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Original Russian Text © G.Yu. Yurkov, A.S. Fionov, Yu.A. Koksharov, V.V. Kolesov, S.P. Gubin, 2007, published in Neorganicheskie Materialy, 2007, Vol. 43, No. 8, pp. 936–947.
e-mail: gy-yurkov@mail.ru
Received December 25, 2006
834
ELECTRICAL AND MAGNETIC PROPERTIES OF NANOMATERIALS CONTAINING IRON 835
Fe3ë(102)
Fe3ë(002)
(a) (b)
Fe3O4(311)
Fe3ë(201)
Fe3ë(211)
Fe3O4(220)
Fe3ë(210)
Fe3ë(112) Fe3ë(131)
Fe3ë(121)
Fe(110)
Fe3ë(122)
Fe3ë(040)
Fe3ë(221)
Fe3O4(511)
Intensity
Fe3O4(440)
Fe3ë(133)
Fe3O4(533)
Fe(200)
Fe3ë(123)
30 40 50 60 70 80
100 nm 2θ, deg
Fe3O4(311)
(c) (d)
Fe3ë(211)
Fe3O4(440)
Fe(110)
Fe ë(031)
Fe3ë(102)
Fe3O4(220)
Fe3ë(201)
Fe3O4(511)
Fe3ë(112) 3
Fe3O4(422)
Fe3ë(112)
Fe3ë(040)
Fe3ë(221)
Intensity
Fe3O4(533)
Fe3ë(133)
Fe3ë(123)
Fe(200)
30 40 50 60 70 80
50 nm 2θ, deg
Fe3O4(311)
(e) (f)
Fe3O4(440)
Fe3O4(511)
Fe3O4(400)
Fe3O4(220)
Intensity
Fe3O4(422)
Fe3O4(533)
Fe2O3(311)
Fe2O3(113)
Fe2O3(024)
Fe3O4(620)
30 40 50 60 70 80
100 nm 2θ, deg
Fig. 4. (a, c, e, g, i) TEM micrographs and (b, d, f, h, j) XRD patterns of the nanocomposites studied: (a–h) iron-containing nano-
particles synthesized from (a–d) iron pentacarbonyl, (e, f) iron(III) formate, and (g, h) iron(II) oxalate; (i, j) cobalt-containing nano-
particles synthesized from cobalt(II) acetate. The composition of the nanoparticles was determined using ICDD PDF 1999 data.
Fe3O4(311)
Fe2O3(104)
(g) (h)
Fe3O4(400)
Fe2O3(024)
Fe2O3(113)
Intensity
Fe3O4(220)
Fe(110)
Fe3O4(422)
Fe2O3(110)
Fe3O4(511)
Fe2O3(300)
Fe3O4(440)
Fe2O3(1010)
Fe(200)
Fe3O4(533)
Fe(211)
30 40 50 60 70 80
100 nm 2θ, deg
CoO(200)
(i) (j)
CoO(111)
CoO(220)
Intensity
CoO(311)
Co(111)
CoO(222)
Co3O4(311)
Co3O4(400)
Co3O4(220)
Co3O4(331)
Co3O4(511)
Co3O4(440)
Co(200)
Co(222]
30 40 50 60 70 80
100 nm 2θ, deg
Fig. 4. (Contd.)
polyethylene matrix. The XRD pattern of sample 1 (JCPDS 85-1436), Fe3ë (JCPDS 85-1317), and Fe
(Fig. 4b) shows weak reflections attributable to Fe3O4 (JCPDS 85-1410). The reflections present in the XRD
pattern of sample 2 (Fig. 4d) correspond to Fe3O4
(JCPDS 85-1436), Fe3ë (JCPDS 85-1317), and ε-Fe
Particle–matrix Polymer chain
bonding (JCPDS 34-0529). Unfortunately, the major metal-con-
taining component of sample 1 cannot be identified
from XRD data. The relative intensities of the reflec-
tions from sample 2 suggest that the major iron-con-
taining component of this material is Fe3O4. The aver-
age size of the iron-containing nanoparticles in samples 1
and 2 is 4.9 and 5.1 nm, respectively, as determined by
TEM (Figs. 4a, 4c).
