Intermetallics 145 (2022) 107557

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Intermetallics
journal homepage: www.elsevier.com/locate/intermet

The manufacturing process optimization and the mechanical properties of

FeCoCrNi high entropy alloys fabricated by selective laser melting
Yingbo Peng a, c, *, Caijun Jia a, Lingfeng Song d, Yuchao Bian a, Hongwei Tang a, Guanglu Cai a,
Gaoyan Zhong a, b, **
a
College of Engineering, Nanjing Agricultural University, Nanjing, 210031, China
b
State Key Laboratory of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology, Wuhan, 430074, China
c
Powder Metallurgy Research Institute, Central South University, Changsha, 410083, China
d
Huzhou Vocational and Technical College, Huzhou, 313099, China

A R T I C L E I N F O A B S T R A C T

Keywords: The quality of metal parts fabricated by selective laser melting (SLM) is strongly depended on the manufacturing
Selective laser melting process parameters. The establishment of relationship between manufacturing parameters and the formability is
High entropy alloy the effective way to obtain forming parts with high density, defect-free and excellent mechanical properties by
Processing parameters
SLM. In this study, the effect of SLM process parameters on the relative density (RD) and mechanical properties of
Microstructures
Mechanical properties
FeCoCrNi high entropy alloys (HEAs) were systematically investigated, involving single tracks, single layers and
block samples. By optimizing the laser power, scanning speed and hatching space, the highest RD of 99.85% was
obtained under the moderate energy density of 95.24 J/mm3, with no defect as prosity, cracks, un-melted
powders and spheroidization under other SLM parameters. The tiny changes in RD significantly affected the
mechanical properties of FeCoCrNi HEAs. The highest RD sample corresponded to the optimal comprehensive
mechanical properties of 585 MPa in yield strength, 714 MPa in ultimate strength and 45.30% in elongation. The
elevation of mechanical properties attributed to the high RD, defect-free, grain refinement and the unique
cellular substructure.

1. Introduction Hitherto, scientists worldwide have made many long-term and

Additive manufacturing (AM) provided effective approaches and
technical methods in directly manufacturing robust structures with
complex geometries from its computer-aided design [1,2]. Selective
laser melting (SLM) is one of the most promising technology of AM.
Among the different types of materials, metals and alloys fabricated by
SLM are the most challenging issue [3–5]. Due to the high repeatability
manufacturing strategy of line-by-line and layer-by-layer of SLM, some
additional processing-related factors will be generated, such as porosity,
residual stress and unique microstructure, etc [6–8]. The manufacturing
strategy and the involvement of the additional factors increase consid­
erable complexity to the exploration of the SLM formability. Therefore,
the structural integrity and performance reliability are still the main
challenges hindering the wide application of SLM. The key to solve this
challenge is to establish the elaborate correlation among process pa­
rameters, microstructure and mechanical properties.
beneficial efforts in SLM technology, and the researches mainly focused
on two aspects. On one hand, the effect of process parameters on the
SLM processability and formability has been extensively investigated. By
adopting some mature and commercial materials in SLM technology,
such as stainless steel [9], Ni-based alloy [10], copper alloy [11], tita­
nium alloy [12] and etc, the formability of single track/layer [13–17],
relative density [18] and surface roughness [19] were studied by opti­
mizing process parameters. On the other hand, the microstructure and
mechanical properties of many advanced materials by SLM has been
studied, in order to achieve remarkable performance, such as high
strength aluminum alloy [20], ultra-high strength martensitic steel [21],
especially high entropy alloys (HEAs) [22–24], which usually exhibited
a simple solid solution structure with superior mechanical properties
[25].
The SLM forming characteristics (domain by domain) and the addi­
tional processing factors (relative density, defects and unique

* Corresponding author. College of Engineering, Nanjing Agricultural University, Nanjing, 210031, China.
** Corresponding author. College of Engineering, Nanjing Agricultural University, Nanjing, 210031, China.
E-mail addresses: ybpengnj@njau.edu.cn (Y. Peng), gyzhong@njau.edu.cn (G. Zhong).

