Vacuum 157 (2018) 354–360

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Vacuum
journal homepage: www.elsevier.com/locate/vacuum

The influence of cooling rate on the microstructure and phase fraction of gas T
atomized NiAl3 alloy powders during rapid solidification
Liming Sang, Yi Xu∗, Pengjun Fang, Honglin Zhang, Yuntao Cai, Xinyu Liu
School of Materials Science & Engineering, Southwest Jiaotong University, Chengdu, 610031, China

A R T I C LE I N FO A B S T R A C T

Keywords: NiAl3 alloy powders were produced by nitrogen gas atomization in this paper. The microstructure and phase
NiAl3 alloy powder compositions of different particle size powders were characterized by scanning electron microscopy (SEM), X-ray
Gas atomization diffraction (XRD) and electron backscattered diffraction (EBSD). The atomized powders are composed of Ni2Al3,
Solidification microstructure NiAl3 and Al-eutectic phases, and three main types of solidification microstructures were identified: dendrites,
Phase fraction
refined dendrites, and compounds. Phase fraction of three representative particles with diameter of 60, 140 and
Raney nickel catalyst
220 μm were measured. Moreover, the Newtonian heat transfer formulation coupled with the classical hetero-
geneous nucleation was used for analyzing the influence of heat transfer coefficient and cooling rate on the
thermal history of droplets. Therefore, this work highlights the experimental results matched well with the
theoretical calculation and guides the further production of high NiAl3 phase Raney nickel catalytic powders.

1. Introduction experimental measurements to predicate surface distribution of residual

Raney nickel catalysts are wildly applied to promote hydrogenation
or dehydrogenation reactions since it was discovered [1], for instance
in hydrogen fuel cells [2,3]. Traditionally, Raney nickel catalysts are
produced by casting ingots of a 50-50 wt% mixture of Ni and Al that are
subsequently crushed into coarse powders so that the catalysts can be
activated by leaching in a concentrated solution of alkali metal hy-
droxide [4]. Rapid solidification of the gas atomization process can
result in better catalytic performance compared with the cast-and-crush
process [5,6]. The powders are prepared by gas atomization own a high
cooling rate and deep undercooling because of high heat transfer be-
tween the droplets and gas [7,8]. The products usually have dis-
tinguished characteristics such as good sphericity, fluidity, reduced
segregation, ultrafine microstructure, and new metastable phase [9,10].
Wei [11] et al. researched the effect of atomization pressure on the
breakup of alloy. Different pressures control the microstructure and
phase of powders. The catalytic activity and performance of powders
depend strictly on the microstructures and phase compositions during
rapid solidification process, nominal composition, as well as droplet
size [12,13]. Devred [14] et al. studied the effect of microstructure of
gas atomized various Ni-Al alloys on catalytic activity. After the acti-
vation process, the catalytic activity was two times higher than that for
a catalyst produced by the classical industrial cast-and-crush process.
Barnard [2] et al. have combined numerical modelling and
aluminium left over from the leaching process. However, different
thermal histories make powders have different phase fraction and mi-
crostructure [12,15], the relationship between the phase fraction and
thermal history is rarely reported. To illuminate the evolution of mi-
crostructure and phase during atomization process, it is necessary to
analyze the heat and mass transfer between the atomized droplets and
atomized gas.
The objective of this study is to build mathematical modelling to
provide critical insight into how the thermal history affects the for-
mation of microstructure and NiAl3 phase. The Newtonian heat transfer
formulation coupled with the classical heterogeneous nucleation has
been introduced to predict in-flight dynamic and thermal history of
atomized NiAl3 alloy droplets. The microstructure, EDS and phase
compositions of NiAl3 alloy powders with different size range have been
monitored by SEM, XRD, EBSD. Besides, the cooling rate curve and heat
transfer coefficient of three representative size powders were in-
vestigated, in order to provide a scientific basis for the improvement of
gas atomized NiAl3 alloy powders catalyst efficiency.
2. Experimental and numerical simulation
2.1. Preparation and characterization of powders
During the gas atomization process, it was crucial to hold the high

∗
Corresponding author.
E-mail address: xybwbj@swjtu.cn (Y. Xu).

https://doi.org/10.1016/j.vacuum.2018.08.057
Received 3 June 2018; Received in revised form 27 August 2018; Accepted 28 August 2018
Available online 29 August 2018
0042-207X/ © 2018 Elsevier Ltd. All rights reserved.
L. Sang et al. Vacuum 157 (2018) 354–360

