Materials and Manufacturing Renaissance Additive Manufacturing of Highentropy Alloys

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Materials and manufacturing renaissance: Additive manufacturing of high-

entropy alloys
Article in Journal of Materials Research · June 2020

DOI: 10.1557/jmr.2020.140
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DOI: 10.1557/jmr.2020.140
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Materials and manufacturing renaissance: Additive

manufacturing of high-entropy alloys
Jinyeon Kim, Akane Wakai, Atieh Moridia)
Sibley School of Mechanical and Aerospace Engineering, Cornell University, Ithaca, New York 14850, USA
a)
Address all correspondence to this author. e-mail: moridi@cornell.edu
Received: 17 February 2020; accepted: 15 May 2020
The disruptive potential of additive manufacturing (AM) relies on its ability to make customized products with
considerable weight savings through geometries that are difficult or impossible to produce by conventional
methods. Despite its versatility, applications of AM have been restricted due to the formation of columnar grains,
resulting in solidification defects and anisotropy in properties. To achieve fine equiaxed grains in AM, alloy design
and solidification conditions have been optimized in various alloy systems. In this review paper, the
microstructure of high-entropy alloy (HEA) parts produced by selective laser melting and powder-based directed
energy deposition is investigated. Solidification maps based on laser process parameters (as opposed to most
commonly used solidification velocity and temperature gradient) are constructed by compiling available literature
for single-phase face-centered cubic, body-centered cubic, and multiphase HEAs. These maps could guide
printing of HEAs and provide an insight into the design of novel HEAs for AM.
INTRODUCTION The thermodynamics of phase stability is used to describe

the formation of the solid solution in HEAs [2]. When the
High-entropy alloys
number of alloying elements increases, the contribution of con-
Generally, the properties of metallic materials are improved by figurational entropy exceeds the enthalpic one, and as a result,
adding a low fraction of alloying elements. For instance, the Gibbs free energy is decreased [Eqs. (1) and (2)]. Thus, despite
content of manganese and carbon is altered in steel to change multiple alloying elements, HEAs stabilize to a solid solution
the deformation mechanism and improve mechanical proper- rather than intermetallic compounds [12, 13, 14], as schemati-
ties [1]. Thus, the numerous alloy systems have been explored
▪ Journal of Materials Research ▪ Volume 35 ▪ Issue 15 ▪ Aug 14, 2020 ▪ www.mrs.org/jmr

cally shown in Fig. 1(b).
near the edge of the phase diagram [marked by the blue area in
Fig. 1(a)]. However, using this approach, the compositional DSmix = −R xi lnxi , (1)
space of conventional alloys is searched in a restricted manner
based on the belief that alloy design toward the center region of
DGmix = DHmix − TDSmix , (2)
the phase diagram favors the formation of an intermetallic/
intermediate compound rather than a solid solution. However, where ΔHmix, ΔSmix, and ΔGmix are the enthalpy of mixing,
after it was discovered that adding multiple alloying elements configurational entropy, and Gibbs free energy of mixing. T,
in similar quantities allows for the formation of a single solid R, and xi are the absolute temperature, gas constant, and
solution [2], the opportunity to develop new alloy systems has mole fraction of the ith element, respectively.
been extended. These newly developed alloys that consist of The HEA design concept leads to a vast increase in the
more than five elements with similar atomic fractions are called number of possible combinations to make new alloys.
high-entropy alloys (HEAs) [2, 3, 4, 5, 6, 7, 8, 9, 10, 11]. Instead Furthermore, the research scope of HEAs has expanded from
of the term HEAs, other terminologies are sometimes used to equimolar, single-phase solid solution to non-equimolar, mul-
expand the definition of these alloy systems beyond single- tiphase alloys, expanding the versatility of the microstructure
phase solid solutions or restriction on the configurational and consequently the applications of these alloys [Fig. 1(a)].
entropy, e.g., multi-principal element alloys and composition- In particular, new alloy systems with superior mechanical prop-
ally or complex concentrated alloys [11]. erties have been discovered by deviating from equiatomic HEAs
© Materials Research Society 2020 cambridge.org/JMR 1963

REVIEW
Figure 1: (a) Schematic ternary phase diagram of multicomponent alloy systems, showing the compositional range of conventional alloy ( blue region), non-
equiatomic HEA ( yellow region), and equiatomic HEA ( red dot). The compositional space of HEAs is located in the central area of the phase diagram. (b)
Illustration of the atomic distribution of conventional alloys and HEAs. Conventional alloys tend to form an intermetallic compound in the matrix, and HEAs favor
the formation of solid solution with random atom distribution. All the colored dot indicates different kinds of alloy elements, and the boxed black line shows the
ordered intermetallic/intermediate compounds.
with five elements. For example, CrCoNi [7] exhibits superior resistance, and high density could be overcome in refractory
tensile strength, ductility, and fracture toughness even at cryo- HEAs [35, 36, 37].
genic temperature. Moreover, VCoNi [15] shows exceptional Due to their unique structural characteristics and outstand-
strength and ductility, hinting to the possibility that severe lat- ing mechanical properties, HEAs have gained significant inter-
tice distortion is a crucial factor in improving strength. Another est over the past several years in various fields. Casting has been
approach is to reduce the stacking-fault energy (SFE) in order widely used to fabricate HEAs. However, it involves several
to change the deformation mechanism from slip to TWIP processing steps that require extensive tooling, dies, or casting
(TWinning-Induced Plasticity) to TRIP (TRansformation- molds and leads to a formation of casting defects. On the
Induced Plasticity), showing remarkable strain hardening other hand, a promising fabrication technique, additive manu-
[4, 5, 6, 10, 16]. facturing (AM), provides increased design freedom, including
In general, HEAs having a solely solid solution are classi- the ability to print topology-optimized parts, extending the
fied into three groups in terms of crystal structure: face- capability of HEAs in various industrial fields. As HEAs are rel-
centered cubic (FCC), body-centered cubic (BCC), dual-phase atively complex systems and their applications mostly limited
FCC–BCC HEAs, and composites. The design of FCC HEAs to highly demanding industries, AM may be a suitable candi-
has been strongly focused on the combination of 3d transition date for manufacturing these materials cost effectively and
metals, e.g., CrCoNi [7, 17, 18], CrFeCoNi [19], and with minimal waste.
CrMnFeCoNi [3, 17, 19, 20, 21]. This family of HEAs has a
similar chemical composition and microstructure to austenitic
stainless steel, which provides a guideline for their alloy design. Additive manufacturing

A wide fluctuation of the atomic distances in HEAs, referred to AM is capable of building 3D parts directly from a computer
as the lattice distortion, offers an increased intrinsic strength file by adding material in successive layers [38, 39, 40, 41,
and leads to enhanced solid-solution strengthening [15, 22]. 42]. This bottom-up approach requires less material and does
Thus, alloy elements with a different atomic size such as alumi- not need several conventional processing steps. Furthermore,
num (Al), titanium (Ti), and vanadium (V), are introduced in AM enables a direct construction of materials into the desired
a substitutional solid solution to achieve severe lattice distor- shape, making it easier to optimize the design for enhanced
tion [2, 15, 23, 24, 25, 26, 27, 28, 29, 30]. Specifically, the addi- functionality [38, 39, 40, 41, 42]. There are several methods
tion of Al in FCC HEAs results in a phase transition from FCC for 3D printing metals, including selective laser melting
to dual BCC–B2 phase, and as a result, interconnected struc- (SLM), selective electron beam melting (SEBM), binder jetting,
tures by spinodal decomposition are evolved, providing and directed energy deposition (DED) [43, 44, 45, 46, 47].
increased hardness [2, 29, 31, 32, 33, 34]. BCC HEAs have Among various AM techniques, the two most widely used
been investigated in refractory metal systems to achieve excel- techniques—SLM and powder-flown DED—are discussed in
lent mechanical properties at elevated temperatures due to this paper and schematically shown in Fig. 2.
their high melting temperature. Because the HEA design con- In AM, the process parameters and feedstock control the
cept provides more flexibility of selecting alloy compositions, target variables, such as chemical composition, chemical homo-
common drawbacks in conventional alloys such as high geneity, porosity, and microstructure, as shown in Fig. 3. The pre-
brittle-to-ductile transition temperature, poor oxidation cise control of chemical composition and chemical homogeneity

