Metalcarbon nanocomposites based on polyacrylonitrile and nickel chloride are synthesized under the influence of infrared heat. The resulting materials represent a system of carbon matrix formed during the carbonization of PAN, and distributed in it nickel nanoparticles. The average size of the nanoparticles in the nanocomposite was 15-25 nm. It was found that the distribution of nickel nanoparticles sizes is determined by temperature synthesis nanocomposite. Thus with increasing temperature, the predominant average particle size of the metal increases, and the distribution is spread and shifted toward larger sizes.
When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/3360

Emelyanov, S.G.

Kozhitov, L.V.

Kozhitov, S.L.

Muratov, D.G.

Savchenko, A.G.

Shchetinin, I.V.

Yakushko, E.V.

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 5 No 4, 04007(4pp) (2013) Том 5 № 4, 04007(4cc) (2013) 
 
 
The article was reported at the International Conference «Physics and Technology of Nanomaterials and Structures», Kursk, 21-22 November, 2013 
2077-6772/2013/5(4)04007(4) 04007-1  2013 Sumy State University 
The Synthesis of Metalcarbon Nanocomposite Ni / C on the Basis of Polyacrylonitrile 
 
L.V. Kozhitov1, D.G. Muratov1,2, E.V. Yakushko1, S.L. Kozhitov1, A.G. Savchenko1, I.V. Shchetinin1,  
S.G. Emelyanov3, L.M. Chervjakov3 
 
1 National University of Science and Technology "MISIS", 4, Leninskii Pr., 119049 Moscow, Russia 
2 Institute of Petrochemical Synthesis named A.V. Topchiev of the Russian Academy of Sciences,  
119991 Moscow, Russia 
3 Southwest State University, 94, 50 Let Oktyabrya Str., 305040 Kursk, Russia 
 
(Received 05 August 2013; revised manuscript received 29 November 2013; published online 10 December 2013) 
 
Metalcarbon nanocomposites based on polyacrylonitrile and nickel chloride are synthesized under the 
influence of infrared heat. The resulting materials represent a system of carbon matrix formed during the 
carbonization of PAN, and distributed in it nickel nanoparticles. The average size of the nanoparticles in 
the nanocomposite was 15-25 nm. It was found that the distribution of nickel nanoparticles sizes is deter-
mined by temperature synthesis nanocomposite. Thus with increasing temperature, the predominant av-
erage particle size of the metal increases, and the distribution is spread and shifted toward larger sizes. 
 
Keywords: Metalcarbon nanocomposite, Carbon matrix, Nanoparticles of nickel. 
 
 PACS numbers: 61.48.De, 81. – b 
 
 
1. INTRODUCTION 
 
Currently functional nanomaterials are of great in-
terest to researchers because of its unique properties, 
which manifest themselves in the nanostate. In the 
nanostate for the materials new opportunities are 
opened up in both the theoretical aspect and the exper-
imental use. Special interest is composite nanomateri-
als. The composite materials comprising nanoparticles 
3d-metal (Fe, Co, Ni), and their oxides are of interest 
from the viewpoint of use as heterogeneous catalysts 
for petrochemical processes [1, 2], the growth of carbon 
nanotubes [3, 4], components of dispersed radar ab-
sorbing media [5, 6, 7]. 
Currently, there are several groups of methods and 
approaches to the formation of nanomaterials including 
nano-sized metal particles. Regardless of the approach, 
the controlled synthesis of nanoparticles with a narrow 
size distribution and well-defined structure is one of 
the main problems. 
The aim of this work is to obtain the metalcarbon 
nanocomposites based in polyacrylonitrile under IR-
heating including nickel nanoparticles dispersed in the 
carbon matrix, and the study of the structural charac-
teristics of the synthesized material. 
 