The XRD pattern of sample 3 (Fig. 4f), prepared
from iron(III) formate, Fe(HCOO)3, shows reflections
Structurally Structurally
uncompensated ordered core of the characteristic of Fe2O3 (JCPDS 86-0550) and Fe3O4
layer particle (JCPDS 85-1436). XRD intensities indicate that major
component of this sample is Fe3O4. The average nano-
Fig. 5. General model for the structure of the synthesized particle size in sample 3 is 11.5 nm, as determined by
nanoparticles. TEM (Fig. 4e).
The XRD data for sample 4 (Fig. 4h), synthesized There are also a number of weaker reflections attribut-
through thermal decomposition of iron(II) oxalate, able to metallic Co (JCPDS 15-0806) and ëÓ3é4
FeC2O4 · 2H2O, indicate the presence of Fe3O4 (JCPDS (JCPDS 78-1969). In sample 6, the average size of
85-1436), Fe2O3 (JCPDS 86-0550), and Fe (JCPDS 85- cobalt-containing nanoparticles is 8.3 nm (Fig. 4i), and
1410). The major component of sample 4 is probably the major component is CoO, as inferred from XRD
Fe3O4; the average nanoparticle size inferred from intensities. In an earlier study [43], nanoparticles with
TEM data is 2.4 nm (Fig. 4g). a similar composition were stabilized on the surface of
poly(tetrafluoroethylene) microgranules.
The XRD pattern of sample 5 (Fig. 4j), prepared
through thermal decomposition of cobalt(II) acetate, Characteristically, the XRD patterns of nanoparti-
shows strong reflections at 2θ = 36.5°, 42.35°, 61.55°, cles stabilized in polymer matrices show a small num-
73.8°, and 77.6°, attributable to CoO (JCPDS 78-0431). ber of reflections, which are broadened and occasion-
1.5 1013
1
1.4 2
3
1.3
Resistance, Ω
ρcomposite/ρPE
1.2 1012 1
2
3
1.1
1.0
0.9 1011
0 5 10 15 20 0 2 4 6 8 10
wt % filler Time, min
1015
1014
1014
ρV, Ω m
1013
1013
ρV, Ω m
1012
1012
1 1 4
2 2 5
1011 3 6
1011
0 5 10 15 20
wt % filler 101 102 103
Voltage, V
Fig. 8. Resistivity as a function of filler content for sam- Fig. 9. Resistivity as a function of applied voltage for (1) PE
ples 1–3 at an applied voltage of (1) 100 and (2) 1000 V. and samples (2) 1, (3) 2, (4) 3, (5) 4, and (6) 5.
ally overlap. Unfortunately, this prevented us from tance versus time, filler content, and applied voltage for
unambiguously determining the composition of the our materials are displayed in Figs. 7–9.
nanoparticles and the exact phase composition of the The permittivity data are presented in Table 3 and
samples from XRD data. Nevertheless, based on the Figs. 10 and 11.
general trends in the compositions of the synthesized
metal-containing nanoparticles, we developed a model The observed magnitudes and time dependences of
of a nanoparticle stabilized in a polymer matrix (Fig. 5), resistivity lead us to the following conclusion: the elec-
which is consistent with earlier results on the composi- trical transport in the nanocomposites follows the same
tion of nanoparticles stabilized both in the interior of mechanisms as in unloaded polyethylene (ionic con-
polymers [12, 35, 41] and on the surface of microgran- duction, dipole polarization, displacement polarization,
ules [42–44]. electrical cleaning, electron injection through the elec-
trode–sample interface). The resistivity and dielectric
The densities of our samples (determined by hydro- permittivity of the unloaded polyethylene differ from
static weighing and calculated) are listed in Table 1. standard values (1016 to 1018 Ω m and 2.2–2.3, respec-
Figure 6 plots the density versus filler content. The vol- tively), which is attributable to contamination during
ume coefficient in Table 1 is introduced to match the processing.