REVIEW
Figure 2: Schematic diagram of (a) SLM process and (b) powder-flown DED process.
Figure 3: The process parameter

map of the HEA fabricated by AM.
(a and b) Parameters that control
the target variables in (c) that are
indirectly influenced by controllable
variables.
is especially critical when materials with large differences in their layer thicknesses and laser diameter and less need for the sup-
melting and boiling temperatures are used. The chemical compo- port structure. Thus, it is more appropriate to build complex
sition of the printed samples may differ from the nominal com- geometries using SLM rather than DED. However, SLM is lim-
position of the powder blend due to the evaporation of more ited by a slower build rate, which makes it suitable for building
volatile elements. relatively small components [48, 49, 50]. On the other hand,
In SLM, a laser beam is scanned over a thin powder bed, DED builds parts by spraying powders through nozzles and
which selectively melts and fuses powders together. After this melting them on the substrate simultaneously [Fig. 2(b)].
step, the build platform is lowered by the layer thickness. DED provides a lower resolution and higher deposition rate,
Then, powder from the container is transported to the build which offers a higher productivity and is useful in fabricating
platform by a recoating mechanism. This process is repeated larger structures [48, 49, 50]. One important process parameter
until the part is completed [Fig. 2(a)]. SLM offers several in DED is the powder feed rate (Fig. 3), which is strongly tied
advantages over DED such as higher resolution using smaller to the layer thickness of printed layers. Overall, finding the

REVIEW
optimal process parameters for a given alloy is done through an microstructure transition with different processing parameters.
iterative parametric study. Powder properties, such as composi- The volumetric energy density (E) (J/mm3) that integrates most
tion, melting and boiling point, powder morphology, powder processing parameters (Fig. 3) is determined by the following
size, and its distribution, also play a significant role in produc- equation [81]:
ing high-quality parts by AM [51].
P
Despite the versatility of AM, only a few alloy systems can E= . (3)
vht
be reliably printed. Due to a steep temperature gradient (G)
along building direction (BD), columnar grains are generally Processing parameters for AM are varied in each literature,
present after AM [52, 53]. The formation of columnar grains rendering it difficult to understand the effects of processing
is not desirable, as they are susceptible to solidification cracking parameters on microstructures. Thus, microstructures in differ-
and result in anisotropic properties [52, 54, 55, 56]. On the ent HEA systems are mapped out based on the processing
other hand, fine equiaxed grains can accommodate strain easily parameters such as laser power, scanning speed, and energy
and are preferred in AM. However, the formation of equiaxed density. In the following sections, the CET, which shows the
grains requires a large amount of undercooling [52]. This chal- relationship between the size and morphology of grains and
lenge has been resolved in certain cases by employing nano- solidification conditions, will be discussed for SLM and DED
sized particles in the pre-alloyed powders to provide heteroge- to provide a guideline for building HEAs using AM and further
neous nucleation sites [52, 57, 58, 59, 60], by introducing alloy designing HEAs specifically for AM.
elements that facilitate grain nucleation [58, 59], and by intro-
ducing external stimuli such as a pulsed laser and ultrasonic
vibration. Besides alloy design optimization, processing param- MICROSTRUCTURAL EVOLUTION OF AM
eters such as laser power, laser scanning velocity, and scanning PROCESSED HEAs
strategy must be controlled to facilitate the formation of equi- HEAs processed using SLM
axed grains during AM [58, 60, 61, 62, 63]. Thus, a solidifica-
tion map, which shows a columnar-to-equiaxed transition FCC HEAs
(CET), has been widely used to predict the solidification The FCC HEAs, e.g., CrMnFeCoNi [57, 82, 83, 84], CrFeCoNi
mode [58, 64, 65, 66, 67]. The two dominant variables in the [85, 86], and AlxCrFeCoNi (x = 0.3, 0.5) [26, 27, 28], have
solidification map, temperature gradient (G) [68, 69, 70] and been fabricated using SLM. Among different alloying elements,
growth rate of the solid/liquid (S/L) interface (R) [71, 72, 73] Cr, Fe, Co, and Ni show a homogeneous distribution;
can be obtained numerically or experimentally using thermo- however, Mn is usually segregated at the melt-pool boundary
couples, pyrometers or thermal cameras. Among these appara- [82, 87]. In this section, interstitial-free single-phase FCC
tuses, a non-contact infrared camera has been widely utilized to HEAs fabricated by SLM are discussed, and carbon-containing
monitor the temperature in AM for its excellent spatial and HEAs are discussed in the “Carbon-containing HEAs”
temporal resolution. However, it is hard to measure the abso- section.
lute or even relative temperatures due to the difficulty in esti- CrMnFeCoNi HEAs have been built using SLM with differ-

mating some properties, such as emissivity [74, 75, 76, 77]. ent processing parameters such as laser power, scanning speed,
Additionally, materials properties used to numerically evaluate hatch spacing, layer thickness, laser spot size, and scanning
G and R are often temperature-dependent, though this strategy (Figs. 4 and 6; Table 1). When CrMnFeCoNi HEAs
temperature-dependence is commonly ignored for simplicity. are manufactured with laser power (P) of 400 W and different
Therefore, these methods have limitations to monitor the tem- scanning speeds (v) from 800 to 4000 mm/s, porosity is nearly
perature during AM, which makes the construction of the sol- unchanged up to 2000 mm/s but abruptly increases with any
idification maps inaccurate. What is more, additive further increase in the scanning speed [82]. Here, the hatch
manufactured materials experience complex thermal cycles spacing, h, and layer thickness, t, are held constant at 90 and
[41, 78, 79, 80] that involve broad temperature ranges and 30 μm, respectively. As a result, energy density (E) is varied
fast cooling rates, which makes it even more challenging to from 37 to 186 J/mm3. The highest relative density is 98.2%,
measure the solidification parameters [58, 74, 76]. Thus, and the mixed columnar and equiaxed grains are formed
instead of G and R, laser processing parameters, which are along the BD when the alloy is fabricated with P = 400 W, v
more straightforward and controllable, are used to discuss = 2000 mm/s, and E = 74 J/mm3. With increasing laser energy
CET in this paper. density, FCC is still sustained with a small amount of tetrago-
To do so, the important processing parameters for AM, nal σ phase [82]. When the laser is run at P = 250 W, v =
e.g., the laser power (P), scanning speed (v), hatching distance 450 mm/s, and E = 165 J/mm3 to deposit CrMnFeCoNi HEA,
(h), and layer thickness (t), are considered in understanding the a large columnar grain structure is formed, and the FCC

