CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413

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CIRP Journal of Manufacturing Science and Technology

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Effects of laser printing parameters on molten pool formation,

microstructure evolution and mechanical properties of laser directed ]]
]]]]]]
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energy deposition of difficult-to-process tungsten heavy-alloy

⁎
Meng Guo, Guangjing Huang, Lixia Xi, Donghuai Dai, Dongdong Gu
Jiangsu Provincial Engineering Laboratory for Laser Additive Manufacturing of High-Performance Metallic Components, College of Materials Science and
Technology, Nanjing University of Aeronautics and Astronautics, Nanjing, People’s Republic of China

a r t i cl e i nfo a bstr ac t

Available online 9 November 2022 Laser directed energy deposition (LDED) additive manufacturing is promising in the fabrication of high-
performance W-based heavy-alloys which are normally difficult-to-process due to their unique nature such
Keywords: as the extremely high melting point and high ductile-brittle transition temperature. In this work, a novel
Laser directed energy deposition 95 W heavy alloy modified by nanosized Ni and Fe particles was manufactured by LDED process. The effects
Tungsten heavy-alloy
of laser power on the formation mechanisms of molten pool were investigated. It was found that a relatively
Molten pool formation
high laser power could promote the complete melting of W powder and formation of regular molten pool
Microstructure evolution
Mechanical properties morphology. The microstructures of laser-processed W heavy alloy showed columnar grains, cellular grains
and equiaxed grains from bottom to top within the molten pool along the building direction. The three-
dimensional finite element simulation revealed the temperature gradient (G), cooling rate (C) and solidi­
fication velocity (S) within the molten pool were different, which was responsible for the microstructural
development. The bulk-form 95 W heavy-alloy part free of defects was produced at the laser power of
1400 W. The optimally processed 95 W heavy-alloy by LDED showed a high average nanohardness of
8.6 GPa and a sound wear performance with a low coefficient of friction (COF) of 0.5. The tensile tests also
revealed the achievement of a combination of an excellent tensile strength of 541 MPa and an elongation of
0.99%. This work demonstrated that LDED was able to manufacture high-performance tungsten heavy-
alloys in bulk form with outstanding mechanical properties.
© 2022 CIRP.

Introduction
Due to the excellent properties such as high strength, high
hardness, and high chemical stability, tungsten and its alloys are
widely used in a number of special fields with extreme service en­
vironment [1]. Unlike the pure tungsten having a brittle physical
nature, tungsten heavy-alloys (WHAs) maintain a high density with
the sufficiently high strength and ductility [2]. Therefore, the WHAs
find their unique applications in kinetic energy penetrator, medical
ray shielding, and counter-balance weights [3,4]. Traditionally,
powder metallurgy methods such as liquid-phase sintering (LPS) [5],
powder injection molding (PIM) [6], and spark plasma sintering
(SPS) [7] are used to fabricate WHAs. For the LPS process of WHAs,
low-melting-point metals such as Fe and Ni are added into W
powder to act as the binder. These metals are melted firstly to form
⁎
Corresponding author.
E-mail address: dongdonggu@nuaa.edu.cn (D. Gu).
the liquid, which subsequently flows and fills between W powder
particles to realize a densification. Due to the nature of high melting
point of W, the W powder normally tend to be un-melted or partially
melted. A typical microstructure of powder metallurgy processed
WHAs thus contains the binder phase and the incompletely melted
W phase [8,9]. However, these conventional methods typically ex­
hibit a shortcoming in producing complex-structured parts. Fur­
thermore, the relatively low operation temperature in conventional
LPS process is not beneficial to elemental diffusion and metallurgical
bonding between different phases, resulting in the limited com­
prehensive properties of the WHAs fabricated by LPS process.
The development of Laser Additive Manufacturing (LAM) tech­
nology provides a feasible manufacturing method for metallic
components with difficult-to-process material nature. The current
researches on metallic materials by LAM usually concentrated on Al
alloys [10], Ti alloys [11], steels [12], and nickel-based superalloys
[13]. A large number of successful application cases of additive
manufactured components in modern industries such as aviation,
aerospace, automobile manufacturing, and energy production