measured densities of the samples to the calculated
ones and represents the relative expansion of the poly- The resistivity of the samples containing 5 and 10 wt %
mer matrix upon the introduction of metal-containing filler (samples 1 and 2), as well as that of unloaded
nanoparticles. The increase in volume is, most likely, polyethylene, is a weak function of applied voltage and
due to an increase in amorphous content and the forma- decreases linearly with increasing nanoparticle content
tion of nanopores in the polyethylene matrix. over the entire voltage range studied. At a nanoparticle
content of 20 wt %, the resistivity is a stronger function
The resistivity data for the polymer-matrix compos- of applied voltage: raising the voltage from 100 to 1000 V
ites are presented in Table 2. The plots of sample resis- reduces the resistivity of samples 4 and 5 by a factor of
ε ε
4.6 3.6
4.4 3.4
4.2
3.2
4.0
3.0
3.8
3.6 2.8
3.4 2.6
3.2 2.4
3.0 1 1
2 2.2 2
2.8 3
2.6 2.0
0 5 10 15 20
15 20 25 30 35 40 45 50 55
wt % filler
Frequency, GHz
Fig. 10. Low-frequency dielectric permittivity as a function Fig. 11. Microwave dielectric permittivity as a function of
of filler content for samples 1–3: (1) 1 kHz, (2) 1 MHz. frequency: (1–3) samples 1–3, respectively.
3 and that of sample 3 by more than one order of mag- reduction in relaxation rate without changes in relax-
nitude. ation time. Increasing the nanoparticle content to 20 wt %
The reduction in resistivity upon the introduction of (sample 3) reduces the relaxation time, with no marked
nanoparticles into polyethylene may be due to changes changes in relaxation rate. Note that increasing the
in its structure, such as an increase in amorphous con- nanoparticle content of the polymer tends to reduce the
tent and porosity, which raise its molecular mobility relaxation time and raise the relaxation rate. These rela-
and reduce the dissociation energy of the ions in the tionships, as well as the low-frequency data, can be
polymer. understood in terms of the polarization of the metal-
An additional contribution to the electrical conduc- containing nanoparticles, whose permittivity increases
tivity of the nanocomposites may come from polariza- with particle size. The present results demonstrate that
tion effects associated with the polarizability of the the microwave absorption and permittivity of our sam-
nanoparticles: macrodisplacement (on the length scale ples vary little in a broad frequency range.
of the sample) and microdisplacement (within local
regions) polarization and slowly developing dipole Samples 1–5 were characterized by magnetic reso-
polarization. nance measurements. The spectrometer recorded the
derivative of microwave absorption with respect to
The composition and size of the nanoparticles have external field H0. The measurements were performed at
a complex effect on the electrical conductivity of the
loaded high-pressure polyethylene, which is well illus- room temperature using samples in the form of thin
trated by the lower resistivity of sample 3 at a voltage
of 1000 V in comparison with that of samples 4 and 5.
5.0
The systematic increase in permittivity with increas-
ing filler content is due to the contribution from the 4.5
polarization of the metal-containing nanoparticles, 4.0
whose polarizability is higher than that of the matrix
Absorption, dB/cm
3.5
owing to the higher mobility of electron shells. As a
result, the permittivity increases with filler content. 3.0
Samples 3 and 4, though identical in the concentra- 2.5
tion of iron-containing nanoparticles, differ in permit- 2.0
tivity, which can be accounted for by the higher permit- 1.5 1
tivity of larger particles. 1.0 2
The microwave permittivity and absorption data for 3
0.5
samples differing in the concentration of nanoparticles
are presented in Figs. 11 and 12. These data can be used 0
15 20 25 30 35 40 45 50 55
to evaluate the amplitudes and time constants of relax- Frequency, GHz
ation processes. For samples 1 and 2, the reduction in
permittivity, with no significant changes in losses in the Fig. 12. Microwave absorption as a function of frequency:
working frequency range, can be accounted for by a (1–3) samples 1–3, respectively.
∆Hpp
1
3
4
Hres H0(||)
5 n
H0(⊥)
80 160 240 320 400 480
H, kA/m 80 160 240 320 400 480
H, kA/m
Fig. 14. Geometry of EMR measurements: ∆Hpp is the lin-
Fig. 13. Room-temperature magnetic resonance spectra: ewidth, Hres is the resonance field, H0 is the external mag-
(1–5) samples 1–5, respectively. netic field, and n is the normal to the sample surface.