REVIEW
Figure 4: The effect of the crystal structure and the processing parameters on the microstructure of SLMed HEAs. (a) SEM image and (b) IPF map of CrMnFeCoNi
HEA built by SLM with high energy density. (c) SEM image and (d) IPF map of CrMnFeCoNi HEA built by SLM with low energy density. (e) SEM image and (f) IPF
map of AlCrFeCoNi HEA fabricated by SLM with high energy density. All the images are obtained parallel to BD.
structure is sustained, as shown in Figs. 4(a) and 4(b) [57]. with P = 400 W, v = 1600 mm/s, and E = 69 J/mm3, and the
When CrMnFeCoNi HEA is built with similar power and equiaxed grains between the columnar grains are obtained
higher scan speed (P = 240 W, v = 2000 mm/s, and E = 60 J/ with the FCC structure [27].
mm3), the relative density is 99.2%, and mixed columnar and
equiaxed grains appear [Figs. 4(c) and 4(d)] [83, 84].
However, interestingly, the aspect ratio of grains is clearly HEAs with mixed FCC and BCC phases
reduced, suggesting that the columnar grains are starting to The combination of Al and transition metals leads to the phase
transform into equiaxed grains [84]. From these microstruc- transformation from FCC to BCC. In as-cast AlxCrFeCoNi

tural changes, it is elucidated that CET is suppressed for the HEA, FCC and BCC structures coexist at the Al content
alloys built at a lower scanning speed. CrFeCoNi HEAs are from 0.5 to 0.8 mole fraction [29]. Moreover, when the Cu ele-
manufactured with P = 150 W, v = 270 mm/s, and E = 111 J/ ment, which is chemically partitioned from other elements
mm3, resulting in 98.7% relative density. Two different scan- such as Cr, Fe, Co, and Ni, is added, the Cu-rich phase and
ning strategies, chessboard and bidirectional stripe patterns, mixed FCC and BCC structures are obtained at a relatively
are used for printing [86]. Both cases generate large columnar high content of Al in the as-cast AlxCrFeCoNiCu HEA [2].
grains, but the chessboard scan forms submicron-sized grains AlCrFeNiCu HEAs have no segregation at the macroscale.
between the large columnar grains, suggesting that this scan They consist of nanoscale alternating sinuous ribbon-shaped
strategy facilitates more grain nucleation. Besides, the chess- BCC and B2 phases and Cu-rich precipitates, showing different
board scanning method utilized to reduce residual stress results precipitate morphology at high-angle and low-angle grain
in numerous aligned cracks and pores, whereas the bidirec- boundaries [89].
tional stripe scanning pattern causes a more random distribu- AlCrFeNiCu HEAs [89] are fabricated with laser power (P)
tion of cracks and pores. of 300 W, scanning speed (v) ranging from 400 to 1200 mm/s,
When Al0.3CrFeCoNi HEA is laser-melted at P = 160 W, v hatch spacing (h) from 60 to 120 μm, and corresponding
= 1100 mm/s, and E = 129 J/mm3, columnar grains are formed, energy densities (E) ranging from 234 to 78 J/mm3. The
and the FCC structure is still sustained during SLM [26]. With printed structure has fine columnar grains with extremely
more Al addition in the alloy, Al0.5CrFeCoNi HEA is fabricated small subgrains composed of BCC, B2, and nanoscale

REVIEW
TABLE 1: Composition, crystal structure, processing parameters, and microstructure for SLMed HEAs.
Laser Scanning Hatching Layer Energy

power speed distance thickness density

Composition Crystal structure (W) (mm/s) (μm) (μm) (J/mm3) Microstructure Reference
CrMnFeCoNi FCC + tetragonal σ 400 800 90 30 186 – [82]

400 1200 90 30 123 – [82]
400 1600 90 30 93 – [82]
400 2000 90 30 74 Mixed [82]
400 2500 90 30 59 – [82]
400 300 90 30 49 Mixed [82]
400 4000 90 30 37 – [82]
FCC 250 450 75 45 165 Columnar [57]
240 2000 50 40 60 Mixed [83]
240 2000 50 40 60 Mixed [84]
240 2500 50 40 48 Mixed [84]
CrFeCoNi FCC 150 270 100 50 111 Columnar [86]
150 270 100 50 111 Columnar [86]
200 300 – 20 – – [85]
200 300 – 50 – – [85]
Al0.3CrFeCoNi FCC 160 1100 45 25 129 Columnar [88]
Al0.5CrFeCoNi FCC 400 1600 90 40 69 Mixed [27]
AlCrFeNiCu BCC + B2 + Cu-rich 300 600 60 40 208 – [89]
precipitates 300 600 80 40 156 Columnar [89]
300 600 100 40 125 – [89]
300 600 120 40 104 – [89]
300 400 80 40 234 – [89]
300 800 80 40 117 – [89]
300 1000 80 40 94 – [89]
300 1200 80 40 78 – [89]
AlCrFeCoNi BCC + B2 250 1000 90 40 69 Mixed [28]
300 1000 90 40 83 Mixed [28]
350 1000 90 40 97 Mixed [28]
400 1000 90 40 111 Mixed [28]
98 2000 52 20 47 Equiaxed [90]
NbMoTaW BCC 400 250 100 100 160 – [91, 92]
CrFeCoNiC0.05 FCC + M23C6 200 800 110 50 46 – [93]
250 800 110 50 57 Mixed [93]
300 800 110 50 68 Equiaxed [93]
350 800 110 50 80 Equiaxed [93]
400 800 110 50 91 Equiaxed [93, 94]
400 1000 110 50 72 Equiaxed [93]
400 1200 110 50 61 Equiaxed [93]
(CrMnFeCoNi)99C1 FCC + Mn-rich oxide and 90 200 80 25 225 Columnar [95]
sulfide, Cr-rich carbide 90 600 80 25 75 Mixed [95]

Fe49.5Mn30Co10Cr10C0.5 FCC 180 1000 55 40 150 Mixed [87]
CrFeCo1.5Ni1.5Ti0.5Mo0.1 FCC + TiCo2, MoFe2 160 650 100 40 62 Mixed [96]
Al0.5Cr0.9FeNi2.5V0.2 FCC + L12 140 900 50 30 104 Mixed [97]
Cu-rich precipitates [89]. Figures 4(e) and 4(f) show the microstructure and Cr–Fe-enriched precipitates with a disordered
structures of the SLMed AlCrFeNiCu HEA built with P = BCC phase [32]. Similarly to induction-melted AlCrFeCoNi
300 W, v = 600 mm/s, and E = 156 J/mm3. AlCrFeCoNiCu HEAs, SLMed HEAs show nanoscale phase separation but
HEA shows columnar grains [89]. Nevertheless, compared with less fluctuation of Cr element due to faster cooling during
with CrMnFeCoNi HEA [57] manufactured with P = 250 W, AM [90]. Moreover, the precipitation of a nano-sized Cr–Fe
v = 450 mm/s, and E = 165 J/mm3, the aspect ratio of grains is phase could be facilitated due to the fine grain structures of
prominently decreased. This shows that the formation of colum- additive manufactured materials, as the increasing number of
nar grains can be suppressed depending on the alloy systems. grain boundaries enhances the overall diffusion [28].
AlCrFeCoNi HEA is laser-melted at different laser powers
P = 250–400 W, v = 1000 mm/s, and energy density (E) from
BCC HEAs 69 to 111 J/mm3, showing a maximum relative density of 98.4%
The combination of transition metals and Al. AlCrFeCoNi HEA at P = 400 W and E = 111 J/mm3. In SLMed AlCrFeCoNi HEA,
consists of the Al–Ni-enriched matrix with an ordered B2 BCC and B2 phases are obtained, and the grain size is increased