https://doi.org/10.1016/j.cirpj.2022.09.002
1755-5817/© 2022 CIRP.
M. Guo, G. Huang, L. Xi et al.
demonstrated significant potential of LAM technology for high-end
engineering applications [14]. LAM was also applied to process pure
W and W-based material [15] and a majority of previous work fo­
cused on laser powder bed fusion (LPBF) of pure W [16–18]. Com­
pared with the powder-bed-based LPBF process, the powder-
feeding-based laser directed energy deposition (LDED) shows unique
advantages such as high process flexibility covering the preparation
of coatings, re-manufacturing, and production of large metallic
components[19,20]. Utilizing high-energy laser beam, LDED can also
realize the forming of hard-to-process W-based materials [21]. Wang
et al. prepared the W-Ni, W-Ni-Fe, and W-Ni-Co WHAs systems
using LDED process [22]. They found that all samples were com­
posed of unmelted W particles surrounded by columnar crystals of
W, and the addition of Ni and Fe did not have any reaction with W,
but could increase the tensile strength of LDED-processed WHAs.
Wang et al. fabricated a 90W-7Ni-3Fe alloy by LDED and compared
its microstructure and mechanical properties with that processed by
LPS [23]. They found that the LDED-processed sample having high W
content and refined microstructure showed a superior tensile
strength of 822 ± 30 MPa, which was about 200 MPa higher than
that of LPS sample. Moreover, they found that high processing
temperature arising from high energy input was beneficial to form
strong interface bonding between binder matrix and W, which
contributed to higher strength.
However, the previous work on LDED-printed WHAs mainly fo­
cused on the WHAs with medium contents of additive metals, with
the content of W normally below 90 wt%. LDED processing of WHAs
with high content of W above 90 wt% was rarely reported. When the
content of W increased in the material system, the laser energy input
should be increased as well. This might cause serious metallurgical
defects such as the burning loss of Ni and Fe, spatters of W, and
formation of coarse microstructures, deteriorating the comprehen­
sive performances of as-printed WHAs. It was reported that the
nanoparticles could be used to regulate the melting and solidifica­
tion processes, improving the manufacturability of the materials in
LAM process [24]. Using the nano-modification strategy, a nano-Ni
and Fe decorated W-Ni-Fe alloy with 98 wt% W was fabricated by
LPBF, showing a considerably high compressive strength of
2638 MPa and a strain of 46%, which was much higher than LPBF-
processed pure W [25]. On the one hand, the Ni and Fe nanopowder
can act as binding phase to promote the densification of W. On the
other hand, the Ni and Fe nanopowder have high specific surface
area, which can promote the surface reaction and interfacial bonding
of W during laser process.
In this work, a nano-modified high specific gravity WHA with
95 wt% W content was designed and fabricated by LDED technology.
The microstructure evolution and mechanical properties were stu­
died to understand the effects of processing parameters on LDED-
printed 95 W alloy. Meanwhile, the formation mechanism of mi­
crostructure during LDED process was revealed through numerical
simulation. This work demonstrated that LDED was promising in
manufacturing high specific gravity WHAs and provided a feasible
material design method for the fabrication of refractory metals.
Materials and experimental methods
Powder preparation and LDED processing of 95W alloy
The raw materials were W (purity: 99.9%), Ni (purity: 99.9%), and
Fe (purity: 99.9%) powder, respectively. The W powder had a sphe­
rical shape with an average diameter of 45 µm (supplied by Shanghai
Dajin Advanced Materials Co., Ltd., China), as presented in Fig. 1a and
e. The Ni and Fe powder were nano particles (Aladdin, Shanghai,
China), as shown in Fig. 1b and c. A horizontal planetary balling
milling (QM-3SP4, Nanjing NanDa Instrument Plant, China) was used
to prepare W-Ni-Fe mixed powder at a shielded atmosphere of
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CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413
argon. The mass ratio of W, Ni and Fe was 95:3.5:1.5, which was
based on the component content of classic tungsten alloy. A ball-to-
powder ration of 1:1, a rotation speed of 250 rpm and a milling time
of 6 h was utilized to make Ni and Fe nanoparticles distribute uni­
formly (Fig. 1d and f). After balling milling, the mixed powder was
dried at 100 ℃ for 4 h in vacuum.
A self-developed LDED system was applied to fabricate W-Ni-Fe
mixed powder, as shown in Fig. 2a. The LDED system mainly con­
tained a TRUMPF Nd: YAG laser system equipped with a maximum
laser power of 3 kW and a focused spot diameter of ∼ 2 mm, a
powder feeder system integrated with a coaxial powder nozzle. A
316 L stainless steel substrate was fixed on the building platform
before the deposition. Subsequently, the mixed W-Ni-Fe powder was
deposited on the substrate through the coaxial nozzle at a feeding
rate of 12 g/min. The LDED process was carried out under the pro­
tection of argon atmosphere to avoid the oxidation. Table 1 shows
the experiment parameters for LDED process. The 95 W parts for the
molten pool characterization were fabricated using laser powers (P)
ranging from 400 W to 1400 W with an interval of 200 W. Then, the
laser powers of 1000 W, 1200 W and 1400 W were further optimized
to manufacture 95 W bulks with a height of 20 mm and a length of
40 mm (Fig. 2c). The scanning speed (v) was fixed on 4 mm/s.
Characterization of microstructures and mechanical properties
After deposition, the 95 W parts were cut from the substrate, and
then polished for metallographic observation. The geometrical fea­
tures of each molten pool at cross section were measured to better
understand the characteristics of the molten pools (Fig. 2d). The
width (W) and height of the molten pool (H), wetting contact ( = ( 1
+ 2)/2), and penetration depth (D) were recorded. For further
analysis of microstructures, a solution composed of HF (10 mL),
HNO3 (30 mL) and distilled water (70 mL) was used to etch the po­
lished samples. Then, a field emission scanning electron microscope
(FE-SEM, Hitachi, Japan) equipped with energy dispersive spectro­
meter (EDS) were applied for microstructure observation. The wear
properties were carried out in a HT-500 ball-on-disc tribometer by
dry sliding wear tests, as shown in Fig. 2e. The counterface material
was GCr15 bearing steel ball, which had a diameter of 3 mm and a
mean hardness of HRC 60. The applied load was 820 g. The friction
unit was set at a speed of 400 r/min and sliding time of 15 min.
Meanwhile, the coefficient of friction (COF) of the as-fabricated parts
were automatically recorded. After wear tests, a laser scanning
confocal microscope (TCS SP8, Leica, Germany) was used to observe
the morphologies of the grinding cracks. Nano-hardness measure­
ments were carried out using the Nano Indenter G200 (Agilent
Technologies Inc.) with a load of 1000 μN and a holding time of 20 s.
The tensile tests were conducted by a double column electronic
universal testing machine (Instron5565, America) with a strain rate
of 0.1 mm/min.
Establishment of finite element model
In order to reveal the temperature field distributions during
LDED-processed 95 W, a simplified three-dimensional finite element
model containing 95 W deposition part and 316 L stainless steel
substrate was established according to the obtained morphologies of
the molten pools, as shown in Fig. 2b. The laser power of 1400 W,
laser diameter of 2 mm, scanning speed of 4 mm/s and deposition
length of 10 mm were used in this finite element simulation. This
model referred to the previous works on LDED [26,27]. The SOLID 70
unit was applied to mesh generation. The monitoring point A at the
molten pool surface, the monitoring point B at the substrate contact
surface and the monitoring point C at 2 mm away from the molten
pool surface were set as monitoring position. The temperature time
history and temperature gradient were extracted to research the
M. Guo, G. Huang, L. Xi et al. CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413

