o
Article history:
Received 26 July 2013
Accepted 22 February 2014
Available online 6 March 2014
Keywords:
Selective laser melting
Tungsten nickel alloy
Microstructure
Hardness
3D printing
WNi alloy parts were produced with selective laser melting (SLM) and the inuence of the Ni content on the
microstructure evolution and microhardness was investigated methodically. The resultant microstructure of
the SLMspecimens with a Ni content of 10 wt.%, 20 wt.% and 40 wt.% exhibited bar-shaped structures, dendrites
and honeycomb structures respectively. It was found that a higher Ni content decreased the melt viscosity and
increased the densities of WNi parts. The microhardness decreased on the other hand with increasing Ni con-
tent. The microstructure formed in the SLM process was characterized by a mixture of typical liquid phase
sintering (LPS) microstructure and W dendritic structure. This revealed that the forming mechanism of the
SLM process on WNi particles was a combination of LPS and partial melting of W particles. The microstructure
showed that SLMprocess improved the bonding ability of the powder particles and therefore enhancing the me-
chanical properties.
2014 Elsevier Ltd. All rights reserved.
Introduction
Tungsten (W) is a refractory material that is difcult to process due
to its high melting point (3420 C), poor owability in liquid state and
high brittleness. These factors are responsible for its poor forming abil-
ity. As such, Nickel (Ni) with a lower melting point of 1455 C is usually
added to W for processing through liquid phase sintering (LPS) where-
by tungsten-based heavy alloys consisting of nearly pure tungsten
grains are dispersed in a ductile matrix of other materials. This allows
the fabrication of WNi parts in a rapid densication rate. There were
some research work on the Ni activated sintered W alloys. Kim et al.
[1] worked on high temperature performance of activated sintered
WNi compacts. Demirkan et al. [2] studied the properties of activated
sintered WNi alloy with additional Al
2
O
3
. Ding et al. [3] investigated
on the forming of ne-grained tungsten heavy alloy by spark plasma
sintering. Gu et al. [4] studied the mechanical alloy preparation and mi-
crostructural evolution of nanocrystalline tungstennickel heavy alloy.
Song and Ming [5] summarized the present research and future devel-
opment of tungsten heavy alloy. Their investigations showed that Ni
can be added in W for activated sintering. In addition, there are many
potential applications on WNi alloys such as bullets, weight and radia-
tion screen where these applications require material with high density
and strength.
One common process to produce WNi part is powder metallur-
gy (PM) which is based on liquid phase sintering (LPS), where the
Ni powder is melted to form the liquid phase. At the same time,
the solid W grains are soluble in the liquid. This solubility causes
the liquid to wet the solid, providing a capillary force that pulls
the grains together [6]. This method allows a lower sintering tem-
perature of about 12001400 C and a shorter sintering time. How-
ever, the PM of WNi possesses some limitations because of
geometrical constraints on the design, expensive mould and dedi-
cated tools. As such, these factors limit its range of applications. In
addition, Kim et al. also found out that the presence of Ni has a neg-
ative effect on the mechanical property of Ni-activated sintered W
compact because it forms a brittle network of Ni-rich second
phase along grain boundary of W [1]. Another forming process is
electrodeposition; according to Eliaz et al.'s research, the shortcom-
ing lies in the difculty to increase the W content beyond 76 wt.%
[7]. Other methods include microwave sintering technology [8,9]
and metal injection moulding (MIM) using prealloyed heavy tung-
sten alloy [10].
Therefore, there is a need and demand for advanced forming
methods of WNi alloys. Zhong et al. [11] studied the forming process
of WNi alloys via laser direct manufacturing (LDM) method and a col-
limation component was fabricated successfully. This formed the basis
of using selective laser melting (SLM), a 3D printing technique to pro-
duce WNi parts. Chua et al. [12] summarized the forming principles
of additive manufacturing or 3D printing technology. Yadroitsev et al.
[13] reported the single track formation of SLM. Gu and Shen [14]
Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
Corresponding author. Fax: +65 6791 1859.
E-mail address: zhangdq@ntu.edu.sg (D.Q. Zhang).
http://dx.doi.org/10.1016/j.ijrmhm.2014.02.007
0263-4368/ 2014 Elsevier Ltd. All rights reserved.
Contents lists available at ScienceDirect
Int. Journal of Refractory Metals and Hard Materials
j our nal homepage: www. el sevi er . com/ l ocat e/ I JRMHM
studied the forming process of SLMof micro/nano-sized CuWpowder.
Gu et al. [15] enabled to produce nanocomposite parts with enhanced
tribological performance using SLM. Liu et al. [16] investigated the spe-
cial structure of M2 high speed steel SLMparts using TEM. Loh et al. [17]
studied the effect of the beamprole during the SLMprocess. According