Table 1 and the change of droplet enthalpy, respectively. Here, CL and CS are the
Thermophysical parameters of nitrogen gas and NiAl3 alloy [18,20,21]. heat capacity per unit mass of liquid and solid, respectively, ΔHf is the
Parameter Symbol Value latent heat per unit mass, and TL is the liquid temperature.
During the atomization process, radiation may occur between the
Specific heat capacity Cpg (J 1039 particles and the surrounding atomization chamber walls under in-
kg−1K−1) vestigation. However, convective cooling is dominant over radiative
Gas dynamic viscosity μg (N s m−2) 1.78 × 10−5
cooling and thus the latter is safely neglected. Hence, we adopt a simple
Gas thermal conductivity k g (W m−1 2.6 × 10−2
Newtonian's law of cooling to describe the surface cooling of the droplet
K−1)
Gas density ρg (kg m−3) 1.16
in the high speed atomization gas flow for a given size d expressed by
Specific heat capacity of liquid Ni- CL (J kg−1 K−1) 690.52 dTd df 6h
Al alloy Cpd = ΔHd s − (Td − Tg ).
dt dt ρd d (3)
Specific heat capacity of solid Ni-Al CS (J kg−1 K−1) 677.69
alloy
The supersonic gas jet, the convective heat transfer coefficient h,
Latent heat per unit mass ΔHf (J kg−1) 7.51 × 105
depends on the surface temperature. The actual value is evaluated using
Density of Al ρAl (kg m−3) 2700
Density of Ni ρNi (kg m−3) 8909
the well-known correlation of Ranz and Marshall [19].
Normal composition w0 (wt.%) 57.97 kg
Density of droplet ρd (kg m−3) (w0/ ρAl + (1 − w0)/ ρNi )−1 h= (2.0 + 0.6 Re ⋅ 3 Pr ).
−2
d (4)
Solid-liquid interfacial energy σsL (J m ) 0.131
Melting point of pure solvent TM (K) 1538 Where kg is the gas thermal conductivity, Re ≡ ρg D ud − ug / μg is the
substance droplet Reynolds, Pr ≡ Cpg μg / k g is the gas Prandtl number, Cpg is the gas
Liquids temperature TL (K) 1383.4
Peretectic temperature TP(K) 1123.5
specific heat per unit mass, and μg is the gas dynamic viscosity. During
Eutectic temperature TE(K) 914.7 the computation, it is assumed that the gas temperature Tg is a constant
and that the density of liquid and solid phases are equal. It is here as-
sumed that the velocity difference varies as a quadric function of
vacuum condition and control the pressure of atomization gas [16,17]. temperature difference between droplet and gas, which is given by
Firstly, the atomization chamber of atomizing device pumped air into 2
Td − Tg ⎞
vacuum state until the vacuum degree reached to 1.1 × 10−2Pa. High ud − u g ≈ u 0 ⎛ ⎜ ⎟ .
purity Ni and Al ingots of Ni25 at%Al75 at% atomic ratio were melted ⎝ Ti ⎠ (5)
in an induction heated vacuum furnace. Then, the melt was drop down
This is only an estimate of the velocity difference due to gas-droplet
through a 3.5 mm internal diameter ceramic nozzle. The molten stream
interaction and there does not seem to exist any other alternatives of
was disintegrated by the impact of a high velocity and purity nitrogen
comparable simplicity. By combining eq. (4) and eq. (5), the cooling
(N2) at a superheat temperature of 1538 K. The liquid droplets flied in
rate in the liquid phase can be approximated as
the atomization chamber, cooled down and solidified to powders. The
atomized pressure was controlled at 3.5 MPa. Consistent with the cal- 6h
T˙ = (Td − Tg ) ≈ [κ + ξ (Td − Tg )](Td − Tg ).
culation parameters and the atomized medium, N2, had a constant ρd CL d (6)
temperature as 300 K. The physical properties of N2 and NiAl3 alloy
Where
were summarized in Table 1. As-received gas-atomization powders
were screened into four standard size ranging from 0 to 45 μm, 12k g 3κ Re′ 3 Pr ρg du 0
κ= , ξ= , and Re′ = .
45–80 μm, 80–120 μm and 120–180 μm. Phase compositions were ρd CL d2 10Ti μg (7)
identified by XRD with a Cu/Kα radiation. Microstructure was observed
using SEM, phase fraction statistics was carried out by EBSD using an
orientation imaging microscope attached to the SEM. 3. Results and discussion

