Met. Mater. Int., Vol. 16, No. 4 (2010), pp.

643~647
doi: 10.1007/s12540-010-0819-8 Published 26 August 2010

Characteristics of Fine Size Fe-Ni Alloy Powders Directly Prepared

by Spray Pyrolysis

H. C. Jang, S. H. Ju, and Y. C. Kang*

Department of Chemical Engineering, Konkuk University,

1 Hwayang-dong, Gwangjin-gu, Seoul 143-701, Korea
(received date: 22 March 2009 / accepted date: 29 November 2009)

Fe-Ni alloy powders with composition of Fe0.25Ni0.75 were directly prepared by spray pyrolysis. The powders
prepared at temperatures of 1200 and 1400 °C had peaks of pure Fe-Ni3 alloy phase. The alloy powders
with a spherical shape and dense structure were prepared at a temperature of 1400 °C by melting the powders.
The composition ratio of Fe and Ni components in the alloy powders prepared at a temperature of 1400 °C
coincided well with that of the spray solution. The mean sizes of the alloy powders changed from 0.20
to 0.74 µm when the concentrations of the spray solution changed from 0.02 to 1 M. The alloy powders
prepared from the spray solution with a concentration of 0.5 M had a maximum saturation magnetization
and minimum coercivity values as 96.95 emu g−1 and 34.67 Oe, respectively.
Keywords: alloys, magnetic materials, chemical synthesis, magnetic properties

1. INTRODUCTION properties of Fe-Ni alloy powders directly prepared by spray

Fe-Ni alloys are of great interest due to their low thermal
expansion and remarkable magnetic and mechanical proper-
ties. Fe-Ni alloy powders have been prepared by various
methods, including melting, mechanical alloying, chemical
reduction, and gas condensation [1-8]. The morphologies,
mean crystallite sizes, mean powder sizes, and phase purities
of the Fe-Ni alloy powders have been affected by the alloy
preparation processes. Therefore, the characteristics of the
Fe-Ni alloy powders have also been affected by the prepara-
tion processes.
Spray pyrolysis, which is one of the gas-phase reaction
methods, is a useful method for synthesizing pure metal and
alloy powders [9,10]. The alloy powders prepared by spray
pyrolysis have a spherical shape, high crystallinity, high den-
sity, and low content of impurity due to the high preparation
temperatures above 1000 °C. Spherical shape FeNi alloy
powders were also prepared by spray pyrolysis [11]. How-
ever, the magnetic properties of the Fe-Ni powders prepared
by spray pyrolysis have not been studied.
In this study, Fe-Ni alloy powders with a composition of
Fe0.25Ni0.75 were directly prepared by spray pyrolysis in a
reduction atmosphere. The effects of preparation tempera-
tures on the morphologies, crystal structures, and magnetic
*Corresponding author: yckang@konkuk.ac.kr
©KIM and Springer
pyrolysis were investigated.
2. EXPERIMENTAL PROCEDURE
The spray pyrolysis system used in this study is shown in
Figure 1. The system consists of a droplet generator, alumina
reactor, and a powder collector. A 1.7-MHz ultrasonic spray
generator with six vibrators was used to generate a large
amount of droplets. The length and diameter of the alumina
reactor were 1,200 and 50 mm, respectively. The reactor
temperature changed from 1000 to 1400 °C. The flow rate of
the mixture gas (10% H2 in N2) used as the carrier gas was
fixed at 20 l/min. The precursor solution was prepared by
dissolving a stoichiometric ratio of ferric nitrate nonahydrate
[Fe(NO3)3·9H2O] and nickel nitrate hexahydrate [Ni(NO3)2
·6H2O] in distilled water. The overall solution concentrations
of Fe and Ni components changed from 0.02 to 1 M.
The crystal structures of the as-prepared Fe-Ni alloy pow-
ders were investigated using X-Ray Diffractometry (XRD,
RIGAKU DMAX-33) that used Cu Kα radiation. The mean
crystallite sizes of the alloy powders were calculated from
the half-height width of the diffraction peak of the XRD pat-
tern by using Scherrer’s equation. The morphological char-
acteristics of the powders were investigated using Scanning
Electron Microscopy (SEM, JEOL, JSM 6060). The compo-
sitions of the alloy powders were analyzed using Energy
Dispersive X-ray (EDX). A vibrating sample magnetometer
644 H. C. Jang et al.

Fig. 3. XRD patterns of Fe-Ni3 powders prepared by spray pyrolysis

at various temperatures.

dense inner structure. The melting of the powders occurred

Fig. 1. Schematic diagram of the spray pyrolysis process.
(VSM; 7300 Lakeshore, USA) was used to measure the sat-
uration magnetization of the Fe-Ni powders.
3. RESULTS AND DISCUSSIONS
The morphologies of the Fe-Ni powders prepared by spray
pyrolysis at various temperatures are shown in Figure 2. The
powders had a spherical shape and non-aggregation charac-
teristics, irrespective of the preparation temperatures. However,
the inner structures, mean sizes, and surface characteristics
of the powders were affected by the preparation tempera-
tures. The powders prepared at a temperature of 1000 °C had
a hollow inner structure, rough surface, and broad size distri-
bution. The sphericity of the powders increased with an
increase in the preparation temperatures. The powders pre-
pared at a temperature of 1400 °C had a clean surface and a
at a high temperature of 1400 °C. The mean size and geo-
metric standard deviation of the powders prepared at a tem-
perature of 1000 °C were 0.77 µm and 1.37, respectively. On
the other hand, the mean size and geometric standard devia-
tion of the powders prepared at a temperature of 1400 °C
were 0.58 µm and 1.21, respectively.
Figure 3 shows the XRD patterns of the powders prepared
at various temperatures. The powders prepared at a tempera-
ture of 1000 °C had peaks of NiFe2O4 and FeNi3 alloy phases.
Complete reduction of the powders did not occur at a prepa-
ration temperature of 1000 °C. However, the powders pre-
pared at temperatures of 1200 and 1400 °C had peaks of a
pure FeNi3 alloy phase. The XRD patterns of the powders
exhibited three distinct diffraction peaks, which matched
well with the cubic (fcc) lattice of a bulk Fe-Ni alloy. The mean
crystallite sizes of the alloy powders prepared at tempera-
tures of 1200 and 1400 °C were 31 and 38 nm, respectively.
Figure 4 shows the EDX spectra of the powders prepared
at various temperatures. The compositions measured from