Fig. 1. SEM images showing the morphologies of (a) W powder, (b) Ni nano particles, (c) Fe nano particles and (d) W-Ni-Fe mixed powder. (e) Particle size distribution of pure W
and W-Ni-Fe. (f) EDS mappings of mixed W-Ni-Fe powder.

Fig. 2. (a) Schematic diagram of LDED process and LDED equipment. (b) The established finite element model (FEM) of LDED-processed 95 W. (c) Photograph showing the LDED-
printed 95 W alloy. (d) Schematic of geometrical features of the molten pool at cross section. (e) Schematic of abrasion ball-on-disk test.

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Table 1 The laser beam energy distribution conforms to Gauss equation,

The experiment parameters for LDED process. which is expressed as:
Experiment parameters Values
2Q 2r 2
Laser power (W) 400, 600, 800, 1000, 1200, 1400 q (r ) = exp
R2 R2 (6)
Scanning speed (mm/s) 4
Feeding rate (g/min) 12
Spot diameter (mm) 2
where Q and R are laser input energy and effective radius of laser
heat source. r represents the distance from any point in the radius of
the heat source to the center of the heat source.
thermal behavior. The physical parameters at different temperatures
of 95 W-3.5Ni-1.5Fe were calculated by JmatPro software. The ob­
Results and discussions
tained thermophysical parameters of 95 W including phase transi­
tion, thermal conductivity and specific heat were presented in Fig. 3.
Molten pool formation of LDED-processed 95W alloy
The thermophysical parameters of 316 L stainless steel are listed
in Table 2 [28]. The heat transfer in LDED process is controlled by the
During LDED process, the laser, powder particles and substrate
heat transfer energy conservation equation, which is described
materials interact with each other, causing formation of the molten
as [29]:
pool. As the molten pools overlap by track and track and by layer and
T T T T layer, the part is built. Therefore, the molten pool directly influences
c = kx + ky + kz +Q the quality of as-built parts[31]. Fig. 4 shows the morphologies and
t x x y y z z (1)
the corresponding size characteristics of the molten pools under
where x, y and z are Cartesian coordinate direction, ρ is the material different laser powers. As the laser power increased from 400 W to
density and c is the specific heat capacity. kx, ky and kz represent the 1400 W, the morphologies of molten pool changed from a flat shape
thermal conductivity in different directions. T, Q and t are tem­ to a cup-shape (Fig. 4a), implying that the molten pool fluidity be­
perature field distribution function, internal heat source and heat came better with the increase of laser power. Meanwhile, the un­
transfer time, respectively. melted W particles in the form of white spots were remained in each
The initial condition is defined as: molten pool. The width and depth of the molten pool increased from
1.61 ± 0.03 mm and 0.14 ± 0.01 mm to 2.54 ± 0.05 mm and
T (x, y , z , t) t = 0 = T0 (2) 1.41 ± 0.14 mm, which increased by 58% and 900%, respectively
(Fig. 4b). This indicated that the laser power had a greater influence
When t = 0, the temperature of substrate and powder is T0. The
on penetration depth. However, the height and contact angle of the
T0 = 298 K is set as initial temperature.
molten pool firstly increased and then decreased (Fig. 4c). Moreover,
According to the energy conservation law, the heat boundary
the proportion of the unmelted W particles in the molten pool was
condition is expressed [30]:
reduced gradually from 44.76% to 6.19% with the laser power in­
T creasing from 400 W to 1400 W (Fig. 4d).
K = ql qc qr
n (3) According to the obtained results of the molten pools, it could be
concluded that the laser powers had a remarkable influence on the
qc = hf (Tc T) (4) morphologies of the molten pools (Fig. 4a). As the laser powers in­
creased, both the width and depth of the molten pools increased
qr = (Tr4 T 4) (5) accordingly (Fig. 4b), implying that there existed a positive re­
lationship between the laser power, and molten pool width and
where ql , qc and qr are laser heat source, surface convection heat and depth. However, the height and contact angle increased at first then
thermal radiation energy, respectively. T∞, Tc and Tr are ambient decreased with the increasing laser powers (Fig. 4c), indicating that
temperature, convective surface temperature and surface radiation there was a threshold for the laser power. In order to reveal the
temperature, respectively. and represent Stefan-Boltzmann effects of laser power on the molten pool morphologies. The pene­
constant and thermal radiation coefficient of material surface. tration shape factors (W/D) and reinforcement form factors (W/H)

