Nanoparticles of Fe-Co-Ni three-component alloy capsulated into carbon matrix were synthesized. Structure, phase composition and magnetic properties of obtained materials were defined by diffractometry and magnetometry. It was established that composition of nanoparticles is determine by synthesis temperature, because nanoparticles of three-component alloy are forms by dissolution of cobalt in Fe-Ni alloy. Magnetization of Fe-Co-Ni/C nanocomposites and coercive force increases from 26 up to 58 A·m2/kg during
temperature increase that relates with growth of particles size and increase of cobalt content in the alloy

Emelyanov, S.G.

Kozhitov, L.V.

Muratov, D.G.

Pavlova, A.A.

Popkova, A.V.

Vasilyev, A.V.

English

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 8 No 3, 03037(3pp) (2016) Том 8 № 3, 03037(3cc) (2016) 
 
 
2077-6772/2016/8(3)03037(3) 03037-1  2016 Sumy State University 
Synthesis of Nanoparticles of Fe-Co-Ni Three-component Alloy Capsulated Into Carbon  
Matrix of Fe-Co-Ni/C Nanocomposites 
 
D.G. Muratov1,2,*, L.V. Kozhitov1, S.G. Emelyanov3, A.V. Vasilyev1,2, A.V. Popkova4, A.A. Pavlova5 
 
1 National University of Science and Technology MISiS, 4, Leninskiy prosp., 119049 Moscow, Russia 
2 A.V.Topchiev Institute of Petrochemical Synthesis, RAS, 29, Leninskiy prosp., 119991 Moscow, Russia 
3 Southwest State University, 94, 50 let Oktyabrya st., 305040 Kursk, Russia 
4 Tver State University, 33, Zhelyabova st., 170100 Tver, Russia 
5 National research Tomsk State University, 36, Lenin ave., 634050 Tomsk, Russia 
 
(Received 11 May 2016; published online 03 October 2016) 
 
Nanoparticles of Fe-Co-Ni three-component alloy capsulated into carbon matrix were synthesized. 
Structure, phase composition and magnetic properties of obtained materials were defined by diffractometry 
and magnetometry. It was established that composition of nanoparticles is determine by synthesis temper-
ature, because nanoparticles of three-component alloy are forms by dissolution of cobalt in Fe-Ni alloy. 
Magnetization of Fe-Co-Ni/C nanocomposites and coercive force increases from 26 up to 58 A·m2/kg during 
temperature increase that relates with growth of particles size and increase of cobalt content in the alloy.   
 
Keywords: Synthesis, Metal-carbon composites, Nanoparticles of Fe-Co-Ni, Saturation magnetization, 
Coercive force, Squareness ratio. 
 
DOI: 10.21272/jnep.8(3).03037 PACS number: 82.50.Bc 
 
 
                                                 
* muratov@ips.ac.ru 
1. INTRODUCTION 
 
Considerable attention has been paid to the 
nanostructured materials, which is caused by specific 
magnetic properties which appear in nanosized state:  
high magnetization and coercitivity, high anisotropy, 
etc. Nanoparticles of alloy of Fe family are perspective 
at with view of their application in magnetic recording 
systems [1], high-frequency devices [2, 3], magnetic 
resonance tomography [4] and biomedicine [5], 
spintronics materials [6], shielding systems from mi-
crowaves in radioabsorbing materials [7-9]. 
Fe-Co-Ni alloys have high magnetically soft proper-
ties and high thermal stability [10]. Nanosized alloys of 
Fe-Co-Ni can be used in magnetic recording systems of 
high density [1] in different diminutive sensors and 
devices [11], as a catalyst [12]. 
Previously, possibility of synthesis of binary nano-
particles capsulated into a carbon matrix of metal-
carbon nanocomposites synthesized based on polyacry-
lonitrile and salts of metals under infrared heating was 
shown [13, 14]. The aim of current investigation is syn-
thesis of nanoparticles of Fe-Co-Ni three-component 
alloy capsulated into nanocomposite carbon matrix. 
 
2. EXPERIMENT 
 
Nonacomposites were synthesized according to the 
method described in [14]. However, salts of three metals 
were used. Precursors of composites were obtained from 
solvent of dimethylformamide (Fluka, 99.5 %) polyacry-
lonitrile, nitrate iron (III) crystalline hydrate (Acros 
Organics, 99 %), nitrates of cobalt (II) and nickel (II) 
hexahydrates (Acros Organics, 99 %) with further re-
moval of solvent under temperature Т ≤ 90 °С were ob-
tained. Concentration of polyacrylonitrile in dimethyl-
formamide solution was 5 % wt. Total concentration of 
metals in precursor was 20 % wt, ratio of metals was 
Fe : Co : Ni  1 : 1 : 1 by mass. 
X-ray phase and X-ray diffraction analysys were car-
ried out at the room temperature on X-ray diffractome-
ter DIFRAY, Crkα radiation. Magnetic properties were 
obtained by PPMS-14 by Quantum Design. Sensitivity 
of this method is 10 – 6 Аm2. 
 
