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

Harseev, V.A.

Kozhitov, L.V.

Kozhitov, S.L.

Kuzmenko, A.P.

Matveev, K.E.

Muratov, D.G.

Popkova, A.V.

Rodionov, V.V.

Yakushko, E.V.

Electronic Sumy State University Institutional Repository

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ Vol. 5 No 4, 04008(3pp) (2013) Том 5 № 4, 04008(3cc) (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)04008(3) 04008-1  2013 Sumy State University Influence of the Ratio of Metal Composed Nanocomposites Fe-Co / C on Phase Composition  L.V. Kozhitov1, A.P. Kuzmenko2, S.L. Kozhitov1, D.G. Muratov1, 3, V.A. Harseev2, V.V. Rodionov2, A.V. Popkova1, K.E. Matveev1, E.V. Yakushko1  1 National Research Technological University "MISIS", 4, Leninsky Prospect, 119049 Moscow, Russia 2 Southwest State University, 94, 50 Let October Str., 305040 Kursk, Russia 3 Institute of Petrochemical Synthesis named A.V. Topchiev of the Russian Academy of Sciences,  29, Leninsky Prospect, 119991 Moscow, Russia  (Received 05 August 2013; revised manuscript received 29 December 2013; published online 10 December 2013)  It is found that the chemical composition of the metal component of nanocomposites satisfies the Fe: Co ratio, that was set on at the stage of preparation of the precursor, wherein there is a slight deviation from the initial metal concentration, due, apparently, to removing metal from the nanocomposite by the for-mation of volatile carbonyls of iron and cobalt in IR heating.  Keywords: Metal-carbon nanocomposites, Nanoparticles FeCo, IR-pyrolisis, PAN.  PACS number: 62.20.F. –   1. INTRODUCTION  Significant interest in nano-structured material for this including in the structure of ferromagnetic nano-particles of metals and alloys caused by specific mag-netic properties, manifested in the nano state: high magnetization and coercivity, the lower the Curie tem-perature, high anisotropy, etc. These materials may find use in magnetic recording systems, high frequency devices MRI and Biomedicine, protection systems elec-tromagnetic radiation. [1]. Additional ferromagnetic alloys FeCo-allocated nanoscale structures as have one of the highest values of magnetization, wherein the magnetic properties are strongly dependent on the composition and dispersion of the alloy. A number of studies [2, 3] demonstrated the effectiveness of the use of nanoparticles in FeCo absorbers of electromagnetic waves in the range of 4-18 GHz. There are several dif-ferent approaches to the synthesis of nanoparticles FeCo. Features of methods is the most significant quantity of the synthetic steps, the need for stabiliza-tion using surfactants, additional recovery step in a hydrogen atmosphere, a significant duration processes. One solution is the inclusion of nanoparticles in the composites [4-5]. This allows controlling the size of the nanoparticles improve chemical stability, reduce the density and weight of the composite coating. The developed methodology allows us to synthesize FeCo nanoparticles composed of metal-carbon nano-composites in one step by the IR - heating, ie in the same process at the same time forming a carbon nano-composite and nanostructured matrix is the formation of alloy nanoparticles FeCo.  2. EXPERIMENTAL SECTION  Polyacrylonitrile (PAN) was synthesized in the presence of a redox catalyst system. Film precursor composition was obtained from the combined solution in DMF (Fluka, 99.5 %) of PAS, iron acetylacetonate hydrate (III) (Acros Organics, 99 %) or ferrocene (Acros Organics, 99 %) and cobalt acetate (II) (Acros Organics, 99 %) followed by removal of solvent at T ≤ 70 C. The concentration of PAN in DMF solution was 5 wt. %. The total concentration of metals in the precursor 20  wt. % by weight of PAN metal ratio Fe: Co  1:1, 1:3, 3:1, by weight. Pyrolysis was carried out in a laboratory furnace of IR-heating [6]. The precursors was heated at 150 and 200 C for 15 min. at each temperature. This processing is necessary to remove the solvent bound with the polymer and the initialisation of process struc-turing of PAN. The samples were heated to the desired temperature of the main infrared pyrolysis process, which was 300-800 C, the time exposure at the  required temperature of infrared heating time was 2-10 min. The process was carried out in vacuum (P ~ 10 – 2-10 – 3 mm Hg). X-ray diffraction analysis was performed on the  X-ray powder