2. EXPERIMENTAL 
 
Metalcarbon nanocomposite are obtained by IR an-
nealing of polyacrylonitrile (PAN) and NiCl26H2O. 
Precursors nanocomposites were prepared by co-
dissolving PAN and NiCl26H2O in dimethylformamide 
(DMF, Fluka, 99.5 %) followed by removal of solvent. 
The concentration of PAN in DMF solution was 5 wt %. 
And nickel – 30 % by mass. Re calculation for chloride 
hexahydrate. 
Pyrolysis was carried out in the IR-camera of pulse 
photon annealing installation. IR-annealing was done 
in a two steps operation: preliminary annealing in air 
at 150 °C and 200 °C for 15 min, during which the sol-
vent is removed and PAN original structuring per-
formed, and basic annealing in an inert atmosphere at 
a desired intensity of infrared radiation that heats the 
sample to a temperature in the range 400-700 °C. The 
holding time at the final temperature was 120 s. The 
heating temperature of the sample was fixed with the 
chromel-alumel thermocouple. 
Calorimetric study carried out on a differential 
scanning calorimeter (DSC) Q20 (TA Instruments, 
USA) at a heating rate 10 °C/min in a range of 50-
350 °C. Measurements were performed in a nitrogen 
flow of 50 ml/min. Pattern in the form of powder was 
placed in a platinum crucible is sealed. 
Thermogravimetric analysis (TGA) was performed 
using a thermogravimetric analyzer Discovery TG TM 
(TA Instruments, USA) in the temperature range 50-
700 °C at a heating rate of 10 °C/min under nitrogen 
flow rate of 50 ml/min. The furnace unit is equipped 
with four heating elements operating in the infrared 
range, which are heated chamber of SiC, in which there 
is a pattern in the form of a powder, placed in a plati-
num crucible. Weighing accuracy of the instrument is 
± 0,1 %, the reproducibility of the weighing - ± 0,01 %. 
The sensitivity of the scale –  7.10 g. Temperature 
accuracy – ± 1 °C. 
TGA was carried out in the temperature range from 
50 to 700 °C at a heating rate of 10 °C/min. Atomic  
absorption spectroscopy (AAS) was performed on the 
spectrometer «AAS – 30». 
Micrographs of the samples obtained in a transmis-
sion electron microscope LEO912 ABOMEGA, 60 -
 120 kV accelerating voltage, increasing the 80-
500000 h. Phase and structural studies were carried 
out at room temperature X-ray diffraction of the com-
pany «Rigaku» Focusing on the Bragg-Brentano on CoK 
-radiation in a continuous mode. The experimental 
results were processed by methods of approximation. 
 
3. RESULTS AND DISCUSSION 
 
Using the previously developed methods [8] were 
obtained metalcarbon nanocomposites based on polyac-
rylonitrile (PAN) and nickel chloride hexahydrate. 
 L.V. KOZHITOV, D.G. MURATOV, E.V. YAKUSHKO, ET AL. J. NANO- ELECTRON. PHYS. 5, 04007 (2013) 
 
 
04007-2 
Formation of metalcarbon nanocomposite precur-
sors are in situ. Uniform distribution of the metal in 
the polymer matrix during the synthesis of the precur-
sor is achieved by processes complexation between ni-
trile groups of the polymer and the metal compound . 
In the pyrolysis of PAN is an allocation of a variety of 
gaseous products [9], among which there are hydrogen , 
CO, NH3, and that reduced nickel chloride. Due to the 
processes of structural and chemical transformations in 
the matrix of PAN and coagulation of clusters of re-
duced metal nanoparticles are formed . 
Application of electron microscopy was used to estab-
lish the structure and morphology nanocomposite Ni / C. 
Fig. 1 shows the results of transmission electron micros-
copy (TEM) nanocomposite Ni/C, obtained at 700 °C. 
 