Fig. 3. Thermophysical properties of 95 W: (a) Phase transition curve with increasing temperature, (b) thermal conductivity and specific heat of 95 W.

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Table 2
Thermophysical parameters of 316 L stainless steel.

Temperature (℃) 25 200 400 600 800 1000 1200 1400

Thermal conductivity (W/(m K)) 55 40 25 25 27 100 150 150
Specific heat (J/(kg K)) 455 501 691 804 698 780 671 1065
Density (g/cm3) 7.73 7.68 7.61 7.54 7.46 7.46 7.35 7.21

Fig. 4. (a) Morphologies of the molten pools under various laser powers. Effects of laser powers on (b) width and depth, (c) height and contact angle. (d) Proportion of unmelted
W particles in the molten pools under different laser powers.

Table 3 to form sound metallurgical bonding with the substrate. Moreover,

The penetration shape factors (W/D) and reinforcement form factors (W/H) of the the insufficient energy input could result in low temperature within
molten pool under various laser powers (The values of W, D and H are average values). the molten pool and resultant a mass of unmelted W particles,
Laser power 400 W 600 W 800 W 1000 W 1200 W 1400 W hindering the formation of molten pool. Thus, the obtained height
W (mm) 1.612 1.962 2.247 2.276 2.424 2.54
and contact angle of the molten pool was small. While the value of
D (mm) 0.138 0.286 0.71 0.948 1.197 1.41 penetration shape factors reduced constantly with increasing laser
H (mm) 0.213 0.211 0.301 0.313 0.306 0.307 power, resulting in a cup-shaped molten pool with a large pene­
W/D 11.68 6.86 3.16 2.40 2.025 1.80 tration depth. In this case, a sound metallurgical bonding could be
W/H 7.57 9.30 7.47 7.27 7.92 8.27
obtained between alloy layer and substrate. Meanwhile, the molten
pool temperature would increase owing to the high laser power and
the reduce of melt viscosity, which could facilitate the wetting and
spreading of the melt. Therefore, the obtained height and contact
were introduced to evaluate the molten pool morphologies of LDED-
angle of the molten pool would be increased. However, further in­
fabricated 95 W [32]. The values of penetration shape factors and
creasing the laser power would bring excessive energy input and the
reinforcement form factors are listed in Table 3. Combined with the
evaporation of substrate material, leading to the sinking of melted
morphologies of the molten pool, it could be found that the molten
material. Thus, the height above the molten pool and the contact
pool morphologies were mainly determined by the penetration
angle would be decreased. Moreover, increasing the laser power
shape factors. During LDED-processed 95 W, the penetration shape
would cause larger penetration depth, resulting in a coarse heat
factors of the molten pools reduced constantly with the increasing
affected zone (HAZ), which was harmful to the mechanical perfor­
laser power. When the laser power was low, the value of penetration
mance of final parts [33]. Meanwhile, the large laser power could
shape factors was large. In this situation, the molten pool presented
cause more melting of the substrate and resultant contamination in
a flat shape with a small penetration depth, which was detrimental