2.2. Numerical simulation 3.1. Phase and microstructure characterization

To analyze and predict the conditions of microstructure evolution
and phase fraction change during rapid solidification, numerical si-
mulation of cooling and rapid solidification of different size ranges
NiAl3 alloy spherical particles were performed using the developed
Newtonian heat transfer formulation coupled with the classical het-
erogeneous nucleation mathematical model.
For a given spherical droplet, its initial melting temperature Ti is
determined by the degree of melt superheat. On the droplet surface,
with the forced convective and radiative, heat exchange with N2 con-
tributes to a rapid heat extraction. The thermal history of droplet so-
lidification containing both liquid and solid phases can be defined by
Ref. [18].
dHd dT df
= Cpd d − ΔHd s .
dt dt dt
Here, Hd , Td , and fs are the droplet enthalpy per unit mass, droplet
temperature, and the solid fraction, respectively.
Where the terms,
Cpd = CL − (CL − CS ) fs and, ΔHd = ΔHf − (CL − CS )(TL − Td ).
Represent the heat capacities per unit mass of liquid-solid mixture,
The XRD patterns of four size ranges examined powders are shown
in Fig. 1. By comparing the experimental determined peaks with XRD
databases, the atomized powders are composed of three phases: Ni2Al3,
NiAl3 and Al-eutectic phase, which are consistent with what we can
expect from phase diagram [9]. Furthermore, the peaks of Ni2Al3, NiAl3
and Al-eutectic phase increase in intensity when associate with the
smaller size range powders, indicating that phase formation is not
subject to the solidification process. Tourret [22] believes that the final
fraction of phase content in the atomized NiAl3 alloy powders are re-
lated to powders size, i.e. cooling rate or cooling kinetics.
Morphology and cross-sectional microstructure of the NiAl3 pow-
ders are given in Fig. 2. A near-spherical powder with the diameter
under 45 μm, as shown in Fig. 2(a), reveals the rough surface mor-
phology of dendritic structures. Fig. 2(b) gives the cross section of a
(1)
similar size powder, where developed dendrites can be found in the
cross section. With particles size increasing, fine and orthogonal den-
drites are clearly observed from the surface and internal morphology,
shown in Fig. 2(c) and (d). The fine dendrite morphology with big
dendrite arms is the characteristic feature of the growth of solid phase
(2)
from the liquid phase during rapid solidification. With further in-
creasing the particle size to 80–120 μm, the particle's surface are