REVIEW
with increasing volumetric energy density due to the decrease when lower laser power is used, the aspect ratio of grains
in the cooling rate, sustaining the mixed columnar and equi- increases. Furthermore, the grain size is increased by decreasing
axed grains [28]. the scanning speed and increasing the laser power [93]. These
Refractory HEAs. Refractory alloys are emerging materials results describe that the transition from columnar to equiaxed
for applications under extreme conditions due to their high grain and the grain size can be manipulated by optimizing the
melting points [98]. However, the intrinsic properties of refrac- processing parameters.
tory alloys, e.g., their high melting point, susceptibility to oxi- (CrMnFeCoNi)99C1 HEA is fabricated at P = 90 W and v =
dation, and their high ductile-to-brittle transition temperature, 200 and 600 mm/s [95]. As a result, (CrMnFeCoNi)99C1 HEA
lead to the formation of cracks and pores during AM [35, 99, 100, built with P = 90 W, v = 200 mm/s, and E = 225 J/mm3 has a
101]. Thus, the AM of refractory HEAs have not been widely prominent large columnar grain structure, while the mixed
investigated, and there are very few studies about SLMed refrac- columnar and equiaxed grain structures are evolved in
tory HEA. (CrMnFeCoNi)99C1 HEA [95] manufactured with P = 90 W,
NbMoTaW HEA built with P = 400 W, v = 250 mm/s, E = v = 600 mm/s, and E = 75 J/mm3.
160 J/mm3, and laser diameter of 500 μm [91, 92] shows severe Fe49.5Mn30Co10Cr10C0.5 HEA is laser-melted at P = 180 W,
warping. Thus, processing parameters, e.g., power, scan speed, v = 1000 mm/s, and E = 150 J/mm3 and consists of the FCC
and the number of layers, are optimized by minimizing the structure without carbides [87]. It shows a hierarchical micro-
temperature gradient and thermal stress and strain via simula- structure that comprises equiaxed grains and columnar
tion of the SLM process. When NbMoTaW HEA is laser- structure.
melted with the optimized process parameters, warping and HEAs with ceramic/intermetallic compound. In this section,
cracks are suppressed but no information on the microstructure pre-alloyed and pre-mixed HEAs consisting of solid solution
is provided [91]. and ceramic/intermetallic compounds are reviewed. CrFeCo1.5
Ni1.5Ti0.5Mo0.1 HEA is manufactured with P = 160 W, v =
650 mm/s, and E = 62 J/mm3, and an FCC matrix with a
HEA composites small amount of TiCo2 or MoFe2 intermetallic compounds is
Carbon-containing HEAs. When a small number of interstitials, observed [96]. In addition, the mixed columnar and equiaxed
e.g., carbon and nitrogen, is introduced in certain alloys, the grains appear in SLMed CrFeCo1.5Ni1.5Ti0.5Mo0.1 HEA. Al0.5
deformation mode can be changed, leading to improved Cr0.9FeNi2.5V0.2 HEA printed with P = 140 W, v = 900 mm/s,
mechanical properties. Among additive manufactured carbon- E = 104 J/mm3 shows a single-phase FCC structure with a
containing HEAs, no carbide is observed in Fe49.5Mn30Co10 nano-sized L12 phase, and the mixed columnar and equiaxed
Cr10C0.5 HEA, providing interstitial solute strengthening [87]. grains are formed [97].
However, CrFeCoNiC0.05 and (CrMnFeCoNi)99C1 HEAs con- These pre-alloyed CrFeCo1.5Ni1.5Ti0.5Mo0.1 and Al0.5Cr0.9
tain carbides in the FCC matrix, which gives additional FeNi2.5V0.2 HEAs exhibit the mixed columnar and equiaxed
strengthening [94, 95]. grains. By laser-melting pre-mixed ceramic particles with
CrFeCoNiC0.05 HEAs [93] are built with laser powers (P) HEA powders, a transition to more equiaxed grains can be pro-

varying between 200 and 400 W, scanning speed (v) changing moted. For example, CrMnFeCoNi pre-alloyed powder is
from 400 to 3000 mm/s, and energy density (E) ranging from mixed with 12 wt% TiN particles [57] and laser-melted with
57 to 91 J/mm3. The relative density of CrFeCoNiC0.05 HEA P = 250 W, v = 450 mm/s, and E = 165 J/mm3. As a result, the
is 99.2% at P = 250 W, v = 800 mm/s, and E = 57 J/mm3. grain size is dramatically decreased, and the transition from
CrFeCoNiC0.05 HEA has the FCC structure with no carbide columnar to equiaxed grains occurs, suggesting that the addi-
phase at the microscale [93]. However, it has been shown tion of TiN particles provides heterogeneous nucleation sites.
that nano-sized M23C6 carbides are precipitated at grain
boundaries and dislocation networks in the CrFeCoNiC0.05
HEA [94] manufactured with P = 400 W, v = 800 mm/s, and
CET depending on processing parameters in
E = 91 J/mm3. Additionally, equiaxed grains are formed when
SLMed HEAs
the laser is run with P = 300 and 400 W and v = 800 mm/s, CET is universally utilized to achieve equiaxed grains in addi-
with the corresponding energy density (E) of 68 and 91 J/ tive manufactured materials. However, temperature gradient
mm3, respectively. However, by increasing the laser power, (G) and solidification velocity of the solid/liquid interface (R)
i.e., increasing the energy density, CrFeCoNiC0.05 HEAs fabri- cannot be easily acquired from experiments due to the inaccu-
cated with both P = 400 W, v = 800 mm/s, E = 91 J/mm3 show racy in temperature measurements. Thus, we want to exploit a
a smaller aspect ratio compared with the alloy built with P = more straightforward way using processing parameters of AM
250 W, v = 800 mm/s, and E = 57 J/mm3, suggesting that instead of G and R to construct a solidification map.

REVIEW
The temperature gradient (G) and solidification front

velocity (R) can be approximated using an analytical approach dT 2a
= 1 +
known as the Rosenthal equation. The Rosenthal equation con- dz V j2 + z 2

siders process parameters (P and v) as well as materials prop-
lP V z V
erties, such as absorptivity, thermal diffusion, density, × − exp − j + j2 + z 2 ,
2pk 2a j2 + z 2 2a
thermal conductivity, specific heat, and melting temperature, (8)
to predict the thermal characteristics in laser melting. This ana-
lytical method [73] calculates the values for G and R for various

locations within the melt pool. The Rosenthal equation is given dT j 2aj
= 1 + +
j2 + z 2 V(j + z 2 )
2
as follows: dt

lP V 2 1 V
× exp − j + j2 + z 2 .
lP V(r + j) 2pk 2a j2 + z 2 2a
T = T0 + exp − , (4)
2pkr 2a (9)
where T0 is the temperature at a location far from the top sur- The approach has been shown to be a reasonable approxi-
face, k is the thermal conductivity, V is the scanning velocity, λ mation when verified with FE calculations and experimentation
is the absorptivity, and α is the thermal diffusivity. Since the despite the following assumptions [73]: (i) Materials properties
laser is considered to move along the x-axis, where the laser such as thermal conductivity, density, and specific heat are
motion is captured by ξ = x − Vt. Finally, r is the distance independent of temperature change; (ii) Process parameters
between the melt pool and the heat source and is given by (P and v) are held constant during the melt, which results in

j2 + y 2 + z 2 . a quasi-stationary temperature distribution in the melt pool;
The process of estimating G and R starts with estimating and (iii) Thermal convection and radiation are negligible, leav-
the width of the melt pool using the following equation: ing conduction as the only mode of heat transfer considered.
The Rosenthal approach is used to generate R versus v and G

8 lP versus E maps shown in Figs. 5(a) and 5(b) to demonstrate
W≈ , (5) the validity of using v and E as an alternate way of constructing
pe rCP V(Tm − T0 )
solidification map for additive manufactured parts. All values
for materials properties used in the Rosenthal method are pre-
where W is the melt pool width, ρ is the density, P is the laser
sented in Table 2.
power, V is the scanning velocity, and CP is the specific heat.
To demonstrate the effect of process parameters in the esti-
The values for ξ are varied from −W/2 to W/2 to span the
mation of G and R values, P and v are varied between 0 and
entire melt pool. Since the solidification is dictated by the
500 W and 0 and 2400 m/s, respectively. Additionally, the
last remelt that the material experiences, z values are varied
layer thickness and the hatch distance are held constant at t
between 0 and the layer thickness (the interval at which remelt-
= 40 μm and h = 100 μm, respectively. The plotted values are

ing occurs for each layer). To consider the center of the melt
for ξ = 0 μm and z = 20 μm to show the values for the middle
pool, y is held constant at 0.
of the melt pool.
Finally, G and R is defined by the following equation:
R is plotted against v in Fig. 5(a), showing a linear correla-
tion between the two variables (values shown for the
1 dT 1 dT
R=
= 2 2 dt . (6) CoMnFeCrNi HEA system). Figure 5(b) shows the relationship
G dt dT dT
+ between G and E for various values of laser power and scan
dj dz speeds. Here, G increases as E decreases; this is due to the
smaller area of the combined melt-pool and heat-affected
Where the local cooling rates are found by the following zone [60, 108, 109]. The values for G as a function of energy
equations: density, obtained for common commercial alloys such as stain-
less steel (SS304 and SS316), nickel-based superalloys (Inconel

dT j 2aj 625 and 718), and titanium alloy (Ti–6Al–4V) are plotted
= 1 + + along with the CoMnFeCrNi values for comparison in Fig. 5
j2 + z 2 V(j + z 2 )
2
dj