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Fig. 5. OM images showing the microstructures of different positions within the molten pool at the laser power of 1400 W: (a) the full morphology of the molten pool, (b) the
columnar microstructure, (c) the cellular microstructure, (d) the equiaxed microstructure.
the molten pools. Thus, the previous deposited layers contaminated
by the substrate need to be cut off, causing the material waste.
Microstructure evolution within the molten pools
During LDED, the multiple physical processes are complex within
the molten pool. Under the combination of gravity, surface tension
and temperature gradient, the melt flow is formed. The melt flow
brings strong transfer of heat and mass, determining the mor­
phology, grain size and growth direction of the solidified structure
[34]. Usually, the columnar grains perpendicular to the edge of the
molten pool are prone to form at the bottom of the molten pool. At
the center of the molten pool, the cellular grains are easy to form.
However, the finer equiaxed grains are generated at the top of the
molten pool [26]. Similarly, the phenomena could be observed in the
molten pool of LDED-fabricated 95 W alloy. As shown in Fig. 5, the
typical microstructures at different positions of the molten pool are
presented. The unmelted W particle could be clearly observed in the
molten pool (Fig. 5a). It could be found that the columnar micro­
structure perpendicular to the molten pool boundaries was formed
at the bottom of the molten pool (Fig. 5b). While the cellular mi­
crostructure was observed at the center of the molten pool (Fig. 5c).
Moreover, at the top of the molten pool, a mass of fine grains was
generated (Fig. 5d). Meanwhile, large zones composed of fine grains
with the same orientation could be clearly observed.
The morphologies of solidification microstructures within the
molten pool is influenced by temperature gradient (G), cooling rate
(C) and solidification velocity (S) [35,36]. Usually, the size of the
microstructure is determined by the cooling rate (C). A fine grain is
prone to form under a high cooling rate. While, the G/S influences
the morphologies of the grains. As the value of G/S changes, the
morphologies of the solidified structure vary from equiaxed to co­
lumnar to cellular to planar [37,38]. To explain the microstructural
evolution in the molten pool, the temperature-time curves of three
typical monitoring points were extracted, respectively. Fig. 6a shows
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CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413
the temperature change along the depth direction of the molten
pool. It could be found that the temperature gradient (3.9 × 103
℃/mm) was maximal at the substrate contact surface. While the
temperature gradient at the molten pool surface was 2.6 × 103
℃/mm. Below the substrate, the temperature gradient decreased
gradually with the molten pool depth increasing. The temperature
evolution of the monitoring point A on the molten pool surface was
presented in Fig. 6b. The maximum temperature of 3918.19 ℃ was
obtained on the molten pool surface, which exceeded the melting
point of W, indicating that the melting was intense on the molten
pool surface. In this case, a maximal cooling rate of 4.16 × 104 ℃/s
was obtained. Fig. 6c is the temperature-time of the monitoring
point B on the substrate contact surface. While a maximum tem­
perature of 3142.65 ℃ and cooling rate of 2.6 × 104 ℃/s were ob­
tained. Thus, the temperature in the molten pool was unable to
completely melt the W particles. Furthermore, the temperature
profiles versus processing time of the monitoring point C at 2 mm
away from the molten pool surface is illustrated in Fig. 6d. As the
molten pool depth increased, the heat and mass transfer processes
weakened. As a consequence, the temperature in the molten pool
would decrease. The maximum temperature and cool rate were
1830.36 ℃ and 0.4 × 104 ℃/s, which were significant lower than
those of the top and center of the molten pool. The representative
results of GMax, CMax, SMax, GMax/SMax and corresponding grain
morphologies are listed in Table 4. Along the direction of the molten
pool depth, the cooling rate decreased from the top to the bottom,
resulting in the remarkable grain growth. While the G/S, also called
the shape control factor, determines the morphology of the micro­
structure. At the top of the molten pool, the obtained cooling rate
was maximal. While the GMax/SMax was only 1.63 × 102 ℃·s/mm2. In
this case, the fine equiaxed grains were easy to form (Fig. 5b). For the
center of the molten pool, the cooling rate of the melt was reduced,
which could facilitate the continuous grain growth along the cooling
direction. Meanwhile, the calculated GMax/SMax had a maximum
value of 5.82 × 102 ℃·s/mm2, which was much larger than that of the
M. Guo, G. Huang, L. Xi et al. CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413

Fig. 6. (a) Temperature gradient distribution along the depth direction under the laser power of 1400 W. Temperature profiles versus processing time at different positions along
the molten pool depth direction: (b) point A, (c) point B, (d) point C.