https://doi.org/10.1016/j.intermet.2022.107557
Received 14 December 2021; Received in revised form 17 March 2022; Accepted 27 March 2022
Available online 30 March 2022
0966-9795/© 2022 Elsevier Ltd. All rights reserved.
Y. Peng et al.
substructures caused by SLM) significantly affected the microstructures
and mechanical properties of the adopted materials. The small change of
these factors, such as relative density or defects, are very likely to lead to
performance fluctuations. Therefore, according to the characteristics of
SLM manufacturing process and material adopted, the SLM parameters,
microstructure and mechanical properties need to be systematically
studied and developed the correlation of these aspects, so as to provide a
theoretical and technological basis for SLM to prepare high-performance
and defect-free alloy parts.
In the presented study, FeCoCrNi HEAs with face-cubic centered
structure was adopted as the target material for SLM. The effect of laser
power, scanning speed and hatching space on the formability of single
track, single layer and block samples was systematically investigated.
The SLM processing parameters were optimized to achieve the full-
dense, defects-free sample. Moreover, the relationship between rela­
tive density (RD) and mechanical properties was studied.
2. Materials and methods
Gas atomized Fe25Co25Cr25Ni25 (at. %) equiatomic HEAs powder
(15–53 μm) was used in SLM process. The spherical powders (D10: 21.6
μm, D50: 35.1 μm, D90: 55.3 μm) exhibited good flowability with Hall
fow rate of 18.97 s/50 g, and powder repose angle of 27.43◦ , which was
necessary for well powder spreading during SLM.
The single tracks, single layers and block samples of FeCoCrNi HEAs
were fabricated in an SLM powder-bed equipment (HK PM250, Wuhan
Huake 3D Technology Co., LTD). The powders were dried at 80 ◦ C for
24 h before SLM. The 316L stainless steel substrates were cleaned with
alcohol. The SLM process was conducted under constant flow of argon to
minimize the oxygen contamination (residual oxygen concentration,
approx. 0.1%). The detailed description for SLM process optimization
are as follows:
Firstly, the full factor experiments of single tracks were carried out.
According to the combination of different laser power and scanning
speed, 48 single track samples with length of 5 mm were prepared. By
observing the size and the morphology of single tracks, the typical single
tracks were classified according to the linear energy density, so as to
obtain the optimized process window of laser power and scanning speed.
Secondly, on the basis of single track experiments, different hatching
space was set to prepare single layer samples with the size of 5 mm × 5
mm. According to the single layer morphology and lapping rate, the
optimized range of hatching space was obtained. Finally, block sample
experiments were carried out to comprehensively consider the coupling
effects of laser power, scanning speed and hatching space. During the
preparation of block samples, the laser scanning direction was reversed
67◦ between adjacent layers to avoid the accumulation of thermal stress
in the forming process. A total of 9 block samples with different SLM
parameter combinations were prepared, with a size of 10 mm × 10 mm
× 5 mm. By observing the RD, microstructures and defects of block
samples, the optimal SLM process parameters of FeCoCrNi HEAs was
determined according to the volume energy density.
A FEI Quanta FEG 250 scanning electron microscope (SEM) was used
to characterized the microstructure of the SLM samples. A Philips CM
200 transmission electron microscopy (TEM) was used to identify the
substructures of SLM sample. The TEM specimen was prepared by Gatan
691 ion-beam thinner. Electron backscatter diffraction (EBSD) was
carried out by HKL Channel5 EBSD Oxford Instruments. EBSD specimen
was prepared by vibration polishing (Buehler) and argon ion polishing
(IB–19530CP, Jeol). Rectangular dog-bone-shaped tensile specimens
was directly fabricated by SLM with a gauge size of 10 mm × 5 mm × 3
mm size. The uniaxial tensile tests were performed at room temperature
with a strain rate of 0.001/s using an Instron 5982/100 kN testing
machine and each tensile specimen was tested at 3 times under the same
conditions. The RD of SLM block samples was measured by Archimedes
drainage method.
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Intermetallics 145 (2022) 107557
3. Results and discussions
3.1. SLM process optimization
3.1.1. Single track
In SLM process, a 2-D layer is formed by lapping multiple tracks, and
then the 3-D entity is formed by superposition of multiple 2-D layers.
Single track is the smallest and basic unit in SLM, so the stability and
continuity of single tracks are the basis to ensure the forming quality
[26]. The main factors of single track formability are laser power (P) and
scanning speed (v). Therefore, the full factorial experiment of P and v
was set. The laser power was set at 6 levels (150–400 W with 50 W
step-length), and the scanning speed was set at 6 levels (250–1300 mm/s
with 150 mm/s step-length). A total of 48 single track samples with
length of 5 mm were prepared.
The track width is the important indicator for evaluating the single
track forming quality. The relationship between process parameters (P
and v) and the track width is shown in Fig. 1. With the constant P, the
track width decreased with the increasing v. With the constant v, the
track width increased with the increasing P. By range analysis, range R
> 0 indicates that this factor has an impact on the results, and the greater
the R is, the more significant the impact is. It can be seen from Table 1
that both P and v exhibited great impact on the track width, and the
impact of v was more significant than P. This is because v directly de­
termines the contact time between the laser beam and the powders.
When v is slow, the contact time between the laser and the powders is
long, resulting in the continuous existence and expansion of molten
pool, so a single track with large width is formed. On the contrary, when
the v is high, the powder cannot be fully melted as the short contact time
between the laser and the powders, resulting in spheroidization, thus
forming a single track with small width.
Fig. 2 shows the single track morphology that the scanning speed is
250–1300 mm/s with laser power of 400 W. When v was 250 mm/s
(Fig. 2(a)), the laser energy input was high with long-time contact with
powders, so the track width at this v reached about nearly twice the
width of the single track formed at other scanning speeds. When v
increased (250–1000 mm/s in Fig. 2(a-e)), the track width decreased
gradually. When v was more than 1000 mm/s, the change of single track
width tended to be stable, but there was a big difference in its
morphology, as shown in Fig. 2(f–h), when v reached 1300 mm/s, due to
the insufficient laser energy to melt the powder completely, the tem­
perature of the molten pool was low. The liquid metal had a high
Fig. 1. Relationship between the width of single tracks and SLM pro­
cess parameters.
Y. Peng et al. Intermetallics 145 (2022) 107557