 
 
Fig. 1 – TEM of the Ni / C nanocomposite, obtained at 700 °C 
(Ni / C 700) 
 
Light grey color - the polymer substrate used in the 
analysis by TEM. Carbon graphite-matrix nanocompo-
sites - dark gray color, which is a layered disordered 
system with the size of the coherent scattering crystal-
lites Lc from 18 to 37 Å. Studying the structure of the 
carbon matrix based on PAN was carried out in [10]. 
Quite dark, black spherical formations - nanoparticles 
of nickel. 
Fig. 2 shows the diffraction pattern of nickel- con-
taining nanocomposites obtained at different tempera-
tures of pyrolysis IR range 400-800 °C. 
The diffraction patterns of all the samples in the 
range of angles 15°-30° fixed amorphous halo, charac-
teristic not strong structured  carbon structures. The 
amorphous halo on radiographs is associated with ir-
regular displacement of graphene planes relative to 
each other and the small size of the coherent scattering 
crystallite graphite-like phase [10]. At higher pyrolysis 
temperatures the formation of ordered carbon struc-
tures  occurs and at T  800 °C reflection peak corre-
sponding graphite-like carbon phase, the lattice con-
stant of which coincides with a lattice constant of 
graphite, detected at the diffraction pattern (Fig. 2). 
Also the diffraction nanocomposites of scattering 
angles 2θ of 55° to 101° there are several peaks , which 
correspond to the angles of reflection of the metal nick-
el phase (56°; 65.8°; 100.5°). 
As a result of TEM calculated distribution of metal 
nanoparticles in the size of the nanocomposite. The 
average size of the nanoparticles of the nanocomposite 
composition of nickel was 15-25 nm, depending on the  
 
 
Fig. 2 – Diffraction pattern of the nanocomposite Ni / C:  
1) 400 °C; 2) 500 °C; 3) 600 °C; 4) 700 °C; 5) 800 °C 
 
temperature of the process IR-pyrolysis of the precur-
sor. Thus, in the nanocomposites , the obtained at 
T  600 °C the average size of the nanoparticles was 
15 nm and at T  700 °C is advantageously fixed nano-
particles with an average size of 25 nm. The results are 
shown in Fig. 3. The distribution is in the nature dome-
shaped curve in mid-sized metal nanoparticles. With 
increasing temperature of obtain nanocomposites curve 
smeared and shifts to larger metal particles. 
 
 
 
 
 
Fig. 3 – The distribution of nanoparticles in size (a) nanocom-
posite Ni / C, 600 °C; (b) nanocomposite Ni / C, 700 °C; direct 
measurement of the photographs, obtained using TEM 
 
According to the atomic-absorption spectroscopy 
(AAC), the nickel content is nanocomposites ~ 15 wt. %, 
which differs from the originally introduced in the pre-
cursor (20 wt. %) and weakly dependent on the tempera-
ture of preparation. Apparently, the trend factor caused 
the formation of volatile metal compounds in the process 
of degradation of the polymer during the IR-heating.  
0
5
10
15
20
25
30
35
7 10 12 15 17 20 22 25
%
 
d, nm 
0
5
10
15
20
8 14 20 25 27 30 36 42
T
h
e
 s
h
a
re
 o
f 
n
a
n
o
p
a
rt
ic
le
s
,%
 
The size of the nanoparticles, nm 
a 
b 
 THE SYNTHESIS OF METALCARBON NANOCOMPOSITE NI / C… J. NANO- ELECTRON. PHYS. 5, 04007 (2013) 
 
 
04007-3 
 
 
Fig. 6 – The mass change with temperature infrared heating for 
samples: 1 – NiCl26H2O / PAN with CNi  10 wt. %; 2 – PAN 
 
 
 
 
 
Fig. 7 – The relationship between d / dt and IR-temperature 
heating: a) from 50 to 300 °C, b) from 300 to 550 °C for sam-
ples 1 – NiCl26H2O / PAN with SNi  10 wt. %; 2 – PAN 
Using thermogravimetric analysis and differential 
scanning calorimeter processes occurring during IR-
heating system NiCl26H2O / PAN have been studied. 
Fig. 6 shows the change of mass during IR-heating and 
differential curve (Fig. 7) for the system in 
NiCl26H2O / PAN compared with the PAN. 
 