Table 4 presented a trapezoid shape with large bottom width and small top
The GMax, CMax, SMax, GMax/SMax and corresponding grain morphology of the three width. The polished surfaces of cross sections of LDED-processed
typical positions. The GMax and CMax represented the maximum temperature gradient 95 W bulk parts are presented in Fig. 7. When the laser power was
and the maximum cooling rate, respectively. The SMax was calculated by CMax/GMax.
1000 W, a small molten pool was formed under the bottom of the
Position Position A Position B Position C bulk parts. Meanwhile, a large amount of metallurgical defects in­
GMax (℃/mm) 2.6 × 103 3.9 × 103 1.5 × 103 cluding unmelted W particles, cracks and large pores were formed at
CMax (℃/s) 4.16 × 104 2.6 × 104 0.4 × 104 the edge of the bulk parts (Fig. 7a). As the laser power increased to
SMax = CMax/GMax (mm/s) 16 6.7 2.7 1200 W, the bottom of the molten pool was enlarged. The fusion
GMax/SMax (℃·s/mm2) 1.63 × 102 5.82 × 102 5.55 × 102
Grain morphology Equiaxed Cellular Columnar
zones expanded (Fig. 7b). However, the large cracks and pores re­
sulted from inadequate metallurgical bonding were remained at the
edge of the bulk parts. While the laser power of 1400 W was applied,
surface of the molten pool. Thus, a large GMax/SMax combined with a the fusion zones further expanded, as shown in Fig. 7c. A large
relatively low cooling rate could result in the formation of cellular molten pool at the bottom of the bulk parts was obtained. Mean­
grains (Fig. 5c). At the bottom of the molten pool, the cooling rate while, the densification level of the center part of the molten pool
was the smallest, while the GMax/SMax was relatively large with a was improved with less unmelted W particles. Due to the in­
value of 5.55 × 102 ℃·s/mm2. The small cooling rate could promote sufficient energy input caused by low laser power, the W particles
the sustained growth of grains. Meanwhile, the large GMax/SMax fa­ were unable to melt to form good wetting and spreading. Therefore,
cilitated the grains to form large columnar crystals. As a con­ a large amount of W particles without melting was observed at the
sequence, the large columnar grains perpendicular to the molten edge of the bulk parts, causing defects such as pores and cracks. As
pool edge were formed (Fig. 5d). the laser power increased, the input energy was enhanced, pro­
moting melting of W particles. As a result, the fusion zone enlarged.
Moreover, the temperature would be improved, resulting in the
Densification behavior and microstructure evolution of LDED-processed
decrease of the viscosity, further facilitating the densification of W.
95W alloy
Nevertheless, as laser power increased, the disturbance in the
molten pool intensified, causing more melting of substrate materials
According to the obtained results of LDED-processed 95 W
to infiltrate into the deposition layers. In this case, the contamina­
molten pool, it was concluded that a high laser power was favorable
tion was serious in the previous deposition of parts.
to the formation of regular molten pools. Thus, laser powers of
In order to understand the effect of deposition process on mi­
1000 W, 1200 W and 1400 W were chosen for fabrication of 95 W
crostructures, the microstructures evolution along the building
bulk parts. Due to the mass deposition effect, the 95 W bulk parts

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Fig. 7. OM images showing the view of the full cross section of LDED-processed 95 W under various laser powers: (a) 1000 W, (b) 1200 W, (c) 1400 W. SEM images displaying the
changes in microstructures along the building direction (BD). d, e, f and g represented the different regions.
direction (BD) of LDED-processed 95 W bulk part are displayed in
Fig. 7d-g. At the bottom of the bulk parts (region A), it could be
observed that a large amount of columnar grains growing perpen­
dicular to the molten pool boundaries was formed (Fig. 7d). At the
upper of the columnar region (region B), a mass of fragile dendritic
crystals was found. Meanwhile, some unmelted W particles re­
mained (Fig. 7e). With the increase of deposition height, the fragile
dendritic crystals grew into elongated dendrites. Moreover, some
dendrites were attached to the unmelted W particles, forming dis­
tinct core-shelled structures (Fig. 7e). As the deposition height in­
creased to the region C, which was located above the substrate
materials, the dendrites were significantly reduced with large
amount of core-shelled W particles remained (Fig. 7f). When the
deposition height reached to region D, which was away from the
substrate, the microstructures had a large difference, as clearly il­
lustrated in Fig. 7g. There was no dendritic crystal and core-shelled
W particles in the microstructures. Meanwhile, the irregular W
grains were formed with apparent grain boundaries. In order to
reveal the phases of the dendrites. Fig. 8a-e shows the element
distribution of the core-shelled structures. It could be seen that W
element mainly existed in the unmelted W particles in Fig. 8c. While
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CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413
the Ni element was distributed uniformly in the microstructure
(Fig. 8d). The Fe element was mainly included in the dark color
phase (Fig. 8e). Meanwhile, the gradient change of W and Fe ele­
ments was clearly depicted in Fig. 8b. The EDS results of the shells,
fragments and W particles were listed in Table 5. According to the
EDS results, the average atomic ratio of W: Fe for shells and den­
drites was close to 6: 7. The W particles contained almost 100% W
element. Thus, it could be concluded that the shell and fragments
were Fe7W6 intermetallic, the dark color phase was Fe-based phase
and the blocky particles were W particles.
Due to the characteristics of the thermal effect of layer-by-layer
deposition, the microstructures along the BD presented significant
differences. Since the melting point of stainless steel substrate was
far below the melting point of tungsten, the W powders were in­
evitable to enter into the iron matrix. At the bottom of the bulk parts,
the cooling rate was small and the GMax/SMax was large, as analyzed
in Section 3.2, which was prone to promote the formation of co­
lumnar grains. As the laser continued to move, the heat accumula­
tion effect increased, resulting in a more dissolution of W powders.
When the temperature reached to the peritectic reaction, the dis­
solved W reacted with Fe to form Fe7W6 [39]. Since the number of W
M. Guo, G. Huang, L. Xi et al. CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413

Fig. 8. (a) SEM image showing the core-shell structure. (b) Variations of W, Ni and Fe contents along the scanning line. (c–e) EDS mappings displaying the distributions of W, Ni
and Fe elements.

Table 5
EDS point analysis showing the element composition results for gray shells and white
W particles.