Table 1
Range analysis of HEAs single track width.
k1 k2 k3 k4 k5 k6 k7 k8 R

P (W) 148.2 151.8 155.4 160.8 168.2 177.7 29.5

v (mm/s) 257.5 183.1 169.7 155.6 146.4 125.8 123.3 122.2 135.2

Fig. 2. Morphology of single tracks at different scanning speed and laser power of 400 W. (a) 250 mm/s, (b) 400 mm/s, (c) 550 mm/s, (d) 700 mm/s, (e) 850 mm/s,
(f) 1000 mm/s, (g) 1150 mm/s, (h) 1300 mm/s.

viscosity and could not be well spread, so there was a serious spher­
oidization phenomenon (Fig. 2(h)). As a typical SLM defect, spheroid­
ization is detrimental to the forming quality [27], exhibiting obvious
segmentation of the single track.
Fig. 3 shows the single track morphology that the laser power is
150–400 W with scanning speed of 700 mm/s. The laser power directly
determines the input energy during SLM process. When P was 150 W,
the single track exhibited segmentation and spheroidization with poor
forming quality due to the low energy input. With the increase of P, the
forming quality of tracks was improved, as shown in Fig. 3(a). When P
increased to 300 W and 350 W, the moderate laser energy input enabled
the powders to be fully melted and the molten pool can be well spread.
Therefore, a relatively flat and regular single tracks were formed in
Fig. 3(d and e). When P increased to 400 W, as shown in Fig. 3(f), due to
the high laser energy input, the single track became wider and showed a
certain extent of excessive melting.
From the above analysis, it can be seen that both laser power and
scanning speed influenced the formability of single track. Therefore,
linear energy density is introduced to comprehensively consider the
effect of P and v. The equation of linear energy density (λ) for single track
is shown as below [28]:
P
λ= (1)
v
The morphology of the single tracks of different λ are shown in Fig. 4
with marked wetting angle θ (The smaller the θ is, the stronger the
spreading ability of the liquid metal of melting pool on the substrate is.).
According to the morphology of different λ, the 48 single tracks can be
divided into three types, as shown in Figs. 4 and 5.
Type I: high laser energy input, the track exhibited poor surface
quality, wide width (>200 μm) and low height (<50 μm). When λ was
high (1.40 J/mm), as shown in Fig. 4(a), the excessive melting caused in

Fig. 3. Morphology of single tracks at different laser power and scanning speed of 700 mm/s (a) 150 W, (b) 200 W, (c) 250 W, (d) 300 W, (e) 350 W, (f) 400 W.