Differentiation by the temperature allowed to de-
termine the stage and the temperature ranges for the 
thermal processes in the synthesis of nanocomposite 
Ni/C. According to [11] were calculated Ea and k0 for 
each step (see Table 2). 
 
Table 1 – Kinetic parameters of the formation of a nanocom-
posite Ni / C under the influence of IR-heating 
 
Composition  
sample 
Т, °С 
Ea,  
kJ/mol 
k0, min – 1 
NiCl2·6H2O/PAN 
 СNi  10 by mass. 
% 
85 153,2 1,4·1014 
165 126,0 1,9·109 
330 97,5 4,2·107 
410 17,9 3,2·107 
PAN 
180 140,2 2,9·1014 
300 100,8 4,2·108 
350 78,2 9,2·107 
430 27,7 4,2·107 
 
The peaks in the kinetic curves of the composite heat-
ing to 300 °C characterize processes of decomposition of 
the precursor. Differences in the position of the peaks may 
depend on the characteristics of chemical processes and 
the degree of drying of the composite. Kinetic curve heat-
ing to 300 °C composites NiCl26H2O / PAN includes peaks 
observed on the kinetic curve heating PAN – 180 and 
300 °C. Accordingly, the peaks at 165 °C are allocated to 
degradation processes PAN. The calculated activation 
energy for these processes indicates kinetic step 
(Ea  40 kJ/mol) as the limiting (Table 2). Accessory 
marked peaks in the processes of decomposition of compo-
site components NiCl26H2O / PAN confirm the results of 
DSC, where the peaks of the most significant changes in 
the thermal effects corresponding to the endothermic 
transition to coincide with peaks in the differential TGA 
curves (Fig. 8). 
 
 
 
Fig. 8 – Derivatives of conversion of raising the temperature 
d / dT(T) of composites NiCl26H2O / PAN (1) and the tem-
perature of the heat of reaction q(T) of composites 
NiCl26H2O / PAN (2) 
 
Comparison of dependences showed that the peaks 
in the kinetic curves composites heating to 250 °C, we 
can refer to the processes of dehydration NiCl26H2O 
and partial destruction of PAN to form a cyclic molecu-
lar structure . 
 
a 
b 
 L.V. KOZHITOV, D.G. MURATOV, E.V. YAKUSHKO, ET AL. J. NANO- ELECTRON. PHYS. 5, 04007 (2013) 
 
 
04007-4 
4. CONCLUSIONS 
 
Metalcarbon nanocomposites based PAN and nickel 
chloride hexahydrate were obtained under IR-heating. 
It is shown that in the system at temperatures IK-
PAN / NiCl2 IR-pyrolysis of 400-800 °C are formed 
nanocomposites consisting of a carbon matrix and me-
tallic nickel nanoparticles . 
According to the results of TGA and DSC nickel in 
the NiCl26H2O / PAN causes a decrease in the temper-
ature of the processes of chemical transformations of 
the polymer matrix, which contributes to the carboni-
zation process. The chemical transformation reactions 
the speed limits and not the diffusion of the compo-
nents. The average size of Ni nanoparticles tempera-
ture-dependent production and is 15-25 nm in the 
range 400-800 °C. Nanoparticle size distribution is 
asymmetrical nature curve whose maximum is in the 
average particle size with increasing temperature 
which the synthesis of nanocomposites is spread and 
shifts to larger nanoparticles. 
This work was supported by the grant of the Presi-
dent of the Russian Federation No МК-1366.2013.8 
and the grant of the President of the Russian Federa-
tion for young scientists and graduate students  
No СП-4341.2013.1. 
 