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L. Sang et al.
Fig. 1. XRD patterns of the NiAl3 alloy powders with four size range:
d < 45 μm, 45 μm-80 μm, 80 μm-120 μm, 120 μm-180 μm.
orthogonal isometric dendrites (Fig. 2(e)), while its internal micro-
structure reveals a compound microstructure: typical equiaxed den-
drites. For some large powders with the diameter of 120–180 μm, a few
satellite powders and cellular microstructure can be seen on the particle
surface, Fig. 2(g). However, there are a larger amount of broken den-
drite microstructures in its profile. As the particles size increase, the
dendrites grow up and some dendrites broken, a similar phenomenon
has been also observed in the rapid solidification alloy powders. It is
mainly attributed to the much higher cooling rate which small powders
received as compared to larger particles [13]. Fig. 3 (b) shows the EDS
image of a NiAl3 alloy powder surface. The EDS spectrum shows that
the main composition of Ni, Al alloy element is basic consistent with the
raw Ni25Al75 material. The metal powder prepared by gas atomization
method will not cause the wastage of element content. No oxygen
element was detected, it illustrated that high vacuum and nitrogen at-
mosphere protection effectively prevented droplets from being oxidized
during atomization.
3.2. Phase formation and cooling curve
The local microstructure characterization of a powder combine with
an EBSD image of the phase morphology is shown in Fig. 4. Three main
types of solidification microstructures (dendrites, refined dendrites, and
few cellular) observed in the powder are documented in Fig. 4(a). Three
different greyscales representing different phase can be seen in this
image, and associate with Fig. 4(b), it is clearly to identify the phase
structure. The brightest with dendrites structure correspond to blue
region are the primary Ni2Al3 phases, the light gray layer surrounding
the primary solid with red region represents the peritectic NiAl3 phases,
the black region filling most of the remaining interdendritic space is the
Al-eutectic phase.
Variation in droplet temperature with flight distance for NiAl3 alloy
powders of 30, 45, 60, 80 μm in diameter are calculated by equations
(1)–(3), shown in Fig. 5. Here, the influence of wetting angle θ , set as a
constant of 40°, can be neglected. The change of droplet temperature
can be divided into five different thermal stages. When the N2 impacts
the melting liquid, atomized droplets rapidly cool to the nucleation
temperature within a short flight distance. A recalescence begins to take
place, and primary Ni2Al3 phase nucleates at TN. The nucleation tem-
perature is nearly insensitive to the droplet size. Subsequently, latent
heat releases and heats the undercooled droplet rapidly until it reaches
approximately the liquidus temperature of 1383.4 K. The recalescence
finished when the heat extraction rate by surrounding gas becomes
comparable to the latent heat release rate due to solidification. Then the
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Vacuum 157 (2018) 354–360
segregated solidification occurs, and the droplet temperature decreases
at a lower rate. Until the droplet temperature cooling to 1123.5 K,
peritectic transformation takes place and shows a constant temperature
plateau. According to equilibrium phase diagram, remaining liquid and
partial primary phase transform into NiAl3 phase. Local microstructure
characterization suggests that NiAl3 forms an envelope around Ni2Al3.
Furthermore, eutectic reaction occurs at 914.7 K, interdendritic residual
liquid forms Al-eutectic phase. Finally, the droplets are continuously
cooled until they completely solidify. It is seen that the onset and
completion of solidification are shifted to greater flight distance with
increasing droplet diameter.
3.3. The relation between phase fraction and cooling rate
The phase maps are show in Fig. 6(a), (b), and (c), respectively.
Histogram in Fig. 6(d) quantifies the percentage population of the solid
phase in analyzed phase fraction of NiAl3 powders in diameter of 60,
140 and 220 μm. The peritectic NiAl3 phase represents the dominant
phase in particles in which diameter less than 140 μm. Its percentage
population decreases with increasing size of phase fraction from 45.3%
to 23.8%, as well as the Al-eutectic phase increases to 58.6% (in particle
220 μm in diameter). Similar tend have been reported previously [9].
Also, it can be speculated that the peritectic transformation plays a
dominant role in the solidification process. The variational phase
fraction of powders in different diameter reflects the competition
phenomenon of phases' nucleation/growth kinetic during the non-
equilibrium solidification.
Fig. 7(a) illustrates the convective heat transfer coefficient which is
calculated by equation (4). The value of heat transfer coefficients in
different diameter particles have similar shifty trend with the flight
distance. Heat transfer coefficient decreases as the droplet velocity
approaches the gas velocity gradually. Additionally, at the distance
where the droplet and gas get the zero relative velocity, it shows a
minimum value. Beyond this distance, the heat transfer coefficients
increase inversely due to the gradual increase in the slip velocity.
Smaller droplets exhibit a higher heat transfer coefficient in whole
flight process, and the heat transfer coefficient significantly affects the
cooling rate of droplet.
Fig. 7(b) shows the computed cooling rate for NiAl3 alloy droplets of
60, 140, 220 μm in diameter with flight distance. The initial cooling
rates of the fully liquid droplets are about 3 × 105 K s−1, 8 × 104 K s−1
and 4 × 104 K s−1 for droplet size 60, 140 and 220 μm, respectively,
rapid decline in cooling rate with increasing particle size. The cooling
rate for 60 μm droplet keeps at about 8 × 104 K s−1 when nucleation
occurs and high cooling rate can result in metastable conditions which
promotes primary Ni2Al3 phase formation. However, it has only 25.4%
Ni2Al3 phase remained after complete solidification. This may be at-
tributed to metastable phase fragmentation during solidification pro-
cess. Once recalescence takes place, the cooling rate is negative or
approaches zero when the heat extraction rate through the medium
becomes comparable to the latent heat release rate. Conventional so-
lidification happens after recalescence in accordance with Schiel [18]
equation. At the same time, the cooling rate increases again due to the
increase heat transfer coefficient, up to approximately 1 × 105 K s−1,
which causes rapid liquid undercooling and great composition gradient
within primary Ni2Al3 phase at the pre-peritectic stage. When droplet
temperature reach TP, direct liquid→NiAl3 solidification and peritectic
transformation Ni2Al3→NiAl3 take place. According to statistical phase
fraction results, NiAl3 phase occupies almost one half phases for droplet
size less than 140 μm, the phase fractions of both NiAl3 and Ni2Al3
decease with increase droplets diameter. It can be speculated that the
direct solidification plays a dominant role in smaller droplets during
peritectic reaction stage and quiet restricts Al-eutectic growth. As-
sociate with microstructure characterization, large droplets present
variety fragmentized and compound structures. The result demon-
strates that Ni2Al3→NiAl3 transformation mainly happens in larger
L. Sang et al. Vacuum 157 (2018) 354–360