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Y. Peng et al. Intermetallics 145 (2022) 107557

Fig. 4. The three typical morphology of single tracks of FeCoCrNi HEAs by SLM. (a) 1.40J/mm, (b)0.52 J/mm, (c) 0.27 J/mm.

whether the adjacent track can be closely bonded. In the process of SLM,
the area in the laser beam diameter is not evenly distributed, but
gradually decreases from the center to the edge of the area, showing a
Gaussian distribution. Therefore, in order to obtain better forming
quality, it is necessary to adjust the h to make the adjacent track to have
a certain lapping rate. The lapping of the tracks is shown in Fig. 6.
In Fig. 6, w is the track width, h is the hatching space, and d is the
lapping width. The lapping rate η is shown in Equation (2) [28].
d w− h h
η= = =1− (2)
w w w
The optimized combination of P and v (300 W, 700 mm/s, single
track width 150 μm) in the above single track experiments was selected
to conduct the single layer experiments with different hatching space.
The 6 h levels were set and the corresponding lapping rates calculated
according to Equation (2) are shown in Table 2, and the single layers
formed by SLM are shown in Fig. 7.
The single layer morphology with h of 0.03 mm and 0.05 mm is
shown in Fig. 7(a) and (b), respectively. The high lapping rate made the
Fig. 5. The process window of FeCoCrNi HEAs single tracks by SLM.
large re-melted area, the powders in this area exhibited overmelt and
oxidation due to double melting. In addition, the serious thermal stress
disturbance and large surface tension gradient of the molten pool.
concentration was formed, and obvious thermal cracks appeared in the
Strong Marangoni effect [29] drove the melt to flow at high speed, and
single layer. When h was 0.07 mm, although the lapping rate decreased,
the melt droplets were more likely to escape from the molten pool,
there were still some overlapping areas. When h was 0.09 and 0.11 mm,
resulting in splashing and even direct vaporization. Thus, the thickness
with the moderate lapping rate, the surface of single layer surface was
of the powder layer reduced, forming the single track with poor surface
relatively flat, and there was no overmelting or separation of adjacent
quality, wider width and smaller θ.
tracks in Fig. 7(d) and (e). When h increased to 0.13 mm, due to the low
Type II: moderate laser energy input, the track was continuous and
lapping rate, some incomplete fusion defects were observed at the
smooth with moderate width (120–150 μm) and good wettability (θ <
lapping area of adjacent tracks and some powders in the lapping area
90◦ ), as shown in Fig. 4(b). When λ was 0.52 J/mm, during the forma­
were not be fully melted, as shown in Fig. 7(f). Therefore, the lapping
tion, the Marangoni convection in the molten pool was moderate, so the
rate should be reduced as far as possible on the premise that the adjacent
track was regular, continuous and the surface was smooth with good
tracks can ensure closely lapping, so as to reduce the ineffective re-
wettability.
Type III: low laser energy input, the track was discontinuous and
spheroidized with poor wettability (θ > 90◦ ) as shown in Fig. 4(c). When
λ was low (0.27 J/mm), the input laser energy was not enough to melt
the powders, resulting in the poor bonding between the single track and
the substrate. Due to the relatively low Marangoni convection and
Plateau-Rayleigh instability [30], the molten pool tended to change
from cylindrical to spherical to reduce its surface energy, exhibiting
spheroidization phenomenon and forming a narrow and discontinuous
single track with θ over 90◦ . If the track is irregular or even incon­
tinuous, the forming quality will declined rapidly with the increase of
forming height.
From Fig. 5, it can be seen that the suitable SLM process parameters
of FeCoCrNi HEAs single track were: 300–400 W in P, 700–1000 mm/s
in v, and the corresponding λ was about 0.30–0.57 J/mm.