 
 REFERENCES 
 
1. A. Marangoni, M. Rogers, Appl. Phys. Lett. 82, 3239 
(2003). 
2. M.J.S. Dewar, J. Am. Chem. Soc. 99, 4899 (1977). 
3. M.J. S. Dewar, W. Thiel, Theor. Chem. Acc. 46, 89 (1977). 
4. V.V. Kozlov, G.P. Karpacheva, V.S. Petrov, 
E.V. Lazovskaya, Polym. Sci. Ser. A 43 No 1, 15 (2001). 
5. M.H. Xu, W. Zhong, X.S. Qi, C.T. Au, Y. Deng, J. Alloy. 
Compd. 495, 200 (2010). 
6. G. Carja, A. Nakajima, C. Dranca, K. Okada , 
J. Nanoparticle Res. 12 No 8, 3049 (2010). 
7. S.V. Gornostaeva, A.A. Revina, L.D. Belyakova, 
O.G. Larionov, J. Protection Metal. 44, 5, 533 (2008). 
8. D.G. Muratov, E.V. Yakushko, L.V. Kozhitov, 
A.V. Popkova, M.A. Pushkarev, J. Materials of Electronic 
Technics, 1 (2013). 
9. V.V. Kozlov, G.P. Karpacheva, V.S. Petrov, 
E.V. Lazovskaya, Polym. Sci. Ser. A 43 No 1, 15 (2001). 
10. D.G. Muratov, V.V. Kozlov, V.V. Krapukhin, 
L.V. Kozhitov, L.M. Zemcov, G.P. Karpachyova, J. Mater. 
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331 (Wiley: 1983). 
 


The Synthesis of Metalcarbon Nanocomposite Ni / C on the Basis of Polyacrylonitrile

