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Formation, Structure and Magnetic Properties of Polymer Matrix

Nanocomposites Processed by Thermal Decomposition of the Fe(III)Co(II)
Acrylate Complex

Article  in  Journal of Nanoparticle Research · August 2003

DOI: 10.1023/A:1025504808503

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Journal of Nanoparticle Research 5: 373–381, 2003.
© 2003 Kluwer Academic Publishers. Printed in the Netherlands.

Formation, structure and magnetic properties of polymer matrix

nanocomposites processed by thermal decomposition of the
Fe(III)Co(II) acrylate complex

M. Ławecka1 , M. Kopcewicz2,∗ , A. Ślawska-Waniewska3 , M. Leonowicz1 , J. Kozubowski1 ,

G.I. Dzhardimalieva4 , A.S. Rozenberg4 and A.D. Pomogailo4
1
Faculty of Materials Science and Engineering, Warsaw University of Technology, Warsaw, Poland;
2
Institute of Electronic Materials Technology, Warsaw, Poland; 3 Institute of Physics, Polish Academy of
Sciences, Warsaw, Poland; 4 Institute of Problem of Chemical Physics, Russian Academy of Sciences,
142432, Chernogolovka, Moscow Region, Russia; ∗ Author for correspondence (Tel.: 835 30 41, ext. 448;
Fax: 39 12 07 64; E-mail: kopcew m@sp.itme.edu.pl)

Received 20 January 2003; accepted in revised form 15 April 2003

Key words: metal oxide nanoparticles, nanocomposites, polymers, thermal decomposition

Abstract

Structure and magnetic properties of polymer matrix nanocomposites, processed by pyrolysis of the Fe(III)Co(II)
acrylate complex, were investigated. It was shown that thermal transformation of the complex studied consisted
of three macrostages: dehydration, solid state polymerisation and decarboxylation of a metallopolymer form. The
main products of the decomposition were nanoparticles stabilised by polymeric matrix. The crystalline phases,
which were found in the fully processed material, were Fe3 O4 , CoFe2 O4 and CoO. The mean crystallite size was
10 nm. In the intermediate stages of the thermolysis iron was present in the forms of FeIII (trivalent low – spin iron),
Fe2+ (divalent high – spin iron) and Fe3 O4 . The hysteresis loops measured at temperatures below 200 K were opened
and shifted towards negative field. The coercivity and remanence showed room temperature values of 0.18 T and
15.5 mT, respectively.