Fig. 2. SEM images of Fe-Ni3 powders prepared by spray pyrolysis at various temperatures: (a) 1000 °C, (b) 1200 °C, and (c) 1400 °C.
 Characteristics of Fine Size Fe-Ni Alloy Powders Directly Prepared by Spray Pyrolysis 645

Fig. 4. EDX spectra of Fe-Ni3 powders prepared by spray pyrolysis at

various temperatures: (a) 1000 °C, (b) 1200 °C, and (c) 1400 °C.

Table 1. EDX analysis of Fe-Ni3 powders prepared by spray

pyrolysis at various temperatures
1000 °C 1200 °C 1400 °C Atomic ratio
Fe 19.93 26.93 26.58 1
Ni 58.25 73.07 73.42 3 Fig. 5. Dot mapping analysis of Fe-Ni3 powders prepared by spray
O 21.81 - - - pyrolysis at 1400 °C: (a) Image, (b) Fe, and (c) Ni.

the EDX spectra are described in Table 1. The peak of oxy-
gen was observed from the EDX spectrum, as shown in Fig-
ure 4(a). However, oxygen peaks were not observed from
the EDX spectra of the powders prepared at temperatures of
1200 and 1400 °C. The composition ratios of Fe and Ni
components in the alloy powders prepared at temperatures of
1200 and 1400 °C coincided well with that of the spray solu-
tion. Therefore, evaporation of Fe and Ni components did
not occur, even at a high preparation temperature of 1400 °C.
Figure 5 shows the results of dot mapping of the alloy pow-
ders prepared at a temperature of 1400 °C. Fe and Ni components
were well dispersed inside the submicron-sized powders.
Magnetic properties of the alloy powders prepared at vari-
ous temperatures were investigated at room temperature by
using a VSM with an applied field Oe ≤ H ≤ 9000 Oe. The
hysteresis loops of the Fe-Ni alloy powders are shown in
Figure 6. Values of saturation magnetization (Ms) and coer-
civity (Hc) were estimated from Figure 6. The measured Ms
values of the alloy powders prepared at temperatures of
−1
1000 °C, 1200 °C, and 1400 °C were 42.7 emu g , 90.8 emu
646 H. C. Jang et al.

Fig. 6. Hysteresis loops of Fe-Ni3 powders prepared by spray pyroly-

sis at various temperatures.

g−1 and 96.9 emu g−1. The powders prepared at a low temper-
ature of 1000 °C had a low Ms value because of incomplete
reduction of the powders. The measured Hc values of the
alloy powders prepared at temperatures of 1000 °C, 1200 °C,
and 1400 °C were 131.4 Oe, 45.3 Oe and 34.7 Oe. The Fe-
Ni alloy powders with a high mean crystallite size and dense
structure had high Ms and low Hc values.
The Fe-Ni alloy powders were prepared from the spray
solutions that had various concentrations at a preparation
temperature of 1400 °C. In this study, one Fe-Ni alloy pow-
der was formed from one droplet. Therefore, the mean sizes
of the alloy powders decreased by decreasing the concentra-
tions of the spray solution. The concentrations of the spray
solution changed from 0.02 M to 1 M. Figure 7 shows the
SEM images of the alloy powders prepared from the spray
solutions that had various concentrations. The mean sizes of
the powders measured from the SEM images are described
in Table 2. The mean sizes of the alloy powders changed
from 0.20 µm to 0.74 µm when the concentrations of the
spray solution changed from 0.02 M to 1 M. The broadness
of the size distribution of the alloy powders increased with
an increase in the concentrations of the spray solution. Melt-
ing of the alloy powders to a fine size occurred well, even
with a short residence time of the powders inside the hot wall Fig. 7. SEM images of Fe-Ni3 powders prepared by spray pyrolysis
reactor. Therefore, the fine-sized alloy powders prepared from spray solutions with various concentrations: (a) 1.0 M, (b) 0.07
from the spray solution with a low concentration had a nar- M, and (c) 0.02 M.
rower size distribution than those prepared from the spray
solution with a high concentration. Values of saturation mag- Table 2. Properties of Fe-Ni3 powders prepared by spray pyrolysis
netization (Ms) and coercivity (Hc) of the alloy powders pre- from spray solutions with various concentrations
pared from the spray solutions with various concentrations Total concentration of
1.0 0.5 0.07 0.02
are described in Table 2. The alloy powders prepared from spray solution (mole)
the spray solution with a concentration of 0.5 M had the Mean size (µm) 0.74 0.63 0.42 0.20
−1 Ms (emu/g) 85.10 96.95 79.58 61.02
maximum Ms and the minimum Hc values as 96.95 emu g
and 34.67 Oe, respectively. Hc (Oe) 44.36 34.67 46.99 60.74
 Characteristics of Fine Size Fe-Ni Alloy Powders Directly Prepared by Spray Pyrolysis 647

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