3.1.2. Single layer

The 3-D entity formed by SLM is composed of 2-D layers, so it is of
great significance to investigate the formability of single layer [31].
Besides P and v, the formation of single layer is closely related to the
hatching space h. Hatching space is defined as the vertical distance be­
tween the center of adjacent laser beam during SLM, which determines Fig. 6. Schematic diagram of track lapping.

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Y. Peng et al. Intermetallics 145 (2022) 107557

Table 2 mm3, the RD began to decrease, as 93.13% at 222.22 J/mm3.

Hatching space and corresponding lapping rate. The microstructures of the FeCoCrNi HEAs samples with different
Hatching 0.03 0.05 0.07 0.09 0.11 0.13 volume energy density are shown in Fig. 9. When E was 44.44 J/mm3
space (mm) (sample #4 in Table 3) in the low energy density region, corresponding
Lapping rate 81.0 ± 68.4 ± 55.7 ± 43.0 ± 30.4 ± 17.7 ± to type III single track (Fig. 5), the RD was only 92.44%. As shown in
(%) 5.1 6.3 7.8 5.6 4.0 3.2 Fig. 9(a), due to the low E, there were un-melted powders and serious
spheroidization occurred. There was two kinds of pores in the sample. In
Fig. 9(b), Due to the narrow tracks and high hatching space (0.11 mm),
melting area and improve the forming quality. The surface quality of the lapping area cannot be effectively formed between adjacent tracks.
single layer of FeCoCrNi HEAs was optimized when the h was 0.09–0.11 The incomplete fusion defects were finally generated and small pores
mm and the lapping rate was 30.4–43.0%. with an average size of about 20 μm were formed. In Fig. 9(c), some
large pores with size of ~150 μm were observed with un-melted pow­
3.1.3. SLM formed HEA block ders inside. As the low laser energy input, the un-melted powders
SLMed HEA block experiments were carried out to obtain high-RD gathered and formed spheroidization, finally forming large pores defects
HEA block samples to investigate on the coupling effect of SLM pro­ after the accumulation. These pores seriously affectded the RD of the
cess parameters (P, v and h) and analyze the influence factor significance HEAs block samples.
on RD. The block experiments were shown in Table 3. When E was 95.24 J/mm3 (sample #2 in Table 3) in the moderate
Range and variance analysis were carried out according to the energy density region, the RD of HEA sample reached 99.85% of almost
experimental results in Table 3. As shown in Table 4, the range of P is the full-dense, corresponding to type I single track. As shown in Fig. 9(d),
largest, so P has the greatest influence on the RD of FeCoCrNi HEAs by
SLM. The influence of h is the smallest, and the influence of v is between
P and v. Moreover, the F value in variance analysis is the ratio of the sum Table 3
of mean squares caused by the change of factor level to the sum of mean SLM process parameters and RD of FeCoCrNi block samples (50 μm layer
squares caused by error. The larger the F value is, the more significant thickness).
the influence of this factor on the results is. Given significance level α = No. P (w) v (mm/s) h (mm) E (J/mm3) RD (%)
0.05, P has the most significant influence on the RD, followed by v. The F 1 200 400 0.07 142.86 96.60 ± 0.26
value of the h is less than 1, which does not exceed the influence of the 2 300 700 0.09 95.24 99.85 ± 0.13
test error on the results, so h has little influence on the RD. Therefore, it 3 400 1000 0.11 72.73 95.10 ± 0.38
can be seen from the experiment and calculation results that the influ­ 4 200 1000 0.11 44.44 92.44 ± 0.63
5 300 400 0.09 136.36 98.50 ± 0.39
ence factor significance on RD is as follows: P > v > h. The optimal
6 400 700 0.07 163.27 96.03 ± 0.42
combination of SLM process parameters is 300 W of laser power, 700 7 200 700 0.11 51.95 94.90 ± 0.21
mm/s of scanning speed and 0.09 mm of hatching spacing. 8 300 1000 0.07 85.71 98.10 ± 0.18
Considering the coupling effect of various factors in SLM, the volume 9 400 400 0.09 222.22 93.13 ± 0.76
energy density is introduced, which is defined as [32]:
P
E= 3a Table 4
vhl
Analysis of variance and range.
Where E is volume energy density (J/mm3), l is layer thickness (mm). Factors Degree of Sum of deviation Sum of mean F Range
The relationship between E and RD is shown in Fig. 8. The RD increased freedom squares squares value
firstly and then decreased, with the increase of E. When E was lower than P 2 19.252 9.626 4.56 3.54
85.71 J/mm3, the RD was only 92.44% at 44.44 J/mm3. When E was v 2 4.8480 2.420 1.15 1.58
85.71 J/mm3-136.36 J/mm3, the RD was above 98%, and the highest h 2 3.075 1.538 0.73 1.24
Error 2 4.224 2.112
RD was 99.85% at 95.24 J/mm3. When E was higher than 136.36 J/