(c). When the material properties of the alloys are taken into
lP V 1 V account, the trend is similar for HEA and other commercial
× − exp − j + j2 + z 2 ,
2pk 2a j2 + z2 2a alloys. However, at increasing energy density, values for G
(7) diverge for each material by a few orders of magnitude, as

REVIEW
Figure 5: Plot of (a) R versus scan speed and (b) G versus energy density for the CoMnFeCrNi HEA system at various values for laser power and laser scan speed. (c)
G versus energy density for HEA, Inconel 625, Inconel 718, Ti–6Al–4V, SS 304, and SS 316 at P ≈ 100 W. (d) The corresponding CET schematic using E and v.
can be seen for Ti–6Al–4V and stainless steels at E ≈ 100 J/ parameters. Translating G and R into E and v, an alternative
mm3. These values are particularly sensitive to the thermal method of correlating process parameters to the resulting
conductivity of each material. These changes in G–E correla- microstructure is presented in Fig. 5(d), with increasing v on
tion for different materials should be considered in the context the x-axis and descending E on the y-axis. The G/R (defining
of solidification maps for each material. For example, the differ- the morphology of solidified microstructure) and G * R (defin-
ence between the maximum and minimum of temperature gra- ing the size of solidified microstructure) are derived as a func-

dient showing the mixed columnar and equiaxed grains is tion of E and V using Eqs. (6)–(9) to guide us in building the
1.4 × 106 K/m at the solidification velocity of 0.08 m/s in Ti– schematic map.
6Al–4V [58]. In contrast, this value for Inconel is 8.4 × Figure 6 shows the relationship between grain morphology
104 K/m at 0.08 m/s, which is over an order of magnitude and processing parameters, i.e., laser scanning speed and
lower. This suggests that the difference in temperature gradient energy density, in the individual HEA systems reviewed so
among different materials can affect the microstructural evolu- far. The inverted vertical axis for energy density (E) is used
tion even if these materials are fabricated with similar process to show a similar trend with the solidification map in Fig. 5
TABLE 2: Materials properties for CrMnFeCoNi HEA, Ti–6Al–4V, Inconel 625, Inconel 718, Stainless Steel (SS) 316L, and SS304.
Material Density (kg/m3) Specific heat (J/kg K) Thermal conductivity (W/m K) Absorptivity Diffusivity (m2/s) Melting point (K) Reference
−6
CrMnFeCoNi 7753 483.6 11.6 0.67 3.10 × 10 1550 [102]
Ti–6Al–4V 4430 526.3 6.7 0.7 2.87 × 10−6 1877 [103]
Inconel 625 8440 410 9.8 0.57 2.83 × 10−6 1563 [104]
Inconel 718 8220 435 11.4 0.5 3.19 × 10−6 1643 [105]
SS 316L 8000 500 16.3 0.67 4.08 × 10−6 1643 [106]
SS 304 8000 500 16.2 0.67 4.05 × 10−6 1673 [107]

REVIEW
when AlCrFeCoNi HEA [28] is built with increasing laser power

(P) and a fixed scan speed and therefore a decreasing cooling
rate, the grain size is increased. Additionally, CrFeCoNiC0.05

HEAs [94] manufactured with P = 400 W, v = 800 mm/s, E =
91 J/mm3 show an increase in grain size compared with
CrFeCoNiC0.05 HEAs [94] manufactured with P = 400 W, v =
1200 mm/s, E = 61 J/mm3. Therefore, when the volumetric
energy density is decreased while scanning speed is increased,
i.e., an increase in the cooling rate, the grain size is decreased.
All processing parameters should be considered to understand
CET because the complicated AM process affects the transition
of grain morphology in various ways.
Secondly, the contribution of crystal structures to the
microstructure in additive manufactured HEAs is studied. It
is found that, with similar laser processing conditions, additive
Figure 6: The solidification map presented by the scanning speed and energy manufactured HEAs with a single-phase FCC structure are
density, showing the effect of processing parameters on the CET. Filled sym-
bols indicate the columnar grain, partially filled symbols mean the mixed struc-
more susceptible to forming columnar grains. The laser-melted
tures consisting of the columnar and equiaxed grains, and open symbols FCC single-phase CrMnFeCoNi HEA [57] with P = 250 W, v =
describe the equiaxed grains. Sphere indicates the formation of the single 450 mm/s, and E = 165 J/mm3 tends to form a large columnar
FCC phase. Square describes the combination of FCC and BCC phases, and pen-
tagon represents the coexistence of A2 and B2 phases. Triangle and inverted grain structure [Figs. 4(c) and 4(d)]. AlCrFeNiCu HEA built
triangle mean carbon-containing alloys and the composite with ceramic/inter- with P = 300 W, v = 600 mm/s, and E = 156 J/mm3 shows
metallic compounds.
BCC, B2, and nano-sized Cu-rich phases. Additionally, it
exhibits columnar grains but with a lower aspect ratio and
(d). In Fig. 6, filled, half-filled, and open circles indicate colum- smaller grain size even with similar laser processing conditions
nar, mixed columnar and equiaxed, and the equiaxed grain [89]. Furthermore, CrMnFeCoNi HEA [82] fabricated with P =
morphology. Moreover, the symbol shape indicates the crystal 400 W, v = 1200 mm/s, and E = 123 J/mm3 and Al0.3CrFeCoNi
structure of the SLMed HEAs. Specifically, the sphere, square, single-phase HEA [88] manufactured with P = 160 W, v =
and pentagon describe the single FCC phase, dual FCC–BCC 1100 mm/s, and E = 160 J/mm3 consist of the columnar grains,
phases, and coexistence of BCC and B2 phases. In addition, but AlCrFeCoNi HEA (with mixed FCC and BCC phases) [28]
the triangle and inverted triangle represent carbon-containing built with P = 400 W, v = 1000 mm/s, and E = 111 J/mm3 has
HEAs, regardless of the formation of carbide or ceramic/inter- the mixed columnar and equiaxed grains. It suggests that
metallic compounds. CET is more suppressed in single-phase HEAs, i.e.,
First, the effect of solidification velocity (R) and tempera- CrMnFeCoNi and Al0.3CrFeCoNi HEA, with respect to multi-
ture gradient (G) on CET is investigated. CrMnFeCoNi HEA phase HEAs built with similar process parameters.

[83] built with P = 240 W, v = 2000 mm/s, and E = 60 J/mm3 Thirdly, the effect of the addition of carbon on grain mor-
shows the mixed columnar and equiaxed grains; however, phology in additive manufactured HEAs is discussed. In
CrMnFeCoNi HEA [57] fabricated with P = 250 W, v = (CrMnFeCoNi)99C1 HEA [95] fabricated with P = 90 W, the
450 mm/s, and E = 165 J/mm3 shows the large columnar grains. columnar grains start to transform into equiaxed grains with
For carbon-containing HEAs, (CrMnFeCoNi)99C1 HEAs [95] increasing scanning speed (v) from 200 to 600 mm/s and
built with P = 90 W, v = 200 mm/s, and E = 225 J/mm3 display decreasing energy density (E) from 225 to 75 J/mm3.
the columnar grains. However, (CrMnFeCoNi)99C1 HEAs [95] However, CrMnFeCoNi HEA [57] built with P = 250 W, v =
laser-melted with P = 90 W, v = 600 mm/s, and E = 75 J/mm3 450 mm/s, and E = 165 J/mm3 shows the prominent columnar
exhibit the mixed columnar and equiaxed grains. As a result, grains even though the laser processing parameters of the
it can be interpreted that the transition into equiaxed grains CrMnFeCoNi HEAs fall between those of the
results from the increase in scanning speed. Besides, the equi- (CrMnFeCoNi)99C1 HEA [95]. This result suggests that adding
axed grains in CrFeCoNiC0.05 HEA [93] change to the mixed interstitials can promote the formation of equiaxed grains due
columnar and equiaxed grains with a decrease in energy density to the introduction of additional heterogeneous sites. Similarly,
from 91 to 57 J/mm3. These results suggest that an increase in G, the addition of heterogeneous nucleation sites (e.g., addition of
attributed to the reduction in energy density, can facilitate the ceramic phase TiN in the CrMnFeCoNi FCC matrix [57]) pro-
formation of columnar grains. Furthermore, the cooling rate motes the formation of equiaxed grains. Even though
(the product of G and R) influences the grain size. For example, CrMnFeCoNi HEA laser-melted at P = 250 W and E = 165 J/