diffractometer EMMA, equipped with a high voltage generator type IGBT, midrange output of 3 kW (60 kV / 80 mA) with high stability of ± 0.005 %. In most diffractometer uses standard Proven anode  X-ray tube ( anti-cathode ) of copper with low power 2.2 kW. Focal spot size – 0.4  12 mm. As a device for recording the scattered X-radiation detector is used Xe proportional detector for focusing geometry with a graphite monochromator. Reflexes are recorded using a goniometer radius of 180-250 mm with a range of changes 2θ: – 30-160° with a minimum step on each axis – 0.002. Software VisualXRD, Traces v.6, Siro-quant provides automated control at all stages of the measurements. In addition, there is an automated da-tabase containing 250,000 records for the automatic identification of the diffraction patterns obtained, it is even more facilitated the implementation of the totality of the planned research. The surface morphology and composition of the samples were determined using a scanning electron microscope (SEM) JEOL JSM6610LV (W-cathode). De-tectors of secondary and backscattered electrons can allow to register the signals in the different mods: com-posite, topographical and shadow contrasts; the energy dispersive analyzer (X-Max Silicon Drift Detector Ox-ford Instruments) is used for elemental analysis of the surface layer. Two modes: high and low vacuum SEM, the application of conductive films of platinum (JEOL   L.V. KOZHITOV, A.P. KUZMENKO, S.L. KOZHITOV, ET AL. J. NANO- ELECTRON. PHYS. 5, 04008 (2013)   04008-2  700600500400300200100* data - backg round16001400120010008006004002000030- 65-4131 -Cobalt Iron010- 76-6587 -Ir on10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0 700600500400300200100* data - backg round* peaks10008006004002000030-65-4131 -Cobalt Iron010-76-6587 -Iron10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.01000800600400200* data - background10008006004002000030-65-4131 -Cobalt Iron010-76-6587 -Iron10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0  Fig. 1 – X-ray analysis of nanocomposite FeCo / С (Fe:Co  1:1), synthesized at differents temperatures:  600 °C (a), 700 °C (b), 800 °C (с)  JFC- 1600 Auto Fine Coater) can acquire images at an accelerating voltage of 300 V to 30 kV magnification range 5÷300,000 times the spatial increase to 3 nm regardless of sample conductivity. Metal-carbon nanocomposites were prepared based on polyacrylonitrile (PAN) and the compounds of Fe and Co. By results of X-ray analysis it was established that nanocomposites are homogeneous material, wherein the nanoparticle metal (Fe, Co) or FeCo-alloys are dis-tributed in the graphitelike carbon  matrix. Fig. 1 shows the result of X-ray analysis of nanocomposites obtained at T  600-800 C (Fe: Co  1:1).  Amorphous halo, which characteristic for weakly or-dered carbon structures, is fixed on the of all the samples in the range of angles 20°-30°. The amorphous halo on X-ray diffraction patterns is associated with irregular dis-placement of graphene planes relative to each other and the small size of the coherent dispersion of crystallite of graphitelike phase [6]. During process of IR-pyrolysis of polymer are secreted significant amounts of various gas-eous products (H2, NH3, CO etc.), which can recover metal from their compounds [7]. It should be noted that the recovery takes place in the solid polymer phase, so that the recovery of the metal occurs in situ, where atomic hydrogen which is generated due to degradation of the polymer backbone during the IR heating can par-ticipate in the recovery process. The diffractograms of nanocomposites, synthesized at temperatures 600-800 °C, is contain several maxima (45; 65,5°) corresponding to angles of reflection from the FeCo phase in the range of scattering angles 2θ from 50° to 80°. Reflexes phase fcc-Co is very weak at large angles, which also confirms the formation of the alloy FeCo, having the bcc lattice. The intensity of  these reflections is increased, which indicates an in-crease in the size of alloy nanoparticles with increasing temperature synthesis of nanocomposites. Simultaneous-ly, there is an increase in the intensity of the halo (2θ from 20° to 30°) and the displacement of its maximum in the region of large angles, which is associated with the processes of graphitization and the formation of graphitelike structure with a larger size of crystallites. When