Introduction metal acrylates, due to its simplicity and effectiveness

Currently exists a great variety of methods which
enable processing of polymer matrix nanocomposites,
among them such well established as mechanical mix-
ing of pre-synthesised nanoparticles with polymer or
synthesis of nanoparticles via polymerisation of col-
loidal solutions containing metal ions and monomers
(Cabasso & Yuan, 1996). The particle size can be
controlled by the pH, concentration and properties
of the colloidal solution. The stability of colloidal
solution is one of the major problems. We can over-
come these complications by producing nanoparticles
via solid state polymerisation. The method based on
thermal transformation of metal-containing monomers,
appears to be particularly promising. We have already
shown that it is possible to synthesise ultradispersed
particles and simultaneously chemically passivate them
by the in situ formation of polymer matrix during
thermal decomposition of metal-containing monomers
(Aleksandrova et al., 1993; Rozenberg et al., 1993;
1995; 1998). Pyrolysis of metal-containing monomers
occurs via three main processes: dehydration, solid
state polymerisation of the initial monomer, decar-
boxylation of the metallocarboxylate groups in the
metallopolymer, followed by formation of metal or
metal-oxide ultradispersed particles. The metal parti-
cles formed in the last reaction can be oxidised by
CO2 . The nanocomposite material can be in a form
374
of MOr(CH2 CHCOO)p-x(CH2 CH)x(CHCHCOO)q-
y(CHCH)y, where M is a transition metal. The pyroly-
sis products of metal monomers such as Fe(III), Co(II)
exhibit ferromagnetic properties. The whole processing
method leading to the formation of the nanocomposite
materials is very simple. The composition and the parti-
cle size in the final material depend on the temperature
and time of thermal decay.
In this study, thermal decomposition of the
[Fe3 O(CH2 CHCOO)6 OH][Co(CH2 CHCOO)2 ]1.5 ·3H2 O
complex, having the Fe : Co atomic ratio close to 2 : 1,
was investigated. Composition, structure and mag-
netic properties of the nanocomposites obtained were
analysed for different processing temperatures.
Experimental
The Fe(III)Co(II) acrylate complex with nom-
inal composition: [Fe3 O(CH2 CHCOO)6 OH]
[Co(CH2 CHCOO)2 ]1.5 ·3H2 O (Fe2 CoAcr) was pre-
pared by coprecipitation of [Fe3 O(CH2 CHCOO)6 OH]·
3H2 O (FeAcr3 ) and Co(CH2 CHCOO)2 ]·H2 O (CoAcr2 )
salts from an alcoholic solution at Fe/Co = 2. The metal
acrylates FeAcr3 , CoAcr2 and Fe2 CoAcr were obtained
according to a procedure described earlier (Dzhardi-
malieva et al., 1988). The thermal transformations
of Fe2 CoAcr complex proceeded in a self-generated
atmosphere and under static non-isothermal condi-
tions, in the temperature range of 613–663 K. The
kinetics of gas evolution was recorded using a mem-
brane zero-manometer. The mass loss of the sample
and the amounts of gaseous products at ∼300 K and
those condensing at 77 K were determined at the end of
the thermal transformation. The following specimens
were analysed:
sample 1 – precursor acrylate – Fe2 CoAcr;
sample 2 – product of thermal decomposition at
493 K, weight loss, m = 25.1%;
sample 3 – product of thermal decomposition at
643 K, weight loss, m = 37.3%;
sample 4 – product of thermal decomposition at
643 K, weight loss, m = 42% (longer
annealing time).
The specific surface area of the precursor sample
and the solid-phase products of the thermal trans-
formation were determined by the low-temperature
nitrogen adsorption method. The infrared absorption
spectroscopy (IRA) spectra of gaseous and condensed
products were recorded using an UR-10 instrument
from 400 to 4000 cm−1 . Optical microscopy (OM)
observations were performed in transmitted light on
MBI-15 Leitz Metalloplan microscope. Mass spectral
analysis was performed using MS 3702 quadruple mass
spectrometer. X-ray diffraction phase analysis was car-
ried out at room temperature using a Philips PW 1050
diffractometer, Cu Kα radiation. The Mössbauer mea-
surements were performed at room and liquid nitro-
gen temperatures using the 57 Co∗ in –Rh source. The
isomer shifts are related to the αFe standard. For
the transmission electron microscopy (TEM) investi-
gations a Philips EM 300 microscope, operating at
100 kV and for the high-resolution electron microscopy
(HREM) investigations a JEM 3010 microscope, oper-
ating at 300 kV, were used. Magnetic measurements
were carried out using Oxford Instruments vibrating
sample magnetometers. The magnetic measurements
were done for the sample 4. The hysteresis loops
were recorded at different temperatures in the range of
5–300 K up to the maximum field of 1.1 T. The mag-
netisation versus temperature was measured in the
same temperature range, in a low magnetic field of
2 × 10−3 T, during heating after zero field cooling
(ZFC) and in the course of subsequent cooling (FC).
The magnetisation was also recorded and in a field
of 0.6 T during heating from 5 to 300 K. Room tem-
perature hysteresis loop was measured in a maximum
field 9 T.
Results and discussion
Composition of the thermolysis products
According to the data of the IRA and mass spec-
troscopy, CO2 is the main gaseous product of Fe2 CoAcr
pyrolysis. The H2 and CO emission is in substan-
tially smaller amounts. The vapours of acrylic acid,
CH2 = CHCOOH, and H2 O also exist as gaseous prod-
ucts. They condense on cool parts of the reaction vessel
in the process of heating.
The dispersion of the Fe2 CoAcr sample is evi-
denced from the broad absorption bands related to the
stretching vibrations of the H−
−O bond of coordinated
water (3000–3600 cm−1 ) and stretching vibrations of
the H− −C bond of the CH2 CHCOO− anion (2900–
3050 cm−1 ), which are observed in the IRA spectra of
Fe2 CoAcr complex (Table 1). The system of bands in
the 1360–1540 cm−1 range is caused by the stretching
vibrations of the COO groups (McCluskey et al., 1989;
 375