Electronic Sumy State University Institutional Repository

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ Vol. 5 No 4, 04007(4pp) (2013) Том 5 № 4, 04007(4cc) (2013)   The article was reported at the International Conference «Physics and Technology of Nanomaterials and Structures», Kursk, 21-22 November, 2013 2077-6772/2013/5(4)04007(4) 04007-1  2013 Sumy State University The Synthesis of Metalcarbon Nanocomposite Ni / C on the Basis of Polyacrylonitrile  L.V. Kozhitov1, D.G. Muratov1,2, E.V. Yakushko1, S.L. Kozhitov1, A.G. Savchenko1, I.V. Shchetinin1,  S.G. Emelyanov3, L.M. Chervjakov3  1 National University of Science and Technology "MISIS", 4, Leninskii Pr., 119049 Moscow, Russia 2 Institute of Petrochemical Synthesis named A.V. Topchiev of the Russian Academy of Sciences,  119991 Moscow, Russia 3 Southwest State University, 94, 50 Let Oktyabrya Str., 305040 Kursk, Russia  (Received 05 August 2013; revised manuscript received 29 November 2013; published online 10 December 2013)  Metalcarbon nanocomposites based on polyacrylonitrile and nickel chloride are synthesized under the influence of infrared heat. The resulting materials represent a system of carbon matrix formed during the carbonization of PAN, and distributed in it nickel nanoparticles. The average size of the nanoparticles in the nanocomposite was 15-25 nm. It was found that the distribution of nickel nanoparticles sizes is deter-mined by temperature synthesis nanocomposite. Thus with increasing temperature, the predominant av-erage particle size of the metal increases, and the distribution is spread and shifted toward larger sizes.  Keywords: Metalcarbon nanocomposite, Carbon matrix, Nanoparticles of nickel.   PACS numbers: 61.48.De, 81. – b   1. INTRODUCTION  Currently functional nanomaterials are of great in-terest to researchers because of its unique properties, which manifest themselves in the nanostate. In the nanostate for the materials new opportunities are opened up in both the theoretical aspect and the exper-imental use. Special interest is composite nanomateri-als. The composite materials comprising nanoparticles 3d-metal (Fe, Co, Ni), and their oxides are of interest from the viewpoint of use as heterogeneous catalysts for petrochemical processes [1, 2], the growth of carbon nanotubes [3, 4], components of dispersed radar ab-sorbing media [5, 6, 7]. Currently, there are several groups of methods and approaches to the formation of nanomaterials including nano-sized metal particles. Regardless of the approach, the controlled synthesis of nanoparticles with a narrow size distribution and well-defined structure is one of the main problems. The aim of this work is to obtain the metalcarbon nanocomposites based in polyacrylonitrile under IR-heating including nickel nanoparticles dispersed in the carbon matrix, and the study of the structural charac-teristics of the synthesized material.  2. EXPERIMENTAL  Metalcarbon nanocomposite are obtained by IR an-nealing of polyacrylonitrile (PAN) and NiCl26H2O. Precursors nanocomposites were prepared by co-dissolving PAN and NiCl26H2O in dimethylformamide (DMF, Fluka, 99.5 %) followed by removal of solvent. The concentration of PAN in DMF solution was 5 wt %. And nickel – 30 % by mass. Re calculation for chloride hexahydrate. Pyrolysis was carried out in the IR-camera of pulse photon annealing installation. IR-annealing was done in a two steps operation: preliminary annealing in air at 150 °C and 200 °C for 15 min, during which the sol-vent is removed and PAN original structuring per-formed, and basic annealing in an inert atmosphere at a desired intensity of infrared radiation that heats the sample to a temperature in the range 400-700 °C. The holding time at the final temperature was 120 s. The heating temperature of the sample was fixed with the chromel-alumel thermocouple. Calorimetric study carried out on a differential scanning calorimeter (DSC) Q20 (TA Instruments, USA) at a heating rate 10 °C/min in a range of 50-350 °C. Measurements were performed in a nitrogen flow of 50 ml/min. Pattern in the form of powder was placed in a platinum crucible is sealed. Thermogravimetric analysis (TGA) was performed using a thermogravimetric analyzer Discovery TG TM (TA Instruments, USA) in the temperature range 50-700 °C at a heating rate of 10 °C/min under nitrogen flow rate of 50 ml/min. The furnace unit is equipped with four heating elements operating in the infrared range, which are heated chamber of SiC, in which there is a pattern in the form of a powder, placed in a plati-num crucible. Weighing accuracy of the instrument is ± 0,1 %, the reproducibility of the weighing - ± 0,01 %. The sensitivity of the scale –  7.10 g. Temperature accuracy – ± 1 °C. TGA was carried out in the temperature range from 50 to 700 °C at a heating rate of 10 °C/min. Atomic  absorption spectroscopy (AAS) was performed on the spectrometer «AAS – 30». Micrographs of the samples obtained in a transmis-sion electron microscope LEO912 ABOMEGA, 60 - 120 kV accelerating voltage, increasing the 80-500000 h. Phase and structural studies were carried out at room temperature X-ray diffraction of the com-pany «Rigaku» Focusing on the Bragg-Brentano on CoK -radiation in a continuous mode. The experimental results were processed by methods of approximation.  