used other ratio of metal-containing components (Fe: Co  1:3) for the synthesis of nanocomposites, the material, having a different composition of the phases, are formed. On the diffraction patterns for samples, synthe-sized for Т  600-800 °С, along with the phase of the alloy FeCo the reflexes of phase fcc-cobalt are clearly recorded (2θ  44, 51.3). Fig. 2 shows XRD-pattern nanocomposite FeCo / C (Fe: Co  1:3), synthesized at T  800 C. Apparently, the formation of intermetallic nanopar-ticles occurs in several stages: first, there is a restora-tion of cobalt acetate and nanoparticles are formed. Then the iron is reduced and reacted with nanoparti-cles Co, dissolved in they. In result, solid solution of Fe     Fig. 2 – X-ray analysis of nanocomposite FeCo / С (Fe : Co  1:3), synthesized at T  700 °C a b c  INFLUENCE OF THE RATIO OF METAL COMPOSED NANOCOMPOSITES… J. NANO- ELECTRON. PHYS. 5, 04008 (2013)   04008-3 in Co is formed. This is supported by the fact that ac-cording to the thermodynamics, the temperature of reduce of cobalt compounds by hydrogen is substantial-ly lower (~ 200 °C), than for iron (~ 400 °C). Because of an excess content of cobalt the nanoparticles are formed to fcc-phase, which do not react with iron or solid solution Fe in Co is formed in with concentration less than 10 %, which also has an fcc-lattice.       Fig. 3 – SEM nanocomposite FeCo / C synthesized at T  700 °C (a) and 800 °C (b), and the results of energy-dispersive analysis (c) Table 1 – The results of the chemical analysis of nanocompo-sites FeCo / C  Ratio  Fe:Co Temperature of synthesis, °С Content, wt.% C Fe Co 1:1 600 82,3 8,4 9,3 700 82,7 7,9 9,3 800 82,3 8,6 9,1 1:3 600 83,9 3,8 12,3 800 79,9 4,7 15,4  The results of the SEM with using the console of  X-ray dispersion chemical analysis are supports this assumption, because the ratio Fe:Co is remains practi-cally unchanged in all samples and corresponds to the original, i.e. the loss of metals during the IR processing of the precursor are comparable. SEM results of nano-composite FeCo/C (1:1), obtained at T  800 °C, are shown in Fig. 3. The summarized results of the chemical analysis of nanocomposites of Fe: Co  1:1 and 1:3 were obtained under different conditions are presented Table 1. For all samples, the ratio of Fe: Co slightly different from the original. Differences may be due to the differ-ence in temperature of reduce of the metal. Also, a slight reduction of the total concentration of the metal observed with increasing temperature synthesis of nano-composites. apparently, during the synthesis process volatile carbonyls of iron and cobalt are formed, which are released into a gas phase and pumped by a vacuum system of IR heating apparatus. As a result,  a metal-carbon nanocomposite are formed, where in the metal content by a few percent lower than the original. After forming the metal nanoparticles or alloy this pro-cess has little effect on the chemical composition of the resulting material.  3. CONCLUSIONS  Nanoparticles of alloy of FeCo were obtained in the metal-carbon nanocomposites based on polyacrylonitrile under IR - heating. It was found that the initial ratio of metal introduced into the precursor affects the phase composition of the nanocomposite. It is shown that in-creasing the temperature of synthesis result increases the size of FeCo alloy nanoparticles, thus there increases the size of the crystallites of the graphitelike matrix of nanocomposites. Chemical composition of the nanocom-posite weakly dependent on synthesis temperature and determined by the initial metal ratio. 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 Federation for young scientists and graduate students No СП-4341.2013.1.  REFERENCES  1. Y. Yang, C. Xu, Y. Xia, T. Wang, F. Li, J. Alloy. Comp. 493, 549 (2010). 2. Y. Yang, C.L. Xu, Y.X. Xia, T. Wang, F.S. Li, J. Alloy. Compd. 493, 549 (2010). 3. C. Wang, R. Lv, F. Kang, J. Gu, X. Gui, D. Wu J. Magn. Magn. Mater. 321, 1924 (2009). 4. Xu.W. Zhong, Z.H. Wang, C. Au, et. al, Physica E 52, 14 (2013). 5. C. Wang, R. Lv, Z. Huang, F. Kang, J. Gu. J. Alloy. Comp. 509, 494 (2011). 6. D.G. Muratov, V.V. Kozlov, V.V. Krapukhin,  7. L.V. Kozhitov, L.M. Zemcov, G.P. Karpacheva, Proc. of Inst. of High. Ed. Mater. Electronics 3, 26 (2007). 8. V.V. Kozlov, G.P. Karpacheva, V.S. Petrov, E.V. Lazovskaya, Polym. Sci. Ser. A 43 No 1, 20 (2001). a b c 