Table 1. Frequencies of stretching vibrations∗ in the IRA absorption spectra of the Fe2 CoAcr complex and the products of transformation
of the Fe2 CoAcr complex at 643 K (Irel = ν /maxν is the relative intensity, ν is the absorption at frequency ν)

The initial Fe2 CoAcr complex Products of transformation of the Fe2 CoAcr complex
ν cm −1
Irel Assignment m = 25.1% m = 37.3% m = 42.0% Assignment
ν cm −1
Irel ν cm −1
Irel ν cm −1
Irel

3000–3600 br ν(OH) (H2 O)

3045 νas(CH)
2960 νs(CH) 2930 ν(CH)
1630 0.74 ν(C= C), 1640 0.35 1680 0.46 1685 0.38 ν(C= C)
δ(OH)(H2 O)
1575 1.00 νas(COO) 1555 1.00 1555 1.00 1565 1.00 νas(COO)
(Fe cluster) (Fe cluster)
1540 0.80 νas(COO) (Co) 1540 0.99 1540 0.99 1550 1.07 νas(COO) (Co)
1525 0.77 νas(COO) 1520 0.92 1520 0.98 1520 0.99 νas(COO)
(Fe cluster) (Fe cluster)
1505 0.485 νas(COO) (Co) 1505 sh 0.715 1498 0.89 νas(COO) (Co)
1490 sh 0.39 δ(CH) 1490 0.6 δ(CH)
1435 0.92 νs(COO) 1435 0.85 1440 1.02 1420 1.23 νs(COO)
(Fe cluster) (Fe cluster),
ν(OH2 ) (−−CH2 −
−CHR− −)
1420 0.92 νs(COO) (Co) 1415 0.85 1408 1.07 νs(COO) (Co), δ(OH2 )
(H2 C−−CR− −)
1360 0.82 νs(COO) 1400 0.97 1395 1.10 1400 1.20 νs(COO)
(Fe cluster) (Fe cluster),
δ(OH2 ) (CH2 = CR−−)
1350 0.71 1315 0.57 νs(COO) (Co), δ(OH)
(−−CH2 − −CHR−−)
1270 0.44 ρt (CH2 ) 1280 sh 0.51 1270 sh 0.665 1265 1.08 ρt (CH2 )
(CH2 −−CH= CH− −)trans
1185 0.35 1160 1150 1.37 ν(C− −C) (= CH−−CHR− −)
1120 br 0.10
1068 0.32 ν(C−−C)
990 0.38 π (CH)
(−−CH= CH2 )
965 0.31 π (CH)
(−−CH= CH2 )
910 0.07 ρ(OH) (H2 0), 855 0.08 860 0.15 875 0.33 δ(CH) (−
−CH= CHR)
ν(M−−OH2 )
830 0.61 ρw (CH2) 835 0.09 830 0.10 830 0.20 −CH2 −
ρw (CH) (− −CHR−
−)
728 0.12 775 0.07 755 0.11 750 1.11
673 0.50 ρr (CH2), 645 br 0.03 ρt (CH)
δ(M− −OH2 ) (−−CH2 −−CR= CH−−)cis,
598 0.11 δ(CH2 ), 592 0.02 δ(CH2 ), ρw (CH)
δ(M− −OH2) (−−CH= CHR)
545 0.07 δ(CH2 ),
δ(M− −OH2 )
∗
The following designations for vibrations are used: ν, stretching; δ, bending; ρw , wagging; ρr rocking; ρt , twisting; π , out of plane; as,
asymmetric; s, symmetric; sh, shoulder; br, broad.