3. RESULTS AND DISCUSSION  Using the previously developed methods [8] were obtained metalcarbon nanocomposites based on polyac-rylonitrile (PAN) and nickel chloride hexahydrate.  L.V. KOZHITOV, D.G. MURATOV, E.V. YAKUSHKO, ET AL. J. NANO- ELECTRON. PHYS. 5, 04007 (2013)   04007-2 Formation of metalcarbon nanocomposite precur-sors are in situ. Uniform distribution of the metal in the polymer matrix during the synthesis of the precur-sor is achieved by processes complexation between ni-trile groups of the polymer and the metal compound . In the pyrolysis of PAN is an allocation of a variety of gaseous products [9], among which there are hydrogen , CO, NH3, and that reduced nickel chloride. Due to the processes of structural and chemical transformations in the matrix of PAN and coagulation of clusters of re-duced metal nanoparticles are formed . Application of electron microscopy was used to estab-lish the structure and morphology nanocomposite Ni / C. Fig. 1 shows the results of transmission electron micros-copy (TEM) nanocomposite Ni/C, obtained at 700 °C.    Fig. 1 – TEM of the Ni / C nanocomposite, obtained at 700 °C (Ni / C 700)  Light grey color - the polymer substrate used in the analysis by TEM. Carbon graphite-matrix nanocompo-sites - dark gray color, which is a layered disordered system with the size of the coherent scattering crystal-lites Lc from 18 to 37 Å. Studying the structure of the carbon matrix based on PAN was carried out in [10]. Quite dark, black spherical formations - nanoparticles of nickel. Fig. 2 shows the diffraction pattern of nickel- con-taining nanocomposites obtained at different tempera-tures of pyrolysis IR range 400-800 °C. The diffraction patterns of all the samples in the range of angles 15°-30° fixed amorphous halo, charac-teristic not strong structured  carbon structures. The amorphous halo on radiographs is associated with ir-regular displacement of graphene planes relative to each other and the small size of the coherent scattering crystallite graphite-like phase [10]. At higher pyrolysis temperatures the formation of ordered carbon struc-tures  occurs and at T  800 °C reflection peak corre-sponding graphite-like carbon phase, the lattice con-stant of which coincides with a lattice constant of graphite, detected at the diffraction pattern (Fig. 2). Also the diffraction nanocomposites of scattering angles 2θ of 55° to 101° there are several peaks , which correspond to the angles of reflection of the metal nick-el phase (56°; 65.8°; 100.5°). As a result of TEM calculated distribution of metal nanoparticles in the size of the nanocomposite. The average size of the nanoparticles of the nanocomposite composition of nickel was 15-25 nm, depending on the    Fig. 2 – Diffraction pattern of the nanocomposite Ni / C:  1) 400 °C; 2) 500 °C; 3) 600 °C; 4) 700 °C; 5) 800 °C  temperature of the process IR-pyrolysis of the precur-sor. Thus, in the nanocomposites , the obtained at T  600 °C the average size of the nanoparticles was 15 nm and at T  700 °C is advantageously fixed nano-particles with an average size of 25 nm. The results are shown in Fig. 3. The distribution is in the nature dome-shaped curve in mid-sized metal nanoparticles. With increasing temperature of obtain nanocomposites curve smeared and shifts to larger metal particles.      Fig. 3 – The distribution of nanoparticles in size (a) nanocom-posite Ni / C, 600 °C; (b) nanocomposite Ni / C, 700 °C; direct measurement of the photographs, obtained using TEM  According to the atomic-absorption spectroscopy (AAC), the nickel content is nanocomposites ~ 15 wt. %, which differs from the originally introduced in the pre-cursor (20 wt. %) and weakly dependent on the tempera-ture of preparation. Apparently, the trend factor caused the formation of volatile metal compounds in the process of degradation of the polymer during the IR-heating.  