(0.5- to 1-mm in thickness) square (2- to 3-mm side) significant magnetization of the sample and scatter of
plates. The spectra of all the samples show inhomoge- local magnetic fields. The scatter may arise from the
neously broadened singlets (Fig. 13). To analyze the presence of different phases in the cobalt nanoparticles
spectra, we determined the linewidth ∆Hpp and reso- (cobalt metal and cobalt oxides), differing in magnetic
nance field Hres for two field directions: parallel (||) and properties. The magnetization of the samples was esti-
perpendicular (⊥) to the sample surface (Fig. 14). The mated from the difference in resonance magnetic field
values of ∆Hpp, Hres(⊥), and Hres(⊥) – Hres(||) are listed between two sample orientations, which is due to the
in Table 4. difference in the corresponding demagnetizing factors.
In a field normal to the plate surface, the demagnetizing
In samples 1–4, the EMR linewidth increases with factor is rather large (4π in an infinite plate). In a field
metal content (Fig. 13), characteristic of ferromagnetic parallel to the plate surface, it is close to zero. It can be
nanoparticles. ∆Hpp increases most rapidly upon an seen from Table 4 that the magnetization of the sample
increase in metal content from 10 to 20% (samples 2 containing cobalt nanoparticles is several times higher
and 3, respectively). This fits well with the conclusion than that of the sample containing magnetite nanoparti-
that sample 3 has a reduced relaxation time, inferred cles in the same concentration (20%) and of nearly the
from permittivity and microwave absorption data. The same size.
EMR linewidth, however, depends not only on the total
metal concentration but also on the average nanoparti- We also studied the low-field microwave absorption
cles size. In particular, the smaller particle size in sam- hysteresis, which characterizes the remanent magnetic
ple 4 compared to sample 3 (2.4 and 11.5 nm, respec- moment of the material. The highest remanent magne-
tively) leads to significant narrowing of the resonance, tization (~100 to 200 G) was observed at the highest
by more than 30% (Table 4). nanoparticle concentration. All the above demonstrates
that, among the materials containing magnetite and
The largest linewidth was observed in sample 5, cobalt nanoparticles, the highest magnetization (includ-
containing cobalt nanoparticles. This may be due to a ing the remanent one) is offered by the cobalt-contain-
ing samples and that, on the whole, increasing the metal
Table 4. EMR parameters of samples 1–5
concentration improves the magnetic properties of the
nanomaterials.
Sample ∆Hpp , Hres(⊥), Hres(⊥) – Hres(||),
no. kA/m kA/m kA/m
CONCLUSIONS
1 48.54 250.57 0.0
2 76.40 266.60 3.98 We prepared nanocomposites consisting of nar-
3 132.90 246.70 3.98 rowly sized metal-containing nanoparticles embedded
in a polyethylene matrix and established conditions for
4 94.70 246.70 3.18 the fabrication of thick films and bulk materials from
5 141.65 250.68 11.14 the resulting polymer powders.
Our results on the electrical properties of the poly- 8. Smith, T.W. and Wychick, D., Colloidal Iron Dispersions
ethylene-matrix nanocomposites containing iron nano- Prepared via the Polymer-Catalyzed Decomposition of
particles demonstrate that, with increasing nanoparticle Iron Pentacarbonyl, J. Phys. Chem., 1980, vol. 84,
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mittivity and absorption coefficient of the nanostruc- 9. Gubin, S.P., What is a Nanoparticle? Current Trends in
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The electrical properties (dielectric permittivity and
resistivity) of the composites depend on the nanoparti- 10. Zanetti, M. and Costa, L., Preparation and Combustion
Behaviour of Polymer/Layered Silicate Nanocomposites
cle size and concentration. Based upon PE and EVA, Polymer, 2004, vol. 45,
Our results demonstrate that the microwave absorp- pp. 4367–4373.
tion and permittivity of the nanocomposites vary little 11. Zanetti, M., Camino, G., Reichert, P., and Mülhaupt, R.,
in a broad frequency range. Thermal Behaviour of Poly(propylene) Layered Silicate
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ACKNOWLEDGMENTS and Iron-Containing Nanoparticles, Composites, 2006,
vol. 37, no. 6, pp. 413–417.
This work was supported by the Russian Foundation
14. Zanetti, M., Lomakina, S., and Camino, G., Polymer
for Basic Research (grant nos. 07-03-00885, 07-08- Layered Silicate Nanocomposites, Macromol. Mater.
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President’s Grants Council (grant no MK-253.2007.3),
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the National Science Promotion Foundation, INTAS Thermal Stability of Cu/LDPE Nanocomposites, Mater.
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and Technology Center (grant no. 3457), and the Rus-
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