Shulga et al., 1993). The following changes in the the M ← OH2 bond disappears due to the dehydra-
IRA spectra are observed as the degree of conver- tion of Fe2 CoAcr complex. The absorption band at
sion increases: the absorption related to the stretching ∼1630 cm−1 shifts towards the high-frequency region
and bending vibrations of H2 O and the vibrations of which may be caused by the appearance of the
376

stretching vibrations of the conjugated C= C group.

The stretching vibrations of COO and C= C groups also
disappear as the degree of conversion increases. Thus,
the analysis of the IRA spectra of the solid phase in the
course of the transformation indicates that the Fe and
Co fragments are dehydrated and decomposed.

Structural and microstructural characterisation

OM studies show that the initial sample of Fe2 CoAcr

complex is morphologically similar before and after
thermal transformation. Initial compound consists
of light brown, transparent crystals having irregular
shape. Their average size is 10–15 µm with fairly
narrow size distribution. They form agglomerates,
usually 100–150 µm in size, however some are as big
as ∼1–2 mm. The agglomerates grow in the course
of thermal transformation. Their specific surface
increases from 8.1 to 11.3 m2 g−1 . They are brittle,
porous and consist of glass-like platelets (∼100 µm).
The colour of these platelets changes continuously
Figure 1. X-ray diffraction patterns for the precursor acrylate and
from light brown to dark brown. This indicates that thermolysis products.
the transformation of Fe2 CoAcr is voluminous, homo-
geneous. At the end of the transformation, the average
size of agglomerates decreases again. The final prod-
uct consists of irregular platelets, which are black in
reflected light.
A fairly complex crystalline structure was found for
the precursor material (sample 1) using X-ray phase
analysis. This structure was, however, not analysed at
this stage. In the specimen, which was annealed at
493 K, m = 25.1% (sample 2), crystalline phases
were not found, some unidentified reflections were
present. After the thermolysis at 643 K, m = 37.3%,
(sample 3), the only phase, which could be identified
was Fe3 O4 . After longer annealing at this temperature,
m = 42% (sample 4) CoO, Fe3 O4 and CoFe2 O4
phases were found, however, the crystallographic
parameters for cubic inverse spinels CoFe2 O4 and
Fe3 O4 are very similar. Some unidentified reflections
were also present (Figure 1).
The TEM investigations proved the existence of
metallic particles, which were distributed in a polymer Figure 2. TEM microstructure for the fully processed sample
matrix. The mean size of the particles was about 30 nm (annealed at 643 K, weight loss m = 42%).
(Figure 2). From HREM investigations it was found
that these particles were agglomerated and the mean (sample 1), a presence of FeIII only was apparent from
size of the crystallite was about 10 nm (Figure 3). the spectrum (Figure 4a). In the course of anneal-
The parameters of Mössbauer spectra, for all the ing at 493 K (sample 2) a reduction of the FeIII to
samples, which were investigated at 295 K, are shown Fe2+ occurred which is represented in Figure 4b by
in Table 2 and Figure 4. For the precursor acrylate an additional doublet with large quadruple splitting.
 377

On increasing the annealing temperature up to 643 K
(sample 3) the reduction of FeIII proceeded further
(Figure 4c). The percentage of the Fe2+ ions increased
from 8.8% at 493 K up to 57.8% at 643 K, however, for
longer annealing times at the latter temperature (m =
42%) the amount of the Fe2+ started to decrease again,
down to 8.1% (sample 4, Figure 4d). A new phase,
Fe3 O4 , appeared which was evidenced from the values
of the two sextets representing hyperfine fields of triva-
lent iron in the tetrahedral sites (A) as well as trivalent
and divalent iron in the octahedral sites (B) (Figure 6a).
The values of those fields were 48.7 and 45.9 T, respec-
tively. We could suppose that the spectrum related to
CoFe2 O4 , was included in the FeIII spectrum. The pres-
ence of CoO was not confirmed in this experiment
because cobalt is not the Mössbauer isotope.
Low temperature Mössbauer measurements, at 80 K,
were performed for the samples 2, 3 and 4. The results
are collected in Table 3 and shown in Figures 5–
7. For the sample 2 the same phase structure as at
the room temperature was found (Figure 5). Mag-
netic phases were not detected. However, the spectra
of the sample 3, which were recorded at room and low
temperatures, respectively, were somewhat different