051015202530357 10 12 15 17 20 22 25% d, nm 051015208 14 20 25 27 30 36 42The share of nanoparticles,% The size of the nanoparticles, nm a b  THE SYNTHESIS OF METALCARBON NANOCOMPOSITE NI / C… J. NANO- ELECTRON. PHYS. 5, 04007 (2013)   04007-3   Fig. 6 – The mass change with temperature infrared heating for samples: 1 – NiCl26H2O / PAN with CNi  10 wt. %; 2 – PAN      Fig. 7 – The relationship between d / dt and IR-temperature heating: a) from 50 to 300 °C, b) from 300 to 550 °C for sam-ples 1 – NiCl26H2O / PAN with SNi  10 wt. %; 2 – PAN Using thermogravimetric analysis and differential scanning calorimeter processes occurring during IR-heating system NiCl26H2O / PAN have been studied. Fig. 6 shows the change of mass during IR-heating and differential curve (Fig. 7) for the system in NiCl26H2O / PAN compared with the PAN.  Differentiation by the temperature allowed to de-termine the stage and the temperature ranges for the thermal processes in the synthesis of nanocomposite Ni/C. According to [11] were calculated Ea and k0 for each step (see Table 2).  Table 1 – Kinetic parameters of the formation of a nanocom-posite Ni / C under the influence of IR-heating  Composition  sample Т, °С Ea,  kJ/mol k0, min – 1 NiCl2·6H2O/PAN  СNi  10 by mass. % 85 153,2 1,4·1014 165 126,0 1,9·109 330 97,5 4,2·107 410 17,9 3,2·107 PAN 180 140,2 2,9·1014 300 100,8 4,2·108 350 78,2 9,2·107 430 27,7 4,2·107  The peaks in the kinetic curves of the composite heat-ing to 300 °C characterize processes of decomposition of the precursor. Differences in the position of the peaks may depend on the characteristics of chemical processes and the degree of drying of the composite. Kinetic curve heat-ing to 300 °C composites NiCl26H2O / PAN includes peaks observed on the kinetic curve heating PAN – 180 and 300 °C. Accordingly, the peaks at 165 °C are allocated to degradation processes PAN. The calculated activation energy for these processes indicates kinetic step (Ea  40 kJ/mol) as the limiting (Table 2). Accessory marked peaks in the processes of decomposition of compo-site components NiCl26H2O / PAN confirm the results of DSC, where the peaks of the most significant changes in the thermal effects corresponding to the endothermic transition to coincide with peaks in the differential TGA curves (Fig. 8).    Fig. 8 – Derivatives of conversion of raising the temperature d / dT(T) of composites NiCl26H2O / PAN (1) and the tem-perature of the heat of reaction q(T) of composites NiCl26H2O / PAN (2)  Comparison of dependences showed that the peaks in the kinetic curves composites heating to 250 °C, we can refer to the processes of dehydration NiCl26H2O and partial destruction of PAN to form a cyclic molecu-lar structure .  a b  L.V. KOZHITOV, D.G. MURATOV, E.V. YAKUSHKO, ET AL. J. NANO- ELECTRON. PHYS. 5, 04007 (2013)   04007-4 4. CONCLUSIONS  Metalcarbon nanocomposites based PAN and nickel chloride hexahydrate were obtained under IR-heating. It is shown that in the system at temperatures IK-PAN / NiCl2 IR-pyrolysis of 400-800 °C are formed nanocomposites consisting of a carbon matrix and me-tallic nickel nanoparticles . According to the results of TGA and DSC nickel in the NiCl26H2O / PAN causes a decrease in the temper-ature of the processes of chemical transformations of the polymer matrix, which contributes to the carboni-zation process. The chemical transformation reactions the speed limits and not the diffusion of the compo-nents. The average size of Ni nanoparticles tempera-ture-dependent production and is 15-25 nm in the range 400-800 °C. Nanoparticle size distribution is asymmetrical nature curve whose maximum is in the average particle size with increasing temperature which the synthesis of nanocomposites is spread and shifts to larger nanoparticles. This work was supported by the grant of the Presi-dent of the Russian Federation No МК-1366.2013.8 and the grant of the President of the Russian Federa-tion for young scientists and graduate students  No СП-4341.2013.1.    REFERENCES  1. A. Marangoni, M. Rogers, Appl. Phys. Lett. 82, 3239 (2003). 2. M.J.S. Dewar, J. Am. Chem. Soc. 99, 4899 (1977). 3. M.J. S. Dewar, W. Thiel, Theor. Chem. Acc. 46, 89 (1977). 4. V.V. Kozlov, G.P. Karpacheva, V.S. Petrov, E.V. Lazovskaya, Polym. Sci. Ser. A 43 No 1, 15 (2001). 5. M.H. Xu, W. Zhong, X.S. Qi, C.T. Au, Y. Deng, J. Alloy. Compd. 495, 200 (2010). 6. G. Carja, A. Nakajima, C. Dranca, K. Okada , J. Nanoparticle Res. 12 No 8, 3049 (2010). 7. S.V. Gornostaeva, A.A. Revina, L.D. Belyakova, O.G. Larionov, J. Protection Metal. 44, 5, 533 (2008). 8. D.G. Muratov, E.V. Yakushko, L.V. Kozhitov, A.V. Popkova, M.A. Pushkarev, J. Materials of Electronic Technics, 1 (2013). 9. V.V. Kozlov, G.P. Karpacheva, V.S. Petrov, E.V. Lazovskaya, Polym. Sci. Ser. 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The Synthesis of Metalcarbon Nanocomposite Ni / C on the Basis of Polyacrylonitrile

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