REVIEW
mm3 shows the columnar grains, these HEAs exhibit fine equi- and 120 J/mm3 [110, 111, 112]. The DEDed CrMnFeCoNi
axed grains with a prominently decreased grain size when HEAs have the columnar grains, sustaining the FCC structure.
added with the ceramic compound, TiN. In this section, the However, the grain sizes decrease from 30–150 μm [111] to
effect of the processing parameters on the microstructural evo- 2.9–5.2 μm [112] when the velocity increases from 2 to
lution in the SLMed HEAs is studied, and the optimized pro- 13.3 mm/s, respectively. Compared to the columnar micro-
cessing parameters are discussed in order to achieve fine structure of SLMed CrMnFeCoNi HEA [84], the width of the
equiaxed grains. dendrites in DEDed samples are an order of magnitude larger,
Although SLMed HEAs have been widely investigated, which can be explained by the lower cooling rate during the
SLM is not an appropriate process to develop new HEAs. In DED process [110, 112]. CrMnFeCoNi HEA samples processed
contrast, powder-flown DED uses several hoppers that enable at varying laser powers (600, 800, and 1000 W) at a fixed scan-
different powders to be sprayed onto the substrate and melted ning speed of 13.3 mm/s show a decrease in both pore size and
by a laser beam, which allows for the building of chemically porosity with increasing laser power [21]. However, with
gradient materials by adjusting the flow rate of individual pow- increasing laser power, the columnar grain coarsening is signif-
ders. This advantage of DED provides the opportunity to icant due to the decrease in the cooling rate.
explore the vast compositional space of HEAs. In the next sec-
tion, we explore the microstructures and mechanical properties HEAs with mixed FCC and BCC phases
of DEDed HEAs. Similarly to SLMed parts described in Section “HEAs with
mixed FCC and BCC phases,” the phase transformation from
HEAs processed using DED FCC to BCC as a result of the addition of Al in transition
metal alloys has also been studied using DED, namely
FCC HEAs AlxCrFeCoNi (x = 0.4, 0.7, and 1.0) [114] and AlxCrFeCo
The FCC CrMnFeCoNi [21, 84, 110, 111, 112] HEAs have been Ni2Cu (0 < x < 1.5) [115] HEA systems. In the AlxCrFeCoNi
most widely fabricated and studied using DED. Chemical seg- HEA system printed with P = 600–650 W, v = 5 mm/s, and
regation of Mn and Ni into the interdendritic region is E = 130–162 J/mm3, the columnar grains appear [114]. In
observed in the DEDed CrMnFeCoNi sample because Mn AlxCrFeCoNi2Cu HEA fabricated by DED, the mixed FCC
and Ni have lower melting points [21, 110, 112, 113]. and BCC structures appear for Al mole fraction from 0.8 to
However, a heat treatment at 1373 K results in a homogeneous 1.5, where the mixed columnar and equiaxed grain morphol-
distribution of Cr, Mn, Fe, Co, and Ni elements without any ogy is achieved [115]. Furthermore, Ti is added to the
segregation or clustering, which indicates a single-phase solid AlCrFeCoNiCu HEA system to investigate whether it stabilizes
solution of the HEA [21]. the ordered Huesler phase (L21) in a B2-forming HEA [116].
Figure 7 shows three instances of the CrMnFeCoNi HEAs Among the BCC phases, the L21 phase has a greater creep resis-
printed with comparable energy densities (E) of between 110 tance compared to B2 for its limited-slip systems and is a
Figure 7: The effect of the crystal structure and the processing parameters of AM on the microstructures in DEDed HEAs at similar energy densities and increasing
scanning velocities. (a–c) IPF map of CrMnFeCoNi HEAs built by DED. The scanning velocities increases from 2 mm/s in (a) to 13.3 mm/s in (c).

REVIEW
favorable phase to obtain ductility over a broad range of tem- in Zr-rich phases rather than the change in the cooling rate as a
peratures [117]. The resulting microstructure has finer grains function of the distance from the substrate. This was demon-
and intragranular features due to the faster cooling rates com- strated by producing a specimen with reversed chemical gradi-
pared to the arc-melted samples, and mixed columnar grains ent, where the change in grain size along the sample was
are observed in the DEDed sample [116]. reversed, thus showing the correlation between chemical com-
position and grain size.
TiZrNbMoV HEA has been fabricated using various pro-
BCC HEAs cess parameters to observe their effects on the chemical compo-
The combination of transition metals and Al. The AlxCoFeCoNi sition of the resulting alloy [120]. Of the three process
[118] HEA system has been printed with DED, and the result- parameters tested (P = 300 W, P = 1000 W, and remelting
ing microstructure follows a simple trend, where only solid- three times at P = 1000 W), the HEA processed at the low
solution structures change from FCC to FCC and BCC and laser power of 300 W shows the greatest variation from the
finally to BCC with increasing Al content (x > 0.7). Similarly, nominal chemical composition of the pre-mixed powder and
AlxCrFeCoNiCu [33] and AlxCrFeNi2Cu [115] systems pro- contain unmelted Mo and Nb powders. The HEAs built at
mote the formation of FCC and L12 to BCC and B2, and the higher laser power also show a loss of Mo and an excess of
grain morphology changes from columnar to equiaxed as Nb. The low laser power fabrication results in a two-phase den-
more Al is added. Adding Cu to the above-mentioned HEA dritic matrix with a BCC solid solution and an orthorhombic
systems (AlxCrFeCoNi and AlxCrFeNi2) brings in positive mix- NbTi4-type phase and α-Zr-rich precipitates. The alloys pro-
ing enthalpy with the other elements, which causes the liquid cessed at a higher laser power achieve a predominant BCC
phase separation. When the Al content is increased even phase with no dendritic segregation [120], as higher cooling
more, a mixture of BCC and B2 forms [116, 119]. rates restrict the diffusion and prevent multiple phase transfor-
AlCrFeCoNi HEAs fabricated by DED show nano-phase sepa- mation and the formation of undesired intermetallic phases
ration especially at high Al contents but show more chemical during cooling [121, 122, 123].
homogeneity in each phase [97]. NbMoTaW HEA was also produced using a pulsed multi-
Refractory HEAs. Compositionally graded TiZrNbTa step process with P = 800 W and v = 2.5 mm/s to prevent the
refractory HEAs have been fabricated using DED by varying evaporation of Nb and remelting three times at a higher laser
the Nb and Zr content from Ti25(Zr50Nb0)Ta25 to power of P = 4500 W and v = 8.3 mm/s to achieve a homoge-
Ti25(Zr0Nb50)Ta25 [51]. Unlike other HEAs where the com- neous melt [99]. The powder morphology used in the pre-
prising elements have comparable melting temperatures, pre- mixed powder is different for all elements, where only the
mixed refractory powders require a multistep deposition pro- Mo powder has a spherical shape. Although a clean weld
cess because of the vast difference in the melting points of seam is achieved using irregularly sized shapes, it is suggested
the elemental powders, e.g., between Ti and Ta [51]. A pulsed that spherical shapes for all elemental powders would help
laser that is required to properly melt the Ta powder particles ensure a smoother melt track. The focus is to evaluate the
causes other elements, especially Ti, to evaporate significantly. chemical composition of the sample using a pre-mixed alloy