to their ndings, SLMis a promising technology that is able to fabricate
dense 3D parts with complex designs by melting a thin layer of loose
powder directly, in a layer by layer fashion.
Since our previous studies on pure W [18] and WNiFe [19] using
SLM technology showed that 3D parts can be produced successfully,
the results presented the opportunity and potential to process WNi
powder with SLM in this work.
In this work, a novel methodology of processing WNi powder
with SLM technique was developed. Compared to the previous
work of WNi, the forming mechanism and the inuence of Ni con-
tent in this powder system can be quite different using SLM technol-
ogy with high laser energy input. This is because bre laser was used
instead of CO
2
laser resulting in a high energy absorptivity. To inves-
tigate and understand the forming process, three different powder
mixtures with different Ni content, 10 wt.%, 20 wt.% and 40 wt.%
were processed with SLM to form 3D WNi parts. The aim was to
evaluate the inuence of Ni content in the forming of WNi parts
during the SLMprocess. SLMforming parameters for WNi alloy sys-
tem were addressed and described. The inuence of Ni content on
the resultant microstructure was also investigated. Finally, the mi-
crostructure evolutions of the WNi SLM parts were examined and
the resultant microstructures were characterized.
Experimental procedure
Powder materials
Wpowders (purity 99%, with a meanparticle size of 1 m5 m) and
carbonyl nickel powders (purity 99%, with a mean particle size of
2.3 m) were used in this experiment. Powder mixing was performed
in a stirring mixer for 8 h in argon gas environment. The three powder
systems with different weight ratio of W:Ni are listed in Table 1. The
morphology of the mixture powders as shown in Fig. 1 was examined
by a Quanta 200 scanning electron microscope (SEM) and the two
kinds of powder were observed to be homogeneous.
Laser device
This experiment was performed using HRPM-IIA system. The SLM
system is equipped with a 200 W continuous-wave/modulated bre
laser with a wavelength of 1095 nm and F-theta lens scanning system.
The chamber was rst vacuumed followed by lling of argon gas to pre-
vent oxidation during the SLM process.
Characterization of specimens
Samples were prepared for metallographic examination according
to standard procedures. They were etched with a mixture of NH
3
H
2
O
(10%, 10 ml), H
2
O
2
(10%, 10 ml) and distilled water (20 ml) for 20 s.
An ultrasonic cleanout device lled with distilled water was used to
clean the surface of the samples. The microstructure, phase and the
phase composition of WNi SLM specimens were analysed with Scan-
ning Electron Microscopy (SEM), X-ray diffraction (XRD) and energy
dispersive X-ray spectroscopy (EDS). The used forming parameters
were as follows: P = 200 W (laser power), v = 100 mm/s (laser scan
speed), d = 0.05 mm (scan interval) and h = 0.05 mm (powder layer
thickness).
Results and discussion
Solidication process of powder system
Fig. 2 shows an example of a WNi alloy SLM fabricated specimen.
The fabricated samples showed a dense surface with no cracks.
Fig. 3 depicts the surface morphologies of SLM specimens pro-
duced from powders A, B and C with the forming parameters men-
tioned in the Characterization of specimens section. Since the
melting point of W (3420 C) is much higher than that of Ni
(1455 C), specimen A showed a porous and rough surface where a
large amount of unmelted W particles could be observed (Fig. 3a).
This was due to the low Ni content which resulted in low liquid con-
tent and hence led to a poor densication. On the other hand, Fig. 3b
and c showed improved densication where specimen C showed a
smoother surface compared to specimen B. This indicated that an in-
crease in Ni content favours LPS during the SLM process. This is in
fact similar to LPS process in PM technology where the driving
force for sintering is in the minimization of surface energy by reduc-
tion of surface area. During the SLM process, the specimens with in-
creasing Ni content from 10%, 20% to 40% resulted in an approximate
liquid phase of 26%, 44% and 67% in the specimens respectively when
a temperature larger than 1455 C was achieved in the powder bed.
This illustrated that the sintering ability improved when the liquid
content is increased through increasing the Ni content in weight per-
centage. However, it should be pointed out that during the LPS pro-
cess in SLM, particle rearrangement occurred several times owning
to multi-track fabrication process. Furthermore, no further sintering
of solid took place after the Ni liquid phase cooled down owing to the
large cooling rate in SLM.
To further understand the characteristics of the melting surface of
WNi alloys, a coordinate system (see Fig. 4) of powder heating
model can be used to explain the melting behaviour of metal particles
[20].
According to the lawof conservation of energy, during a laser radia-
tion time (t, t), a metal powder particle at position (x(t), y(t), z(t)), the
powder heating model can be obtained by:
T
T
a