Points 1 2 3 4 5 6

W(%) 38.65 37.51 38.38 99.86 96.98 99.89

Ni(%) 56.27 57.18 56.73 0.14 3.02 0.11
Fe(%) 5.08 5.31 4.89 0.00 0.00 0.00

particles was small underneath the substrate, the Fe7W6 nucleated

freely in the solution, growing into fragments with different shapes
(Fig. 7d). With the deposition height increasing, the W particles in­
crease. Thus, some Fe7W6 nucleated on the W particles to form
shelled structure. Meanwhile, the Fe7W6 fragments coarsened and
grew into large dendrites due to the heat accumulation (Fig. 7e).
When the deposition height continued to increase, the diffusion and
migration of Fe weakened. Therefore, the Fe7W6 only nucleated on
the surface of the W particles and resultant shelled structure, as
shown in Fig. 7f. As the deposition position was away from the
substrate, the influence of Fe in the substrate disappeared. In this
case, the added nano Fe and Ni in the powders served as binders
under the action of high temperature, promoting the W to melt and
forming irregular W bulk grains [40], as shown in Fig. 7g. Fig. 9. XRD patterns of the 95 W alloy cut from the upper part of the substrate.

Mechanical properties of LDED-processed 95W alloy

To avoid the effect of Fe7W6 intermetallic on the mechanical
properties of LDED-processed 95 W alloy, the bulk parts were cut at
the position away from the substrate. Fig. 9 is the XRD patterns of
the 95 W bulk parts. It was obvious that there were no oxide and
intermetallic in the LDED-processed 95 W alloys. The BCC W and
little FCC nickel-iron solid solution phase were formed in 95 W.
Meanwhile, with the increase of laser powers, the intensity of FCC
nickel-iron significantly weakened. Although, the increase of laser
power could cause strong disturbance in the molten pool, the de­
position layer was free of contamination from the substrate material.
This indicated that the laser printing parameters were appropriate.
Fig. 10 shows the coefficient of friction with sliding time and
corresponding outlines of grinding grooves at different laser powers.
When the laser power of 1000 W was applied, the obtained COF
presented great fluctuation with time going on and a large COF of 0.9

409
M. Guo, G. Huang, L. Xi et al.
Fig. 10. Coefficient of friction (COF) with sliding time at various laser powers and corresponding outlines of grinding grooves: (a) 1000 W, (b) 1200 W, (c) 1400 W.
was obtained (Fig. 10a). As a result, a large grinding groove with a
width of 549.771 ± 0.001 µm and a depth of 8.939 ± 0.001 µm was
obtained. As the laser power increased to 1200 W, the COF with
sliding time was stable and an average COF of 0.6 was obtained
(Fig. 10b). Moreover, the width and depth of the obtained grinding
groove reduced to 438.412 ± 0.001 µm and 4.987 ± 0.001 µm, re­
spectively. With further increasing the laser power to 1400 W, the
average COF reduced to 0.5, as shown in Fig. 10c. In this case, the
obtained size of the grinding groove was the smallest with a width of
389.271 ± 0.001 µm and a depth of 2.545 ± 0.001 µm, demon­
strating that the wear performance was enhanced with the increase
of laser power.
It is commonly recognized that the hardness has a huge effect on
the final wear properties of the materials [41]. The improvement of
wear performance is probably owing to the increasing of hardness of
Fig. 11. Nanohardness of LDED-processed 95 W alloys at different laser powers.
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CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413
the materials. Fig. 11 shows the nanohardness of LDED-processed
95 W alloys under different laser powers. When the laser power of
1000 W was applied, it could be seen that the nanohardness curve
had a big fluctuation with an average value of 7.3 GPa. Due to the
limited energy input, the W particles were unable to be completely
melted, resulting in metallurgical defects such as cracks and pores.
Thus, the nanohardness values were fluctuated and resultant poor
wear performance. As the laser power increased to 1200 W, more W
particles were melted and resultant reduce of defects. Therefore, the
nanohardness values became stable and an average value of 8.1 GPa
was obtained, bringing relatively excellent wear performance. With
further increasing the laser power to 1400 W, it was found the
average nanohardness reached to a value of 8.6 GPa. This was owing
to the densification enhancement resulted from the increasing laser
energy input. Meanwhile, the nanohardness curve had a minimum
fluctuation, indicating that the internal uniformity of the obtained
sample was increased. As a result, the wear performance was the
most excellent with the smallest COF and the minimum loss of
abrasion.
The tensile tests were conducted to further study the mechanical
properties of LDED-processed 95 W alloy. The dimensions of small
sized samples were designed in Fig. 12a. The small sized samples for
tensile tests had a length of 20 mm and a thickness of 1 mm. All
tensile samples were cut along the scanning direction (SD) and the
contaminated parts below the substrate were avoided (Fig. 12a).
Fig. 12b shows the tensile stress-strain curves of LDED-printed 95 W
alloy under different laser powers. When a laser power of 1000 W
was applied, an ultimate tensile strength of 413 MPa and an elon­
gation of 0.38% were obtained. As the laser power increased to
1200 W, both the ultimate tensile strength and elongation were
improved with a value of 507 MPa and 0.72%. With the laser power
increasing to 1400 W, the ultimate tensile strength was 541 MPa and
the elongation was 0.99%, which was the highest among the
samples.
In order to reveal the fracture mechanism of LDED-fabricated
95 W, the fracture morphologies are shown in Fig. 13. When the laser
M. Guo, G. Huang, L. Xi et al. CIRP Journal of Manufacturing Science and Technology 39 (2022) 401–413