Fig. 7. Morphology of single layers with different hatching space. (a) 0.03 mm, (b) 0.05 mm, (c) 0.07 mm, (d) 0.09 mm, (e) 0.11 mm, (f) 0.13 mm (P = 300 W, v =
700 mm/s).

5
Y. Peng et al.
Fig. 8. Relationship between volume energy density and the RD of FeCoCrNi
HEA block samples by SLM.
due to fully melted powders, the molten pool was well spread with good
wettability, forming a smooth and fish-scale like morphology. Moreover,
moderate overlapping rate (h = 0.09 mm) enabled the adjacent tracks to
be closely integrated. Finally, the fully-dense HEAs sample was obtained
without defects.
When E was 222.22 J/mm3 (sample #9 in Table 3) in the high energy
density region, corresponding to type II single track, the RD was 93.13%.
As shown in Fig. 9(e) and (f), the sample exhibited excessive melting,
and obvious thermal cracks were observed. Cracks propagated
throughout multiple tracks or along the overlapping of adjacent tracks.
With high E, the molten pool was unstable at high temperature. Due to
excessive residual heat, the thermal stress accumulated continuously
until exceeding the yield strength of HEAs, the thermal cracks generated
rapidly and propagated in order to release stress. In addition, because
the overlapping of adjacent tracks was repeatedly melted, the absorbed
heat was much higher than that in other areas, resulting in the cracks
along the overlapping area. Thermal cracks seriously deteriorated the
RD of HEAs samples.
Fig. 9. Surface morphology of FeCoCrNi HEAs block samples under different volume energy density. (a) E = 44.44 J/mm3, (b) and (c) the defects in (a), (d) E =
95.24 J/mm3, (e) and (f) E = 222.22 J/mm3.
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Intermetallics 145 (2022) 107557
3.2. Mechanical properties
SLM process parameters affect the RD, and RD directly affects the
mechanical properties of SLM-formed FeCoCrNi HEAs. Fig. 10 and
Table 5 are tensile stress-strain curves and mechanical properties of
HEAs at room temperature under different volume energy density (the
corresponding parameters are shown in Table 3), respectively. With the
increase of E, the yield strength, ultimate strength and elongation of
FeCoCrNi HEAs all exhibited the trend which was consistent with the
RD. The HEAs sample formed under the optimized SLM process pa­
rameters (P = 300 W, v = 700 mm/s, h = 0.09 mm, E = 95.24 J/mm3)
had the best tensile mechanical properties. The yield strength, ultimate
strength and elongation were 585 MPa, 714 MPa and 45.30%, respec­
tively. The yield strength and ultimate tensile strength both decreased
with the RD of the HEA samples. Small changes in density of FeCoCrNi
HEAs prepared by SLM can directly lead to large fluctuations in me­
chanical properties. Therefore, the systematical optimization of SLM
process parameters plays an important role in improving the mechanical
properties of HEAs.
The fracture morphology of the HEAs tensile samples were observed
to investigate the effect of RD on the mechanical properties. Fig. 11(a)
shows the HEAs tensile sample of 92.44% RD (44.44 J/mm3), the un-
melted powders and the cavity caused by the gathered powders
formed the source of crack initiation. Due to the low energy input, the
defect of un-fusion and pores caused the degradation of both the
strength and elongation, only 381 MPa of yield strength and 39.71% of
elongation. On the contrary, when E was high (222.22 J/mm3) in Fig. 11
(b), the residual stress produced by the high solidification rate of SLM
led to the crack initiation and propagation along the grain boundary,
resulting in the decease of RD and mechanical properties of HEAs. As the
moderate E (95.24 J/mm3) in Fig. 11(c) and (d), almost no defects were
found, and the fractrue morphology was smooth with the typical ductile
fracture characteristics of dimple fracture, exhibiting the best compre­
hensive mechanical properties.
Table 6 is the room-temperature tensile properties of FeCoCrNi HEAs
prepared by different conventional methods. The yield strength of the
FeCoCrNi HEAs prepared by casting method was generally no more than
200 MPa. The large grain size and the segregation reduced the me­
chanical properties of the alloy. Powder metallurgy method significantly
refined the grain, and the yield strength was nearly twice as high as that
of casting method. In the present study, the yield strength and ultimate
tensile strength of FeCoCrNi HEAs were much higher than those of
casting method respectively, and maintaining relatively good ductility,
Y. Peng et al. Intermetallics 145 (2022) 107557