3r
l
2
p
c
p
r
p
v
l

p
P
l
r
l
2
4 T
4
T
4
a
_ _
_ _
;
T
m
;
T
a

3r
l
2
p
c
p
r
p
v
l

p
P
l
r
l
2
4 T
4
T
4
a
_ _
_ _
;
Q
in
bQ
1
Q
1
Q
in
Q
2
Q
in
NQ
2
_

_
4
where, a
p
is the laser absorption coefcient of powder; is the Stefan
Boltzmannconstant; is the radiation emissivity; v
l
is the laser scanning
velocity; T
a
is the environment temperature; and P(x(t), z(t)) is the dis-
tribution of laser source. c, l
P
, and T
m
are specic heat, latent heat of fu-
sion and melting temperature of metal particles respectively.
FromEq. (4), it can be foundthat powder heating is dependent on its
own characteristics (melting temperature, specic heat and thermal ab-
sorption) and the laser treating time. Every powder particle could ob-
tain its corresponding temperature. The powder particle will melt
when this corresponding temperature reaches the melting temperature
(Fig. 3c). On the contrary, the powder particle may melt partially or not
melt (Fig. 3a and b).
Table 1
Compositions of three powder systems with variation of Ni contents.
Powder system W powder (wt.%) Ni powder (wt.%)
A 90 10
B 80 20
C 60 40
16 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
Phase transformation
Figs. 5 and 6 depict the typical X-ray diffraction spectrum of WNi
powders A, B and C and the respective SLMsamples produced. The pow-
ders mainly consisted of matrix metal Wand Ni, while Ni peaks became
higher when its relative content increases (Fig. 5c). After the SLM
process, the diffraction peaks of W, Ni and Ni
4
W could be observed
(Fig. 6). Furthermore, Fig. 6 reveals the presence of an intermetallic
compound phase, Ni
4
W, after the SLM process. Some Ni peaks were
also observed to be missing after the SLMprocess and this was because
a large amount of Ni powder melted due to its lower melting point rel-
ative to W. On the other hand, reaction of Wphase may also occur after
the temperature has reached about 970 C to form Ni
4
W phase accord-
ing to the WNi phase diagram shown in Fig. 7 [21]. As the Ni content
increased from 10 wt.% to 20 wt.% to 40 wt.% for SLM specimens A, B
and C respectively, the corresponding diffraction peaks of Ni
4
W phase
increased accordingly.
Zhou Y et al. [9] reported that there was a weak WNi phase
(040) peak that appeared in WNi sintered samples through micro-
wave sintering process. This illustrated that the Ni
4
W phase was
formed after the sintering process because at 1450 C, the liquid Ni
phase dissolved a large amount of W. While the LPS process in
SLM of WNi is similar to LPS process in microwave sintering of
WNi, only Ni
4
W was observed and not WNi. Instead, W dendrites
were observed. Therefore, this evidence strongly indicated that
some W particles experienced melting and formed dendrites upon
solidication while the remaining W particles were sintered togeth-
er with Ni.
Microstructure evolution
The resultant microstructures of SLM specimens A, B and C are
shown in Fig. 8. As the Ni content increased from 10 wt.% to
20 wt.% to 40 wt.%, the microstructures evolved from bar shaped
structures to dendrites to honeycomb structures. The forming mech-
anism of SLM process is not the same as LPS in powder metallurgy
Fig. 1. Morphology of powder systems with various contents of Ni powder: (a) powder A, (b) powder B, and (c) powder C.
Fig. 2. Image of WNi alloy SLM specimen.
17 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
and, in some area, Wparticles experience melting/solidication dur-
ing the SLM process (Fig. 9). The experimental results demonstrated
that the content of Ni element played an important role in the micro-
structures of WNi SLM parts. Adding Ni element in the powder sys-
temcould decrease the temperature gradient of powder bed because
of the relatively lower melting temperature of Ni. Based on dendrite
growth theory [22], primary dendritic space would augment with
the fall of temperature gradient. Hence, a larger Ni content of
40 wt.% combined with the decreasing of temperature gradient in
SLM process along Z direction, and the microstructures evolved
from bar shaped structures to dendrites to honeycomb structures
accordingly.
Fig. 10 shows the EDS results of SLM samples using powder A.
The results revealed that the grey phase contained a large W con-
tent (91.88 wt.%) and the dark matrix contained a large Ni content
(51.81 wt.%). Similarly, the EDS results of SLM sample using
Fig. 3. Surface morphologies of SLM-fabricated specimens using: (a) sample A (90 WNi), (b) sample B (80 WNi), and (c) sample C (60 WNi).
Fig. 4. Coordinate system of powder heating model.
Fig. 5. X-ray diffraction peaks of WNi powder systems: (a) powder A; (b) powder B; and
(c) powder C.
18 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
powder B (Fig. 11a and b) demonstrated that the grey phase
contained a large W content and the dark matrix contained a
large Ni content. Based on metal solidication theory [22,23],
supercooling rate is usually considered with regard to its solidica-
tion conditions, initiation grain of crystallization and the growth of
crystal. For SLM of WNi alloys, the heating effect of powder par-
ticles was determined by the thermal conditions of powder bed.
Since the Ni particles melted rst during the SLM process, the W
particles were rearranged by the capillary force. With the increase
of Ni content, the WNi powder experienced a near rapid melting-
solidication process with the composition undercooling as the
primary factor. Under a positive temperature gradient
dT x