Fig. 2. Surface and cross-sectional microstructures of NiAl3 powders with the different particle size: (a) and (b) 0–45 μm, (c) and (d) 45–80 μm, (e) and (f)
80–120 μm, (g) and (h) 120–180 μm.

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L. Sang et al. Vacuum 157 (2018) 354–360

Fig. 3. Microstructure(a) and element composition(b) of NiAl3 alloy powder surface.

droplets and gradually becomes the main method of NiAl3 phase gen-
eration with increasing droplet diameter. As for droplet with the dia-
meter of 220 μm, with lower heat transfer coefficient, plenty of Ni2Al3
phases are induced fragmentation by latent heat release. Besides, NiAl3
forming directly from the liquid is quite restrictive. When droplet
temperature reach TE, abundant Al-eutectic phases form from re-
maining liquid.

4. Conclusions

The phase compositions and microstructure of nitrogen atomized

NiAl3 alloy powders have been characterized. The effect of droplet
temperature, heat transfer coefficient, cooling rate on varying phase
fraction and microstructure transformation of different size powders
during rapid solidification process have been investigated.

(1) Among Ni2Al3, NiAl3 and Al-eutectic phases are identified in four
different size atomized NiAl3 powders. With powder size increases, Fig. 5. Calculated variations droplet temperature of 30, 45, 60, 80 μm diameter
the powder surface morphology is transformed from dendrite to droplets with flight distance.
cellular structure, and the profiles are presented as three main types
microstructures: dendritic, refined dendritic and compound.
the Al-eutectic phases reach 58.6%, when the diameter of powder is
(2) The cooling and solidification process of a droplet consists of five
up to 220 μm.
stages, the primary Ni2Al3 phase nucleation before recalescence, the
(3) Phase formation is accompanied by variational nucleation kinetics
NiAl3 phase forms an envelope around Ni2Al3 phase and last
in different diameter powders. Smaller droplets exhibit higher heat
forming Al-eutectic with remaining liquid. The nucleation tem-
transfer coefficient and get higher initial cooling rate. NiAl3 phase
perature is nearly insensitive to the droplet size. The amount of
direct solidification from liquid plays a dominant role in smaller
Ni2Al3 and NiAl3 phase decreases with increasing particle size, and
droplets during peritectic reaction stage and promotes a large

Fig. 4. Microstructure and phase distribution of solidified NiAl3 alloy powder. (a) SEM images, (b) the EBSD micrograph shows the Ni2Al3, NiAl3 and Al-eutectic
phase.

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L. Sang et al. Vacuum 157 (2018) 354–360

Fig. 6. EBSD phase maps of particles: (a) d = 60 μm, (b) d = 140 μm, (c) d = 220 μm; (d) the fraction of Ni2Al3, NiAl3, and Al-eutectic phase in three particles.

amount of nucleation and growth. Otherwise, Ni2Al3→NiAl3 frag- Acknowledgements

mentation transformation mainly happens in larger droplets and
gradually becomes the main method of NiAl3 phase generation with
increasing droplet diameter. Calculating results explain the law of
phase fraction change in different size powders well and guide
further production of high NiAl3 phase fraction powder catalysts.
The authors thank the National Key Project of Research and
Development Program of China (2016YFB1100202) for financial sup-
port.

Fig. 7. Calculated variations of (a) heat transfer coefficient, and (b) cooling rate versus the flight distance.

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Appendix A. Supplementary data
Supplementary data related to this article can be found at https://
doi.org/10.1016/j.vacuum.2018.08.057.
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