Influence of the Ratio of Metal Composed Nanocomposites Fe-Co / C on Phase Composition

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 5 No 4, 04008(3pp) (2013) Том 5 № 4, 04008(3cc) (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)04008(3) 04008-1  2013 Sumy State University 
Influence of the Ratio of Metal Composed Nanocomposites Fe-Co / C on Phase Composition 
 
L.V. Kozhitov1, A.P. Kuzmenko2, S.L. Kozhitov1, D.G. Muratov1, 3, V.A. Harseev2, V.V. Rodionov2, 
A.V. Popkova1, K.E. Matveev1, E.V. Yakushko1 
 
1 National Research Technological University "MISIS", 4, Leninsky Prospect, 119049 Moscow, Russia 
2 Southwest State University, 94, 50 Let October Str., 305040 Kursk, Russia 
3 Institute of Petrochemical Synthesis named A.V. Topchiev of the Russian Academy of Sciences,  
29, Leninsky Prospect, 119991 Moscow, Russia 
 
(Received 05 August 2013; revised manuscript received 29 December 2013; published online 10 December 2013) 
 
It is found that the chemical composition of the metal component of nanocomposites satisfies the Fe: Co 
ratio, that was set on at the stage of preparation of the precursor, wherein there is a slight deviation from 
the initial metal concentration, due, apparently, to removing metal from the nanocomposite by the for-
mation of volatile carbonyls of iron and cobalt in IR heating. 
 
Keywords: Metal-carbon nanocomposites, Nanoparticles FeCo, IR-pyrolisis, PAN. 
 
PACS number: 62.20.F. – 
 
 
1. INTRODUCTION 
 
Significant interest in nano-structured material for 
this including in the structure of ferromagnetic nano-
particles of metals and alloys caused by specific mag-
netic properties, manifested in the nano state: high 
magnetization and coercivity, the lower the Curie tem-
perature, high anisotropy, etc. These materials may 
find use in magnetic recording systems, high frequency 
devices MRI and Biomedicine, protection systems elec-
tromagnetic radiation. [1]. Additional ferromagnetic 
alloys FeCo-allocated nanoscale structures as have one 
of the highest values of magnetization, wherein the 
magnetic properties are strongly dependent on the 
composition and dispersion of the alloy. A number of 
studies [2, 3] demonstrated the effectiveness of the use 
of nanoparticles in FeCo absorbers of electromagnetic 
waves in the range of 4-18 GHz. There are several dif-
ferent approaches to the synthesis of nanoparticles 
FeCo. Features of methods is the most significant 
quantity of the synthetic steps, the need for stabiliza-
tion using surfactants, additional recovery step in a 
hydrogen atmosphere, a significant duration processes. 
One solution is the inclusion of nanoparticles in the 
composites [4-5]. This allows controlling the size of the 
nanoparticles improve chemical stability, reduce the 
density and weight of the composite coating. 
The developed methodology allows us to synthesize 
FeCo nanoparticles composed of metal-carbon nano-
composites in one step by the IR - heating, ie in the 
same process at the same time forming a carbon nano-
composite and nanostructured matrix is the formation 
of alloy nanoparticles FeCo. 
 