Fig. 12. (a) Schematic diagram of the cutting direction of 95 W tensile samples, (b) Tensile stress-strain curves of LDED-printed 95 W alloy under different laser powers.

Fig. 13. The fracture morphologies of LDED-processed 95 W under different laser powers: (a) 1000 W, (b) 1200 W, (c) 1400 W.

power was low (1000 W), the unmelted W particles could be clearly
observed on the fracture surface (Fig. 13a). Meanwhile, a mass of
cleavage planes was formed. The existence of unmelted W particles
caused the early failure and resultant low tensile strength and
ductility. As the laser power increased (1200 W), the input energy
density was high, resulting in more melting of W and resultant good
metallurgical bonding between molten pools. Therefore, the ob­
tained tensile strength and elongation were improved. However, due
to the brittleness of W, the fracture surface showed many cleavage
planes, indicating brittle fracture (Fig. 13b). With further increasing
the laser power (1400 W), the unmelted W particles were elimi­
nated. However, a small number of pores resulted from the element
burning and evaporation were observed (Fig. 13b). Moreover, the
fracture morphology demonstrated significantly difference with
mixing of cleavage planes and dimple networks. Two reasons ac­
count for the excellent tensile property. First, the increased energy
density brought by the large laser power could promote the densi­
fication and resultant high tensile strength. Second, the formed
dimple networks resulted from the intense reaction of nano Fe and
Ni during the rapid cooling could improve the ductility.
Conclusion
In the present study, the high specific gravity 95 W alloy were
successfully fabricated by LDED. The effects of laser powers on the
molten pool formation and microstructure evolution within the

411
M. Guo, G. Huang, L. Xi et al.
molten pool were studied. Subsequently, a dense 95 W alloy part was
manufactured and the mechanical properties of LDED-processed
95 W alloy were studied. The main conclusions were as follows:
1. As the laser power increased from 400 W to 1400 W, the molten
pool changed from a flat shape to a cup shape. The width and
depth of the molten pool increased from 1.61 ± 0.03 mm and
0.14 ± 0.01 mm to 2.54 ± 0.05 mm and 1.41 ± 0.14 mm, which
increased by 58% and 900%, respectively. Meanwhile, the pro­
portion of the unmelted W particles in the molten pool was re­
duced from 44.76% to 6.19%, demonstrating that a high laser
power could promote the metallurgical process within the
molten pool.
2. At the bottom of the molten pool, where the cooling rate
(0.4 × 104 ℃/s) and the temperature gradient were the smallest
(1.5 × 103 ℃/mm), the columnar grains were formed. At the
central of the molten pool, which was close to the substrate, the
temperature gradient was the largest with a value of 3.9 × 103
℃/mm and the cooling rate was 2.6 × 104 ℃/s, the cellular grains
were generated. At the top of the molten pool, where the cooling
rate was the largest (4.16 × 104 ℃/s) and the temperature gra­
dient was 2.6 × 103 ℃/mm, the finer equiaxed grains were
formed.
3. According to the obtained results of molten pool, the thin walls
were successfully fabricated by applying high laser powers. It was
found that above the substrate, the microstructure was com­
posed of irregular W bulk grains. While underneath the substrate,
due to the abundant Fe element in the substrate, the dissolved W
reacted with the Fe to form Fe7W6 intermetallic.
4. As a high laser power of 1400 W was applied, an excellent wear
performance was obtained with a smallest COF of 0.5. The im­
provement of wear performance was owing to the enhanced
nanohardness. Moreover, an excellent tensile strength of 541 MPa
and elongation of 0.99% were obtained at the laser power of
1400 W, which was due to the high densification and the ex­
istence of dimples from the reaction of nano Ni and Fe.
Declaration of Competing Interest
The authors declare that they have no known competing fi­
nancial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgments
This work was supported by the Science Challenge Project (No.
TZ2018006-0301-02 and No. TZ2018006-0303-03); the Basic
Strengthening Program (No. 2019-JCJQ-JJ-331); National Natural
Science Foundation of China for Creative Research Groups (Grant No.
51921003); The 15th Batch of “Six Talents Peaks” Innovative Talents
Team Program (No. TD-GDZB-001); the Fundamental Research Funds
for the Central Universities (NO. NC2020004). Meng Guo thanks the
Priority Academic Program Development of Jiangsu Higher
Education Institutions and financial support from Postgraduate
Research & Practice Innovation Program of Jiangsu Province (No.
KYCX20_0193).
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