Thus, a low pulse power Pinitial = 500 W at a pulse length of and the quality of the weld seam, and thus, the microstructure
1 ms and a pulse frequency of 300 Hz is followed by a higher is not reported.
laser pulse power Premelt = 2500 W at a pulse length of 0.8 ms
and a pulse frequency of 120 Hz to remelt the partially melted
and nonhomogeneous initial melt. These TiZrNbTa HEAs are DED for combinatorial alloy design
found to be single-phase BCC solid solutions for all tested Due to the extensive composition range of HEAs, time-
compositions [51]. At the microscale, the dual FCC–BCC consuming and labor-intensive studies are needed to develop
phases tend to be formed at high Zr content in the chemically novel HEAs. Thus, the experimental combinatorial methods,
gradient TiZrNTa HEAs. On the other hand, the formation of a e.g., multiple diffusion, combinatorial laser AM, and synthesis
single BCC phase is favored at low Zr content. The grain struc- of multinary thin-film materials, have been proposed to
ture changes from fine, equiaxed grains to larger columnar develop novel materials efficiently [123]. However, the combi-
grains as the Nb content increases and Zr content decreases. natorial multiple diffusion [123, 124] that is fabricated via suc-
Moreover, the average grain size of the BCC matrix increases cessive processing, e.g., casting and hot-isostatic pressing,
from 2 μm for Ti25Zr50Nb0Ta25 near the substrate to 60 μm involves long-term annealing. Furthermore, thin-film deposi-
for Ti25Zr0Nb50Ta25 at the end of the wall structure. This tion cannot be used to investigate bulk properties, as bulk prop-
increase in grain size with the increasing distance from the sub- erties depend on the aggregate of microstructures, which is
strate is found to be affected by the chemical segregation of Ta normally beyond the film thickness [123, 125]. DED offers

REVIEW
not only higher productivity but versatility for alloy develop-

ment. In Section “Additive manufacturing,” the processing
parameters, advantages, and disadvantages of DED are dis-

cussed. Instead of the use of pre-alloyed powders, DED can
offer reasonable cost and a large flexibility in chemical compo-
sition by using the pre-mixed elemental powders and in situ
alloying. Therefore, DED may be a more appropriate technol-
ogy to discover the broad compositional and microstructural
spaces [112]. In particular, compositionally graded samples
facilitate the investigation of different properties such as hard-
ness as a function of the chemical composition. Some work has
been done using the compositionally graded AlxCrFeNi2Cu
HEA system, in which an increase in the microhardness is
demonstrated with increasing Al content [115]. In general,
an increase in Al content facilitates spinodal decomposition Figure 8: The solidification map presented by energy density and scanning
speed, showing the effect of processing parameters on the CET. Filled symbols
and increases the strength of the specimen due to the nanoscale
indicate columnar grains, and open symbols show the equiaxed grains.
alternating phases and the formation of BCC phase, although
at the expense of ductility [118]. The hardness of the
TiZrNbTa refractory HEAs has also been studied, where the R (proportional to scanning velocity) remains constant while G
hardness value increases with increasing Zr concentration decreases (an increase in laser power and thus increase in E), as
[51]. At lower than 25 at.% of the Zr element, the region shown in Fig. 5(d). The dendrite columnar grains show an epi-
shows a single BCC phase, and the hardness increase results taxial growth in the build direction. In the same CrMnFeCoNi
from the enhanced solid-solution strengthening by Zr atoms. HEA system, the columnar grains at similar energy densities (at
At further increasing Zr content, the increase in hardness is around E = 120 J/mm3) have a decreasing average grain size
attributed to the increase in the volume fraction of Ta-rich pre- with increasing scanning velocity (30–150 μm at v = 2 mm/s
cipitates. This allows for an effective way of correlating compo- [111] to 2.9–5.2 μm at v = 13.3 mm/s [112]). This demonstrates
sition with hardness. Gradient materials have also been used to that grain refinement occurs as the scanning velocity increases.
probe other mechanical properties through techniques such as Due to the limited information on processing parameters in
micro-compression tests, which have successfully provided DED studies, it is challenging to come to a definitive conclu-
stress/strain data for various compositions in the sion about other HEA systems as a function of energy density
AlxCrFeCoNi HEA systems [118]. and scanning speed. It is important for researchers to thor-
oughly report the processing parameters to achieve a full
understanding of the trends of crystal structures and CET
CET depending on processing parameters in with respect to these processing parameters to aid with the

DEDed HEAs advancement of knowledge and the subsequent application of
The grain morphology in DED is less affected by energy den- HEAs in practice.
sity and scanning speed compared to SLM. The solidification In general, the scanning velocities used in DED is signifi-
map of DEDed samples is shown in Fig. 8. Similar to what is cantly lower than those used in SLM (v = 2–15 mm/s in DED
shown in Fig. 6, filled indicate the columnar morphology. compared to v = 200–2500 mm/s in SLM). This results in cool-
Additionally, the various shapes of the symbols represent the ing rates that could be an order of magnitude slower in DED
crystal structures of DEDed HEAs sphere and pentagon than in SLM (103 to 105 K/s compared to 104 to 106 K/s,
shows the single FCC phase and the coexistence of BCC phases, respectively) [46, 126]. The majority of DEDed structures
respectively. Data points are not represented in Fig. 8 for stud- shows the columnar grains, which suggests that the scanning
ies with missing information (presented as "–" in Table 3). velocity (and therefore the cooling rate) is too low to achieve
When a range of values is given for process parameters, the equiaxed grains. This pattern is broken only for Al-containing
data points are shown with error bars to represent the corre- and Ti25Zr50Nb0Ta25 samples, where the composition contrib-
sponding range of energy densities. utes more significantly to the nucleation of grains (these data
In the CrMnFeCoNi HEA system, the grain thickness points are not shown in Fig. 8 due to unreported process
increases from 2 to 5 μm and 7 μm as laser power increases parameters that are necessary for energy density calculation).
from 600 to 800 W and 1000 W, respectively [21]. This increase This is also the pattern observed in other materials such as
in grain thickness is explained by the decrease in G * R, where stainless steels 304 and 316, Ti–6Al–4 V, and nickel-based

REVIEW
TABLE 3: Composition, crystal structure, processing parameters, and microstructure for DEDed HEAs.
Scanning Hatching Layer Powder Energy

speed distance thickness feed rate density

Composition Crystal structure Laser power (W) (mm/s) (μm) (μm) (g/min) (J/mm3) Microstructure Reference
CrMnFeCoNi FCC 600 13.3 1000 800 10 56 Columnar [21]