2. EXPERIMENTAL SECTION 
 
Polyacrylonitrile (PAN) was synthesized in the 
presence of a redox catalyst system. Film precursor 
composition was obtained from the combined solution 
in DMF (Fluka, 99.5 %) of PAS, iron acetylacetonate 
hydrate (III) (Acros Organics, 99 %) or ferrocene (Acros 
Organics, 99 %) and cobalt acetate (II) (Acros Organics, 
99 %) followed by removal of solvent at T ≤ 70 C. The 
concentration of PAN in DMF solution was 5 wt. %. 
The total concentration of metals in the precursor 20  
wt. % by weight of PAN metal ratio Fe: Co  1:1, 1:3, 
3:1, by weight. Pyrolysis was carried out in a laboratory 
furnace of IR-heating [6]. The precursors was heated at 
150 and 200 C for 15 min. at each temperature. This 
processing is necessary to remove the solvent bound 
with the polymer and the initialisation of process struc-
turing of PAN. The samples were heated to the desired 
temperature of the main infrared pyrolysis process, 
which was 300-800 C, the time exposure at the  
required temperature of infrared heating time was 2-
10 min. The process was carried out in vacuum 
(P ~ 10 – 2-10 – 3 mm Hg). 
X-ray diffraction analysis was performed on the  
X-ray powder diffractometer EMMA, equipped with a 
high voltage generator type IGBT, midrange output of 
3 kW (60 kV / 80 mA) with high stability of ± 0.005 %. 
In most diffractometer uses standard Proven anode  
X-ray tube ( anti-cathode ) of copper with low power 
2.2 kW. Focal spot size – 0.4  12 mm. As a device for 
recording the scattered X-radiation detector is used Xe 
proportional detector for focusing geometry with a 
graphite monochromator. Reflexes are recorded using a 
goniometer radius of 180-250 mm with a range of 
changes 2θ: – 30-160° with a minimum step on each 
axis – 0.002. Software VisualXRD, Traces v.6, Siro-
quant provides automated control at all stages of the 
measurements. In addition, there is an automated da-
tabase containing 250,000 records for the automatic 
identification of the diffraction patterns obtained, it is 
even more facilitated the implementation of the totality 
of the planned research. 
The surface morphology and composition of the 
samples were determined using a scanning electron 
microscope (SEM) JEOL JSM6610LV (W-cathode). De-
tectors of secondary and backscattered electrons can 
allow to register the signals in the different mods: com-
posite, topographical and shadow contrasts; the energy 
dispersive analyzer (X-Max Silicon Drift Detector Ox-
ford Instruments) is used for elemental analysis of the 
surface layer. Two modes: high and low vacuum SEM, 
the application of conductive films of platinum (JEOL  
 L.V. KOZHITOV, A.P. KUZMENKO, S.L. KOZHITOV, ET AL. J. NANO- ELECTRON. PHYS. 5, 04008 (2013) 
 
 
04008-2 
 
700
600
500
400
300
200
100
*
 data - backg round
1600
1400
1200
1000
800
600
400
200
0
030- 65-4131 -Cobalt Iron
010- 76-6587 -Ir on
10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0
 
700
600
500
400
300
200
100
*
 data - backg round
*
 peaks
1000
800
600
400
200
0
030-65-4131 -Cobalt Iron
010-76-6587 -Iron
10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0
1000
800
600
400
200
*
 data - background
1000
800
600
400
200
0
030-65-4131 -Cobalt Iron
010-76-6587 -Iron
10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0
 