with the aspect ratio of 0.6. Higher volume fraction of grain boundaries
impede dislocation motion and bring strengthening effect. The rela­
tionship between yield strength and grain size can be described by the
classical Hall-Petch Equation [41,42]:
k
σ y = σ0 + √y̅̅̅ 3b
d

where σy is the yield stress, σ0 is again the lattice friction stress, ky is the
strengthening coefficient and d is the average grain size. According to
Equation (3), yield strength increase caused by grain size difference
(ΔσG) can be defined as:
1 1
Δσ G = ky (√̅̅̅̅̅ − √̅̅̅̅̅ ) (4)
d1 d2

Fig. 10. Stress-strain curves of FeCoCrNi HEAs with different volume energy
density. The inset shows the tensile specimens after deformation.
where d1 and d2 represent the grain size of the FeCoCrNi HEAs by SLM in
this work (15 μm) and the conventional as-cast method (289 μm, e.g. as-
cast FeCoCrNi alloy in Ref. [33]). The value of ky adopted is 226
MPa/μm1/2 from the FeCoNiCrMn system [43]. According to Equation

Table 6
Table 5 Mechanical properties of FeCoCrNi HEAs prepared by different preparation
Tensile properties of FeCoCrNi HEAs with different volume energy density. methods.
E (J/ RD Yield strength Ultimate tensile Elongation Preparation Grain Yield Ultimate tensile Elongation
mm3) (%) (MPa) strength (MPa) (%) method size (μm) strength strength (MPa) (%)
44.44 92.44 381 ± 15 540 ± 13 39.71 ± 3.37 (MPa)
85.72 98.10 487 ± 7 669 ±9 44.53 ± 2.36 As-cast 289 165 453 68 [33]
95.24 99.85 585 ± 8 714 ±7 45.30 ± 2.97 As-cast ~200 140 488 83 [34]
163.27 96.03 450 ± 10 649 ± 10 43.80 ± 2.73 As-cast ~300 151 446 64.8 [35]
222.22 93.13 435 ± 12 585 ±7 36.53 ± 3.45 As-cast N/A 185 360 38 [36]
MA + SPS N/A 419 487 N/A [37]
Hot extrusion 34.5 359 712.5 56 [38]
due to the 99.85% RD and no SLM defects. Hot rolling 14 310 660 42 [39]
It is well known that grain refinement can improve the strength of SLM N/A 495 695 30 [40]
SLM (this 15 585 714 45.30
alloys. The extremely high cooling rate (106 K/s) during SLM greatly
study)
refined the grains of HEA, which increased the yield strength and ulti­
mate tensile strength. As shown in Fig. 12(a) and (b), the average grain N/A: Not available in the reference. MA: Mechanical alloying. SPS: Spark plasma
size of HEA fabricated under the optimal E of 95.24 J/mm3, is ~15 μm sintering.

Fig. 11. Fracture morphology of FeCoCrNi HEAs with different volume energy density.