Figure 3. HREM microstructure for the fully processed sample Figure 4. The 295 K Mössbauer spectra for samples annealed at
(annealed at 643 K, weight loss m = 42%). different temperatures.

Table 2. Parameters of Mössbauer spectra at 295 K

Sample/annealing δ (IS) QS Hhf (T) Iron forms Relative

conditions (mm/s) (mm/s) percentage
of iron (%)

1/precursor complex Fe2 CoAcr 0.200 0.886 0 FeIII 100

2/493 K; m = 25.1% 0.172 0.788 0 FeIII 91.2
0.805 2.602 Fe2+ 8.8
3/643 K; m = 37.3% 0.919 2.144 0 Fe2+ 57.8
0.173 0.770 FeIII 42.2
4/643 K; m = 42% 0.175 0.764 0 FeIII 75.3
0.815 2.220 0 Fe2+ 8.0
0.088 0 48.7 Fe3+ (A) 11.2
0.223 0.084 45.9 Fe3+ , Fe2+ (B) 5.5
378

Table 3. Parameters of Mössbauer spectra at 80 K

Sample/annealing δ (IS) QS Hhf Iron forms Relative

conditions (mm/s) (mm/s) (T) percentage
of iron (%)

2/493 K; m = 25.1% 0.301 0.804 0 FeIII 93.9

1.040 2.836 0 Fe2+ 6.1
3/643 K; m = 37.3% 1.090 2.491 0 Fe2+ 60.5
0.216 0.994 0 FeIII 29.5
0.186 0 50.8 Fe3+ (A) 6.8
0.216 0.040 47.4 Fe3+ ,Fe2+ (B) 3.2
4/643 K; m = 42% 0.286 0.890 0 FeIII 35.5
0.996 2.650 0 Fe2+ 18.2
0.386 0 49.0 Fe3+ (A) 6.1
0.356 0 52.0 Fe3+ (B) 9.9
0.186 0 50.8 Fe3+ (A),(B) 19.1
0.216 0.040 47.4 Fe2+ (B) 11.2

1,00

a 295 K

0,98
Relative transmission

1,00

80 K
b

0,95
-8 -4 0 4 8
Figure 5. The 295 and 80 K spectra for the sample 2 (annealed Velocity [mm/s]
at 493 K, weight loss, m = 25.1%).
Figure 6. The 295 and 80 K spectra for the sample 3 (annealed
(Figure 6). The 80 K spectrum showed the existence of at 643 K, weight loss, m = 37.3%).
the FeIII and Fe2+ iron as doublets, and additionally, two
sextets of Fe3 O4 compound. The values of hyperfine The values of hyperfine fields for CoFe2 O4 , in sites A
fields for Fe3 O4 , in sites A and B, were 50.8 and 47.4 T, and B, were 49 and 52 T, respectively (Methasiri et al.,
respectively. Longer annealing at 643 K, m = 42% 1980).
(sample 4), caused the decrease of the amount of the
FeIII iron from 75.3%, when measured at 295 K, down Magnetic properties
to 35.5% at 80 K, in favour of the increasing fraction
of the Fe3 O4 phase up to 30% as well as the appearance At room temperature the material exhibited moder-
of the CoFe2 O4 phase, at a level of 16% (Figure 7). ately hard magnetic properties with the coercivity