 
Fig. 1 – X-ray analysis of nanocomposite FeCo / С 
(Fe:Co  1:1), synthesized at differents temperatures:  
600 °C (a), 700 °C (b), 800 °C (с) 
 
JFC- 1600 Auto Fine Coater) can acquire images at 
an accelerating voltage of 300 V to 30 kV magnification 
range 5÷300,000 times the spatial increase to 3 nm 
regardless of sample conductivity. 
Metal-carbon nanocomposites were prepared based 
on polyacrylonitrile (PAN) and the compounds of Fe 
and Co. By results of X-ray analysis it was established 
that nanocomposites are homogeneous material, wherein 
the nanoparticle metal (Fe, Co) or FeCo-alloys are dis-
tributed in the graphitelike carbon  matrix. Fig. 1 shows 
the result of X-ray analysis of nanocomposites obtained 
at T  600-800 C (Fe: Co  1:1).  
Amorphous halo, which characteristic for weakly or-
dered carbon structures, is fixed on the of all the samples 
in the range of angles 20°-30°. The amorphous halo on X-
ray diffraction patterns is associated with irregular dis-
placement of graphene planes relative to each other and 
the small size of the coherent dispersion of crystallite of 
graphitelike phase [6]. During process of IR-pyrolysis of 
polymer are secreted significant amounts of various gas-
eous products (H2, NH3, CO etc.), which can recover 
metal from their compounds [7]. It should be noted that 
the recovery takes place in the solid polymer phase, so 
that the recovery of the metal occurs in situ, where 
atomic hydrogen which is generated due to degradation 
of the polymer backbone during the IR heating can par-
ticipate in the recovery process. 
The diffractograms of nanocomposites, synthesized 
at temperatures 600-800 °C, is contain several maxima 
(45; 65,5°) corresponding to angles of reflection from 
the FeCo phase in the range of scattering angles 2θ 
from 50° to 80°. Reflexes phase fcc-Co is very weak at 
large angles, which also confirms the formation of the 
alloy FeCo, having the bcc lattice. The intensity of  
these reflections is increased, which indicates an in-
crease in the size of alloy nanoparticles with increasing 
temperature synthesis of nanocomposites. Simultaneous-
ly, there is an increase in the intensity of the halo (2θ 
from 20° to 30°) and the displacement of its maximum in 
the region of large angles, which is associated with the 
processes of graphitization and the formation of 
graphitelike structure with a larger size of crystallites. 
When used other ratio of metal-containing components 
(Fe: Co  1:3) for the synthesis of nanocomposites, the 
material, having a different composition of the phases, are 
formed. On the diffraction patterns for samples, synthe-
sized for Т  600-800 °С, along with the phase of the alloy 
FeCo the reflexes of phase fcc-cobalt are clearly recorded 
(2θ  44, 51.3). Fig. 2 shows XRD-pattern nanocomposite 
FeCo / C (Fe: Co  1:3), synthesized at T  800 C. 
Apparently, the formation of intermetallic nanopar-
ticles occurs in several stages: first, there is a restora-
tion of cobalt acetate and nanoparticles are formed. 
Then the iron is reduced and reacted with nanoparti-
cles Co, dissolved in they. In result, solid solution of Fe  
 
 
 
Fig. 2 – X-ray analysis of nanocomposite FeCo / С 
(Fe : Co  1:3), synthesized at T  700 °C 
a 
b 
c 
 INFLUENCE OF THE RATIO OF METAL COMPOSED NANOCOMPOSITES… J. NANO- ELECTRON. PHYS. 5, 04008 (2013) 
 
 
04008-3 
in Co is formed. This is supported by the fact that ac-
cording to the thermodynamics, the temperature of 
reduce of cobalt compounds by hydrogen is substantial-
ly lower (~ 200 °C), than for iron (~ 400 °C). Because of 
an excess content of cobalt the nanoparticles are 
formed to fcc-phase, which do not react with iron or 
solid solution Fe in Co is formed in with concentration 
less than 10 %, which also has an fcc-lattice. 
 