3. RESULTS AND DISCUSSION 
 
During the infrared pyrolysis of polyacrylonitrile 
and formation of carbon matrix based on it there is an 
extraction of considerable amount of gas products in-
cluding Н2, NH3, CO which are reductants for metals 
compounds. It should be noted that the process of re-
duction takes place in solid phase of polymer. That is 
why the reduction of metal is in situ. In reduction 
atomic hydrogen formed by destruction of the main 
polymer chain under infrared heating is used. 
Metal-carbon nanocomposites based on polyacrylo-
nitrile and compounds of Fe, Co и Ni were synthesized. 
X-ray fluorescence analysis revealed that the formation 
of nanoparticles of three-component alloy occurs at 200-
500 °C. Phase analysis showed that for materials syn-
thesized at Т ≥ 500 °C significant lines of FeNiСо alloy 
(2θ  67,8°, 79°, 132°) are observed. Also there is slight 
content of hexagonal high density (HHD) phase of co-
balt (Fig. 1) 
There are a few phases of oxides (ferric oxide and 
nickel oxide) in obtained samples (Т  200 °С), indicating 
that partial reduction of Fe2O3 to FeO with formation of 
Fe3O4 and, probably, nickel ferrite. Also, cobalt partially 
was reduced with formation of nanoparticles with HDD. 
Increase in the temperature up to 500 °С leads to 
practically full reduction of metal oxides to metals with 
formation of Fe-Co-Ni alloy based on Ni-Fe solid solution 
and high temperature face-centered cubic lattice (FCL) 
 D.G. MURATOV, L.V. KOZHITOV, S.G. EMELYANOV, ET AL. J. NANO- ELECTRON. PHYS. 8, 03037 (2016) 
 
 
03037-2 
of cobalt phase. There is low-temperature phase of cobalt 
HDD. 
Further increase of temperature of nanocomposites 
synthesis induced higher intensity of lines of metal 
phase, indicating the growth of sizes pf alloy crystallite 
Fe-Co-Ni. 
During the increase of synthesis temperature from 
500 to 700 °С HDD phase of cobalt disapears. Maximum 
of peak of the alloy goes to the left that indicates the 
growth of lattice constant. It is well known that cobalt 
and nickel generate a continuous row of solid solutions. 
The higher nickel concentration is the lower the lattice 
parameter solid solution is because nickel has smaller 
atomic radius. 
 
20 30 40 50 60 70 80 90 100 110 120 130 140
300
400
500
600
700 Co-HHD
Ni
Fe
2
O
3
NiFe
2
O
4
/ Fe
3
O
4
c
I,
 i
m
p.
2, degree  
a 
20 30 40 50 60 70 80 90 100 110 120 130 140
200
400
600
800
1000
1200
1400
HDD-Co
FCL-(FeNi)
FCL-Co
Ni
cI
, 
im
p
.
2, degree  
b 
20 30 40 50 60 70 80 90 100 110 120 130 140
500
1000
1500
2000
2500
Ni
NiFe
2
O
4
/ Fe
3
O
4
FCL-Co
FCL-(FeNi)
HDD-Co
c
I,
 i
m
p.
2, degree  
c 
20 30 40 50 60 70 80 90 100 110 120 130 140
1000
2000
3000
4000
5000
HDD-Co
FCL-(FeNi)
FCL-Co
c
I,
 i
m
p
.
2, degree  
d 
65 66 67 68 69 70
0
1000
2000
3000
4000
5000
 
 
I,
 im
p.
2, degree
FeNi
1-x
Co
x
 500 
0
C
 600 
0
C
 700 
0
C
 
e 
 
Fig. 1 – Diffraction pattern of nanocomposites synthesized at 
different temperatures: 200 °С (a), 500 °С (b), 600 °С (c), 
700 °С, fragment of фрагмент diffraction pattern 2θ  65-70° 
 