Figure 7. The 295 and 80 K spectra for the sample 4 (annealed
at 643 K, weight loss, m = 42%).
Figure 8. Selected hysteresis loops for the sample 4, recorded at
5, 75 and 300 K in a field of 1.1 T.
and remanence of 0.18 T and 15.5 mT, respectively.
The magnetisation continuously grew with increasing
magnetising field, and the material did not show satu-
ration of magnetisation even in magnetic field as high
as 9 T, which indicates high magnetic anisotropy.
379
The hysteresis loops were also recorded within tem-
perature range of 5–300 K. The maximum magnetising
field was 1.1 T. In Figure 8 the loops, which were
obtained at temperatures 5, 75 and 300 K are shown.
The loops recorded at temperatures lower than 200 K
were opened, and shifted towards negative magnetic
field. The shift increased with decreasing temperature.
This behaviour arises from complex magnetic structure
of the material, in which we can expect both ferro- and
antiferromagnetic interactions and canted spin struc-
ture, which at temperatures below 200 K could not
produce a continuous closed loop in the presence of
small external magnetising field. Additionally we can-
not exclude some contribution to this phenomenon
resulting from the effect associated with ‘freezing’ of
disordered surface spins, which was reported for ferri-
magnetic nickel ferrite nanoparticles (Berkowitz et al.,
1975; 1996; 1997; 1999; Lin et al., 1995).
In Figure 9 the coercivity and remanence are plot-
ted versus temperature in the range of temperature
changes of reversible magnetisation, i.e. over 200 K.
Both, the M Hc and Mr exhibit dependence characteristic
of ferromagnetic materials.
The magnetisation versus temperature was also mea-
sured in a magnetising field of 0.6 T (Figure 10).
The magnetisation increased slightly up to the temper-
ature of approximately 200 K. For higher temperatures
the magnetisation was constant. The deflection point
on this curve, in the temperature range of 150–200 K,
we attribute to the end of the irreversible magnetisation
processes.
In Figure 11 the magnetic moment versus tempera-
ture in a field of 2 × 10−3 T is shown during heating,
after ZFC and in the course of field cooling (FC). The
difference in the shapes and positions of both curves is
again related to the strong irreversible processes, origin
of which at this stage cannot be fully explained. They
may arise from magnetic interactions within the parti-
cles, between the particles or the particles and polymer
matrix. One has to note that the phase structure com-
prises two ferrimagnetic phases: Fe3 O4 and CoFe2 O4
as well as antiferromagnetic CoO.
Conclusions
Mixed metal oxide particles in a polymer matrix,
having uniform size and distribution, have been suc-
cessfully synthesised. Crystalline phases, which were
found in the fully processed material (643 K, m =
42%), were: ferrimagnetic Fe3 O4 and CoFe2 O4 , and
380
Figure 9. Coercivity M Hc and remanence Mr versus temperature,
recorded in the temperature range of reversible processes, for the
sample 4.
Figure 10. Magnetisation versus temperature, measured in a field
of 0.6 T, for the sample 4.
Figure 11. Magnetisation versus temperature, recorded in a in a
field of 2 × 10−3 T, after ZFC and during FC, for the sample 4.
antiferromagnetic CoO. At the intermediate stages
of the transformation iron was present in a form
of FeIII and Fe2+ ions, and as the Fe3+ , Fe2+ in
Fe3 O4 . Microstructure of the material consisted of
30 nm polycrystalline metallic agglomerates, which
were homogeneously distributed in the polymer matrix.
The agglomerates consist of individual crystallites
having mean size of 10 nm. The precursor acrylate
as well as the sample 2 (493 K, m = 25.1%)
were non-magnetic. The magnetic properties of the
transformation products are characteristic of small
ferrite particles and strongly depend on the intrinsic
magnetic properties of the constituents, temperature
and magnetising field. Room temperature coercivity
and remanence values, for the fully processed mate-
rial, were 0.18 T and 15.5 mT, respectively. Strong
dependence of the magnetic properties on the phase
constitutions, temperature and field puts the material
as a promising candidate for sensor applications.
Acknowledgements
Financial support from the Polish State Committee
for Scientific Research (project 7T08A05622) and
Russian Foundation for Basic Research (project N
01-03-33257) are gratefully acknowledged.
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