 
 
 
 
 
Fig. 3 – SEM nanocomposite FeCo / C synthesized at 
T  700 °C (a) and 800 °C (b), and the results of energy-
dispersive analysis (c) 
Table 1 – The results of the chemical analysis of nanocompo-
sites FeCo / C 
 
Ratio  
Fe:Co 
Temperature of 
synthesis, °С 
Content, wt.% 
C Fe Co 
1:1 
600 82,3 8,4 9,3 
700 82,7 7,9 9,3 
800 82,3 8,6 9,1 
1:3 
600 83,9 3,8 12,3 
800 79,9 4,7 15,4 
 
The results of the SEM with using the console of  
X-ray dispersion chemical analysis are supports this 
assumption, because the ratio Fe:Co is remains practi-
cally unchanged in all samples and corresponds to the 
original, i.e. the loss of metals during the IR processing 
of the precursor are comparable. SEM results of nano-
composite FeCo/C (1:1), obtained at T  800 °C, are 
shown in Fig. 3. 
The summarized results of the chemical analysis of 
nanocomposites of Fe: Co  1:1 and 1:3 were obtained 
under different conditions are presented Table 1. 
For all samples, the ratio of Fe: Co slightly different 
from the original. Differences may be due to the differ-
ence in temperature of reduce of the metal. Also, a slight 
reduction of the total concentration of the metal observed 
with increasing temperature synthesis of nano-
composites. apparently, during the synthesis process 
volatile carbonyls of iron and cobalt are formed, which 
are released into a gas phase and pumped by a vacuum 
system of IR heating apparatus. As a result,  
a metal-carbon nanocomposite are formed, where in the 
metal content by a few percent lower than the original. 
After forming the metal nanoparticles or alloy this pro-
cess has little effect on the chemical composition of the 
resulting material. 
 
3. CONCLUSIONS 
 
Nanoparticles of alloy of FeCo were obtained in the 
metal-carbon nanocomposites based on polyacrylonitrile 
under IR - heating. It was found that the initial ratio of 
metal introduced into the precursor affects the phase 
composition of the nanocomposite. It is shown that in-
creasing the temperature of synthesis result increases 
the size of FeCo alloy nanoparticles, thus there increases 
the size of the crystallites of the graphitelike matrix of 
nanocomposites. Chemical composition of the nanocom-
posite weakly dependent on synthesis temperature and 
determined by the initial metal ratio. 
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 Federation for 
young scientists and graduate students No СП-
4341.2013.1.
 
 
REFERENCES 
 
1. Y. Yang, C. Xu, Y. Xia, T. Wang, F. Li, J. Alloy. Comp. 493, 
549 (2010). 
2. Y. Yang, C.L. Xu, Y.X. Xia, T. Wang, F.S. Li, J. Alloy. Compd. 
493, 549 (2010). 
3. C. Wang, R. Lv, F. Kang, J. Gu, X. Gui, D. Wu J. Magn. 
Magn. Mater. 321, 1924 (2009). 
4. Xu.W. Zhong, Z.H. Wang, C. Au, et. al, Physica E 52, 14 (2013). 
5. C. Wang, R. Lv, Z. Huang, F. Kang, J. Gu. J. Alloy. Comp. 
509, 494 (2011). 
6. D.G. Muratov, V.V. Kozlov, V.V. Krapukhin,  
7. L.V. Kozhitov, L.M. Zemcov, G.P. Karpacheva, Proc. of Inst. of 
High. Ed. Mater. Electronics 3, 26 (2007). 
8. V.V. Kozlov, G.P. Karpacheva, V.S. Petrov, E.V. Lazovskaya, 
Polym. Sci. Ser. A 43 No 1, 20 (2001). 
a 
b 
c 


http://www.redalyc.org/pdf/398/39800504.pdf

Influence of the Ratio of Metal Composed Nanocomposites Fe-Co / C on Phase Composition

Abstract

Similar works

Full text

Available Versions

Electronic Sumy State University Institutional Repository

SocioEconomic Challenges Journal (Sumy State University)