There is the growth of lattice parameter in nano-
composites that indicates the dissolution of cobalt in 
FeNi alloy where cobalt replaces nickel. According to 
computation the average size of crystallite increases 
from 10-12 to 23-25 at the synthesis temperatures 500-
700 °С. 
At diffraction patterns of samples synthesized at 
500 °C at the angles 20°-40° halo is obsereved, which is 
typical of the weakly ordered structures. Amorphous 
halo at X-ray pattern relates to the small size of coher-
ent-scattering region of crystallite of graphite-alike 
phase. Also, halo is defined by bending and irregular 
displacement of grapheme planes from each other, as 
shown in [15]. The intensity of halo increases with in-
crease of temperature that corresponds to a carbon ma-
trix of nanocomposite, and its minimum shifts to angle 
of 39° that corresponds to graphite planes d002 that re-
lates to processes of graphitization and formation of 
nanocrystall structure of matrix. Increase in lines in-
tensity and shifting of maximum to area of big angles 
2θ indicates the decrease of degree of matrix amor-
phism and increase in average size of crystallite of 
graphite-alike phase. 
Analysis of magnetic properties of FeNiCo/C nano-
composites confirms the results of X-ray phase and  
X-ray diffraction analysis (Fig. 2). 
At the synthesis temperature ranged 200-500 °С 
there is considerable increase of magnetization of nano-
composites that relates with formation of metal alloy 
from appropriate oxides and with increase of nanopar-
ticles size. In the synthesis temperature range of 500-
700 °С there is increase of magnetization with increase 
of coercive force. The results are shown in Table 1. 
 
Table 1 – Results of magnetic measurements of nanocompo-
sites of Fe-Ni-Co/C 
 
Synthesis 
temperature, 
ºС 
Мs, 
Аm2/kg 
Мr, 
Аm2/ 
kg 
Нс, 
Oe 
Mr/Ms d, nm 
200 0,8 0,06 98 0,07 7-9 
500 26 4,9 120 0,19 10-12 
600 37 10 255 0,27 15-17 
700 58 17,6 330 0,31 23-25 
 
 SYNTHESIS OF NANOPARTICLES OF FE-CO-NI… J. NANO- ELECTRON. PHYS. 8, 03037 (2016) 
 
 
03037-3 
-4000 -2000 0 2000 4000
-60
-40
-20
0
20
40
60 4
3
2
1
 
 
M
, 
A
 m
2
 k
g
-1
H, Oe
 
Fig. 2 – Loop of magnetization reversal of nanocomposites 
synthesized at different temperatures, °С: 200 (1), 500 (2), 600 
(3), 700 (4) 
 
Analysis of values of magnetization and ratio shown 
that at synthesis temperature Т  200 °С there is a 
primary formation of super paramagnetic nanoparticles 
that shows up in small value Mr/Ms and saturation in 
fields greater than 10 kOe. Also low level of magnetiza-
tion shows the absence of zero-valent metal or alloy. 
During the increase of synthesis temperature from 500 
to 700 °С there is growth of saturation magnetization, 
residual magnetization and squareness ratio of hyste-
resis loop that indicates the nanoparticles size growth. 
Also during the increase of temperature the coercive 
force sufficiently increases from 120 to 330 Oe, which 
relates to dissolution of cobalt in Fe-Ni alloy. 
 
4. CONCLUSION 
 
Thus, metal-carbon nanocomposites of Fe-Co-Ni/C 
were synthesized using salt nitrate of metals and poly-
acrylonitrile under infrared heating. It was established 
that formation of homogeneous solid solution of these 
three metals was in condition of 33 % wg. concentration 
of each metal in that case the FCL of alloy is forming. 
At temperature range of 200-500 °С the HDD phase of 
cobalt is observed. It should be mentioned that for-
mation of alloy arises from metal oxides, which is 
formed by decomposition of nitrates and reduce under 
infrared heating. 
Disagreement of lines maximums with diffraction 
pattern and etalon of FeNi and Co with FCL can be ex-
plained by formation of a three-component alloy. The 
process of alloy formation has a diffusive character that 
is expressed in shifting of lines maximums during the 
increase of synthesis temperature. It also influences 
growth of nanoparticles size. The average size of crystal-
lite increase from 10-12 to 23-25 in synthesis tempera-
ture range of 500-700 °С.  
Investigation of magnetic properties of nanocompo-
sites confirms the results of X-ray diffraction analysis. 
Increase in magnetization and squareness ratio of hys-
teresis loop during the synthesis temperature increase 
indicates the nanoparticles size increase, whereas, in-
crease of coercive force relates with dissolution of cobalt 
in naoparticles of FeNi alloy. 
The research was carried out within the state as-
signment of Russian Ministry of Education and Science 
of National University of Science and Technology 
(theme №3035023 «Complex investigation of multifunc-
tional materials 01.01.2014 – 31.12.2016) and Presi-
dent’s grant for young scientists and graduate student 
№ СП-3513.2016.1. 
 
 
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Synthesis of Nanoparticles of Fe-Co-Ni Three-component Alloy Capsulated Into Carbon Matrix of Fe-Co-Ni/C Nanocomposites

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Synthesis of Nanoparticles of Fe-Co-Ni Three-component Alloy Capsulated Into Carbon Matrix of Fe-Co-Ni/C Nanocomposites

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