x
0 N0
_ _
,
the structural features of the dendrites varied according to the
composition undercooling of the WNi powder. The structural
features of the dendrites transited from cellular crystals to colum-
nar crystals to free dendrites with the increase in undercooling
[24] as shown in Fig. 9ac.
Inuence of Ni content during SLM process
Liu et al. [25] systematically studied the microwave sintering prop-
erties of WNiFe and sintering parameters of tungsten-based alloy
[8]. Zhou et al. [26] also investigated the forming process of high
performance tungsten through microwave sintering. Their results
showedthat the mainfactor of activationmechanismby adding alloy el-
ement could be regarded as volume diffusion through the crystalline
lattice and via short-circuit paths such as particle surfaces and grain
boundaries.
When the surface of the matrix is covered with a metal lm of
high diffusion coefcient, a large amount of vacancy and micro
pores appeared on the surface of metal particles. This resulted from
the diffusion of metal atoms from the metal lm into the matrix.
The nature of diffusion during sintering can be considered as the mo-
tion of lattice vacancies in the material. Adding Ni element is a prom-
ising approach for the sintering of W since it promotes particle
diffusion and reduces viscosity. As a result, the sintering process is
improved.
In SLM, the main driving force in molten pool can be regarded as the
convection applied by the combination of buoyancy, surface tension
gradient and viscous shear stress. Gu and Shen [27] developed a multi
component Cu powder and studied the microstructure during the SLM
process. Averyanova et al. [28] also investigated the inuence of initial
powder characteristics on nal parts. From their work, it is believed
that the mutual solubility of chemical composition and the possible
chemical reaction have inuenced the density and microstructure of
SLM samples. In the present research, the carbonyl nickel powders
(purity 99%, with a mean particle size of 2.3 m) were used to prepare
the WNi composite powder. Owing to the high specic surface area
and low melting point, the composite powder system can enhance the
absorption of laser energy so as to benet the characteristics of sintering
kinetics.
Under the radiation of the laser beam, there was a temperature gradi-
ent in the melt in every direction. Furthermore, the evaporation of mate-
rial at certainlocations as well as the chemical potential gradient of solute
elements resulted from the thermal gradients; the direction of surface
tension gradient and the orientation of liquid ow were codetermined
by these effects. During the SLM forming process of WNi alloy, the
melt consisted of both liquid phase and solid phase. Moreover, under
the force of thermal capillary, the effect of the liquid content to the
melt viscosity () can be dened by [29]:

0
1
1
l

s
_ _
2
5
where,
0
is the basic viscosity value,
l
and
s
are the volume fraction of
liquid and critical solid phase volume fraction, respectively. The weight
percentage increase of Ni could enlarge the liquid content in molten
pool and cause the reduction of the melt viscosity resulting in a better
ow ability and stability of the molten tracks.
During SLM, laser scanning is performed line-by-line, followed by
layer-by-layer over the powder bed. Furthermore, there were some re-
search works on the melting process of metal powder in SLM. For in-
stance, Gusarov et al. [29] worked on the radiation and heat transfer
in laser-powder interface of SLM. Niu and Chang [30] also investigated
the instability of scan tracks of high speed powder in SLM. Shen et al.
[31] developed a porous 316 L with controllable microcellular in SLM.
Their research showed that the surface tension of the liquid phase can
be regarded as the main factor which controlled the resistance of defor-
mation capacity due to the contraction of the liquid phase.
Based on the research by Simchi and Pohl [32], the instability of the
molten tracks can be considered by:
ND 6
Fig. 6. X-ray diffraction peaks of WNi SLM-fabricated samples: (a) sample A, (b) sample
B, and (c) sample C.
Fig. 7. Binary phase diagrams of WNi alloy.
19 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
where is the laser wavelength, and Dis the diameter of continues mol-
ten tracks. It should be pointed out that, under the xed laser wave-
length, large D value had better ability for attaining a continuous
molten track. The increase of Ni weight percentage could prevent the
molten tracks from breaking up due to the decrease in surface tension.
This was consistent with what was observed in Fig. 4ac where the in-
crease of Ni content was benecial to the thermal uidity of the molten
tracks.
Inuence of Ni content on hardness value
Fig. 12 depicts the microhardness variation on the cross-sections of
SLMsamples A, B andC. Generally, the hardness decreased withincreas-
ing Ni content as W content decreases. In addition, the hardness de-
creased along the building direction. Another reason for the hardness
variation was due to the solidication shrinkage of loose powder bed
that resulted in a larger real layer thickness. Based on our previous
Fig. 8. Microstructures of SLM-fabricated samples: (a) sample A, (b) sample B, and (c) sample C.
Fig. 9. Forming mechanism schematic illustration for WNi powder system during SLM.
20 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
research [33], the total shrinkage of metal powder layer sharply in-
creased in the initial layers and then reached to a plateau value with
the increased processing layers. This value was dened by the ratio of
sliced layer thickness (h) to relative density (k) during the SLMprocess.
The real powder thickness (h
real
= H
layernumber
) variation could be
calculated as:
H
max
h a
n
h h 1k =k h=k h
m
=
l
5
where
m
is the density of the solid parts and
l
is the density of loose
powder.
Eq. (5) showed that there was a gradual increase of the real layer
thickness during SLM process, which could result in a decrease of the
microhardness along the Z direction.
On the other hand, the laser energy gradient distribution along the
powder layer thickness direction could induce the uctuation hardness
values between each scan layer.
Conclusions
WNi specimens with different Ni content were successfully pro-
duced by SLM. The microstructure evolution was characterized and
the microhardness was measured. The results can be concluded as
follows:
(1) The forming mechanism of WNi powder mixture in SLM was
characterized by LPS and partial melting of Wwhere Ni particles
melted to form the liquid to wet the solid W particles pull the
grains together through capillary force. W dendrite was also
found in the melted specimens. This illustrated that partial W
particles also underwent the melting/solidication process.
(2) Under the same forming parameters, SLM specimens with dif-
ferent Ni content manifested different microstructure. The mi-
crostructure evolved from bar shaped structure to dendrites
to honeycomb structure for specimens with a Ni content of
10 wt.%, 20 wt.% and 40 wt.% respectively. This indicated an
increase of temperature in powder bed combined with a
decrease of solidication rate.
(3) The different microstructural features were concluded to be a
result of constitutional supercooling of the powder systems.
Increasing Ni content promoted uniformity of melting samples
and decreased the melt viscosity.
(4) The hardness decreased along the building direction which
resulted from the shrinkage of loose powder bed.
Fig. 10. EDS analyses showing elemental distribution of sample A: (a) elemental distribution of point A; and (b) elemental distribution of point B.
Fig. 11. (a) Microstructure morphology of sample B and (b) EDS analysis along line AB.
21 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522
Acknowledgements
The authors would like to thank the open fund of state key laboratory
of powder metallurgy of Central SouthUniversity of China (2008112022).
The authors would like to acknowledge the National Natural Science
Foundation of China (61078078).
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Fig. 12. Changes in microhardness with distance from the bottom surface to top of SLM-
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22 D.Q. Zhang et al. / Int. Journal of Refractory Metals and Hard Materials 45 (2014) 1522

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