800 13.3 1000 800 10 75 Columnar [21]
1000 13.3 1000 800 10 94 Columnar [21]
880 10 1200 600 8.6 122 Columnar [110]
300 2 2000 600 – 125 Columnar [111]
370 13.3 700 350 2 113 Columnar [112]
AlCrFeCoNi BCC 600–650 5 1150 700–800 – 130–162 Columnar [114]
Al1.5CrFeCoNiCu BCC – – – – – – Columnar [33]
Al0CrFeCoNi2Cu FCC – – – 254 – – Columnar [116]
Al0.8CrFeCoNi2Cu FCC + BCC – – – 254 – – Mixed [116]
Al1.0CrFeCoNi2Cu FCC + BCC – – – 254 – – Equiaxed [116]
Al1.3CrFeCoNi2Cu FCC + BCC – – – 254 – – Equiaxed [116]
Al1.5CrFeCoNi2Cu BCC – – – 254 – – Equiaxed [116]
NbMoTaW BCC Ppulse = 800 vpulse = 2.5 – 60 – – – [99]
Premelt = 4500 vremelt =
8.3
TiZrNbMoV BCC 300 5 – 250 – – Columnar [120]
1000 5 – 250 – – Columnar [120]
Ti25Zr50Nb0Ta25 BCC Ppulse = 500 vpulse = 2.5 – 125 – – Equiaxed [51]
Ti25Zr0Nb50Ta25 Premelt = 2500 vremelt = – 125 – – Columnar [51]
8.3
superalloys Inconel 625 and Inconel 718, with a few exceptions grains could be achieved in DED when the heat input is low
explained in the “Achieving equiaxed grains in alternate ways” enough [132]. In Fig. 9(a), a schematic of the grains in each
section for their exploration of the effects of other process melt pool is depicted, where equiaxed grains are obtained at
parameters to manipulate the grain morphology. the top of the layer due to the rapid solidification and columnar
grains underneath. If the laser power is high enough to remelt
Achieving equiaxed grains in alternate ways the previous layer, these equiaxed grains are melted again, and
the columnar grains grow beyond each deposited layer, as
Although it is difficult to attain an equiaxed microstructure in shown in Fig. 9(b). However, if the laser power is low enough,
DED due to the slow scanning speed, there are alternate ways the grain morphology in each melt pool is contained within
in which equiaxed grains are achieved using various approaches one layer, as shown in Fig. 9(c). An iterative process parameter
(such as using a pulsed laser and ultrasonic vibration) that have optimization is highly critical to eliminate pores, particularly
been reported for other materials such as stainless steel and when low energy input (e.g., lower laser power and higher
titanium alloys. For instance, Ti–6Al–4V printed with P =

feed rate) is used to fabricate parts.
480 W, v = 16.7 mm/s, and E = 144 J/mm3 shows purely
columnar grain morphology; however, when the same process
parameters are used to print with a superimposed pulsed laser OUTLOOK
at P = 100 W with a frequency of 500 Hz onto a continuous AM of HEAs is a relatively young field but is attracting more
laser at P = 300 W, the grains become finer and equiaxed and more attention within the scientific community. So far, a
[127]. When repeated at a higher laser power (P = 1200 W great progress has been achieved in this field. However, we
with a pulsed laser at P = 400 W with a frequency of 500 Hz), are still at an early stage, and more systematic and fundamental
the grains are still equiaxed, as compared to the fully columnar studies are needed. Due to directional heat transfer, AM leads
grain structure seen at P = 1800 W [127]. This is believed to be to the formation of columnar grains that are prone to solidifi-
because of a disturbance in thermal behavior caused by the cation cracking. Equiaxed solidification is highly desirable to
pulsed laser that hinders the epitaxial growth of grains into suc- achieve superior damage tolerance and isotropic properties.
cessive layers [127, 128]. Additionally, ultrasonic vibration has The roles of process parameters, compositions that promote
been used to assist in the metal solidification process during the formation of dual phase or composite HEAs, interstitial ele-
DED to promote the growth of equiaxed grains [129, 130, 131]. ments, and inoculant particles are discussed in this paper.
When ultrasonic vibration is added to the fabrication process, Increasing the scan speed seems to promote the CET in single-
the microstructure is refined, and equiaxed grains are achieved. phase HEAs but only for SLM process, which has a wider range
Furthermore, it has been observed that the growth of equiaxed of scan velocities, and only for very high scan speeds.

REVIEW
Figure 9: Schematic of grain growth (a)

within one melt pool, (b) with a high
energy input, and (c) a low energy input.
Increasing the scan speed could lead to the formation of more The composition space of HEAs is huge, and although we
pores inside the structure, as the energy density might not be have seen great studies focusing on a single composition, the
enough to avoid lack-of-fusion defects. Dual-phase and com- scientific community would benefit more from high-
posite HEAs have a greater tendency to form equiaxed grains throughput studies elucidating the role of different elements
compared with single-phase solid solutions. For example, or process parameters on microstructure and properties of
when the Al element is added to the FCC matrix, the transition printed parts. As discussed in the paper, such combinatorial
from columnar to equiaxed growth is observed. Similarly, studies are feasible with DED, and more attention is needed
growth-restricting solutes (e.g., Ti, Cu, and C) [133, 134, 135] to be directed toward using this approach to establish the com-
could be considered as alloying elements in order to reduce position–processing–microstructure–property relationships in
the grain size and transform the microstructure into equiaxed HEAs. While conducting these studies, care must be taken to
grains. The addition of carbon (and perhaps other interstitial make the necessary connection between the powder and

elements) to HEAs could also promote the transition to equi- deposit compositions. A significant difference in melting tem-
axed grains, but studies in this area are too limited to draw a peratures of constituent elements in HEAs makes specific ele-
conclusion. A similar effect is expected by the addition of ments susceptible to evaporation [51]. A laser energy high
nucleant particles. More systematic studies are required in enough to melt the element with the highest melting tempera-
this area to identify the efficient nucleant-particle type and ture causes the evaporation of other elements when the parti-
quantity for each HEA system. Additional strategies such as cles interact with the laser. Al, Mn, and Ti elements, which
application of external stimuli (e.g., ultrasonic vibration) and are widely added in HEAs, are especially susceptible to vapor-
modulating the laser (e.g., operating in pulsed mode) have ization during printing, leading to the change in both compo-
been investigated to a very limited extent for other material sys- sition and lattice parameters. Higher energy densities could
tems. These methods could be applicable to HEAs to achieve cause greater elemental losses [78]. Thus, we need to optimize
equiaxed microstructure without modifying the composition. the processing parameters to prevent preferential vaporization
Future efforts should be focused on an in-depth understanding or tune the composition of the feedstock by adding more of
of the efficiency of each method in shifting the CET transition the elements susceptible to vaporization based on the extent
into the optimized processing window for AM. Our proposed of the elemental loss.
method of correlating process parameters to solidification Among the HEAs studied so far, much attention has been
parameters could be a viable path toward establishing such paid to FCC HEAs and less to BCC and refractory HEAs. This
relationships. is despite the fact that AM could enable the production of

REVIEW
refractory-based materials in near-net shapes rather than alloy- equiaxed grains and provide insight into the alloy design of
ing them with other metals to make them workable. Future additive manufactured HEAs. Chemically gradient HEAs that
efforts should be focused on refractory HEAs to unlock their can be built by DED allow for sorting out the vast composi-
full potential in applications in extreme environments. It is tional space of HEAs effectively, which facilitates the develop-
worth mentioning that refractory powders tend to have irregu- ment and systematic investigation of novel HEAs and their
lar shapes that might affect the processability of these powders potentials.
and eventually the quality of printed parts. Studying the effects
of powder shape on part quality or identifying methods to
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Materials and manufacturing renaissance: Additive manufacturing of high-

Article in Journal of Materials Research · June 2020

Jinyeon Kim Akane Wakai

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Materials and manufacturing renaissance: Additive

INTRODUCTION The thermodynamics of phase stability is used to describe

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Figure 3: The process parameter

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Laser Scanning Hatching Layer Energy

power speed distance thickness density

CrMnFeCoNi FCC + tetragonal σ 400 800 90 30 186 – [82]

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© Materials Research Society 2020 cambridge.org/JMR 1968

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The temperature gradient (G) and solidification front

known as the Rosenthal equation. The Rosenthal equation con- dz V j2 + z 2

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© Materials Research Society 2020 cambridge.org/JMR 1970

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when AlCrFeCoNi HEA [28] is built with increasing laser power

rate, the grain size is increased. Additionally, CrFeCoNiC0.05

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not only higher productivity but versatility for alloy develop-

parameters, advantages, and disadvantages of DED are dis-

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Scanning Hatching Layer Powder Energy

speed distance thickness feed rate density

CrMnFeCoNi FCC 600 13.3 1000 800 10 56 Columnar [21]

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Figure 9: Schematic of grain growth (a)

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© Materials Research Society 2020 cambridge.org/JMR 1980

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Compd. 813, 152196 (2020). 113. M. Laurent-Brocq, A. Akhatova, L. Perrière, S. Chebini,

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© Materials Research Society 2020 cambridge.org/JMR 1982