7
Y. Peng et al.
Fig. 12. Microstructures of FeCoCrNi HEAs with E = 95.24 J/mm3. (a) Optical microstructure, (b) EBSD reconstruction map with grain orientation, (c) and (d) SEM
and TEM morphology showing cellular structures.
(4), the increase of yield strength caused by grain refinement by SLM is
45.2 MPa, showing that grain refinement contributes partly to the
improvement of yield strength. However, the effect of fine grain
strengthening calculated according to Hall-Patch Equation on yield
strength is not significant compared to the 400 MPa improvement.
Therefore, there are other factors contributing to the strength
improvement.
During SLM process, some special microstructure will be produced.
Besides the fish-scale like molten pool line, it can also form a unique
submicron or nanoscale cellular structure inside the grain, as shown in
Fig. 12 (c). The cellular substructure is a unique morphology of metallic
materials by SLM, which is commonly observed in FCC-structure alloys.
The formation of cellular structure is caused by the high G/R value (G-
temperature gradient, R-crystal growth rate) due to the extremely non-
equilibrium solidification in SLM [44]. This cellular structure can be
considered as a dendrite structure without secondary dendrite arms. The
growth direction of the cellular structure is determined by the crystal­
lographic preferred orientation and the local temperature gradient [45].
For FeCoCrNi HEAs with FCC structure, the fastest growth direction is
the [001] direction closest to the temperature gradient field [23], as
shown in Fig. 12 (b). The cellular structure is closely related to dislo­
cation motion [46]. Due to the high thermal stress generated in the
layer-by-layer rapid melting process, this internal stress exceeds the
yield strength of the material at high temperature, which induces plastic
deformation, leading to dislocation formation, multiplication and
accumulation. Element segregation occurs at the wall of cellular struc­
ture, therefore, due to the pinning effect of segregation on dislocation,
dislocations are enriched at the cellular wall [47], forming cellular walls
with high dislocation density and inside-cellular with relatively low
dislocation density, as shown in Fig. 12(d). Compared with conventional
forming methods, nanoscale cellular substructures are considered to be
an important factor for improving the strength of alloys by SLM.
4. Conclusions
In the presented study, according to the high repeatability
manufacturing strategy of line-by-line and layer-by-layer in SLM, the
SLM processing parameters were optimized by single tracks, single
8
Intermetallics 145 (2022) 107557
layers and block samples, the relationship between RD and mechanical
properties of FeCoCrNi HEAs fabricated by SLM was revealed. The
following conclusions can be drawn:
(1) The effect of scanning speed on the single track was more sig­
nificant than laser power. The optimal SLM process parameters of
FeCoCrNi HEAs single track were: 300–400 W in laser power,
700–1000 mm/s in scanning speed, forming continuous and
smooth track with 120–150 μm width and good wettability (θ <
90◦ ).
(2) The hatching space influenced the single-layer formability by
affecting the lapping rate of adjacent tracks. When the hatching
space was optimized as 0.09–0.11 mm and the moderate lapping
rate was 30.4–43.0%, the surface quality of single layer of
FeCoCrNi HEA was relatively good with no defects.
(3) The priority of SLM processing parameters affecting the FeCoCrNi
HEAs block sample on RD was: laser power > scanning speed >
hatching space. The RD exhibited a parabolic trend with the in­
crease of volume energy density E. The improper E caused the
defects of un-melted powders, porosity and thermal cracks. When
E was 95.24 J/mm3, the RD reached 99.85%.
(4) The minor discrepancy of RD significantly affected the mechan­
ical properties of FeCoCrNi HEAs. The optimal comprehensive
mechanical properties were 585 MPa of yield strength, 714 MPa
of ultimate strength and 45.30% of elongation with 99.85% RD
sample. The elevation of strength attributed to the grain refine­
ment and the unique cellular substructure caused by the rapid
solidification during SLM.
Author statement
Yingbo Peng: Conceptualization, Writing- Original draft, Supervi­
sion, Funding acquisition; Caijun Jia: Investigation, Data curation,
Software; Lingfeng Song: Methodology, Investigation; Yuchao Bian:
Formal analysis, Data curation; Hongwei Tang: Validation; Guanglu
Cai: Visualization; Gaoyan Zhong: Project administration, Resources.
Y. Peng et al. Intermetallics 145 (2022) 107557

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