Materials Letters 68 (2012) 251–254

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Materials Letters
journal homepage: www.elsevier.com/locate/matlet

Electrospun PVC/Fe3O4 composite nanofibers for microwave absorption applications

Ovidiu Chiscan, Ioan Dumitru, Petronel Postolache, Vasile Tura, Alexandru Stancu ⁎
Department of Physics, Alexandru Ioan Cuza University, Iasi, 700506, Romania

a r t i c l e i n f o a b s t r a c t

Article history: In this paper we present a study on the microwave frequency properties of PVC/Fe3O4 composite nanofibers,
Received 10 August 2011 with different amounts of iron oxide nanoparticles incorporate in PVC matrix. Using electrospinning where
Accepted 23 October 2011 obtained composite nanofibers with diameters ranging between 100 nm and 600 nm. The transmission loss of
Available online 29 October 2011
PVC/Fe3O4 composites measured in the microwave frequency range of X-band were found to be
below −15 dB demonstrating that these materials can be used as protection material of electromagnetic radia-
Keywords:
Composite nanofibers
tion. The applied magnetic field significantly modifies the measured scattering parameters in our samples case in
Electromagnetic shielding a rather large domain of values for the field.
Electrospinning © 2011 Elsevier B.V. All rights reserved.
Microwave absorber

1. Introduction Polycid, tetrahydrofuran — THF, N,N-dymethilformamide — DMF, parti-

Composite nanofibers consisting of magnetic nanoparticles embed-
ded into a polymer matrix have been under intensive investigation in
the last years because of their magnetic-field dependent physical
properties. A large number of applications like magnetic cell separation
[1], magnetic resonance imaging contrast agents [2], magnetic filters
[3], magnetic sensors [4] and low frequency magnetic shielding [5,6]
were developed based on their properties.
Among the polymeric nanofiber preparation techniques, electro-
spinning proved to be a versatile and effective method to prepare fibers
with diameters ranging from a few nanometers to one micrometer or
more [7,8]. This technique was used over the last decade to prepare
nanofibers from a wide range of natural or synthetic polymers [9–12].
The polymeric nanofibers containing magnetic nanoparticles
combine the typical properties of a polymeric nanofiber material, i.e.
high surface/volume ratio, good mechanical flexibility and high electri-
cal resistivity, with the high magnetic susceptibility of the magnetic
nanoparticles, becoming attractive materials for high-frequency
electronic applications.
In this paper the influence of magnetic nanoparticle concentration
on the high-frequency electromagnetic fields absorption properties of
PVC nanofibers containing Fe3O4 nanoparticles was investigated.
2. Experimental
The chemical reagents used in this study were: emulsion powder
poly(vinyl chloride) — PVC (Vinycel 124) K value 69 supplied by
⁎ Corresponding author.
E-mail address: alstancu@uaic.ro (A. Stancu).
cles of iron (II,III) oxide 98% (metals basis) supplied by Alfa Aesar.
At the beginning, a solution of PVC (7.5 g) dissolved in a THF/DMF
(36 ml/9 ml) solvent mixture was prepared and shared in three equal
parts. Then, each solution part was added with Fe3O4 nanoparticles
(size between 20 and 30 nm) in different amounts (sample A — 0.5 g,
sample B — 2.5 g, sample C — 5.0 g) and homogenized for 90 min
using a mechanical stirrer. These PVC/Fe3O4 solutions were used to pre-
pare composite nanofibers by means of a homemade electrospinning
device containing a syringe pump able to provide flow rates between
1.0 and 30 μl/min. The syringe equipped with a 0.7 mm diameter
blunt needle was placed vertically above a nanofibers collector. The
needle and the collector were connected to a high voltage power supply
(0–30 KV). The morphology of the obtained nanofibers was investigat-
ed by scanning electron microscopy (SEM), Vega 2 Tescan. The micro-
wave transmission/reflection (T/R) parameters were measured in
8–12 GHz frequency domain using a waveguide fixture and an
E8361A PNA Network Analyzer.
3. Results and discussion
Fig. 1 shows SEM images of composite nanofibers prepared using
the same quantity of PVC matrix and three different amounts of Fe3O4
nanoparticles. These SEM images show that the resulted composite
nanofibers consist of Fe3O4 nanoparticles incorporated into PVC nanofi-
bers with diameter range between 100 and 600 nm. It can be seen also
that increasing the concentration of Fe3O4 nanoparticles inside the
nanofibers, the distance between the enclosed nanoparticles decreases
and they tend to agglomerate. The volume of agglomerations increases
with nanoparticles concentration. From histograms showed in Fig. 1 it
can be observed that for sample (A) (with minimum load of magnetite
nanoparticles) composite nanofibers diameter range from 100 to
600 nm. Increasing Fe3O4 loading in PVC matrix we can observe that

0167-577X/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.matlet.2011.10.084
252 O. Chiscan et al. / Materials Letters 68 (2012) 251–254
Fig. 1. SEM image and histograms of composite nanofibers with different amount of Fe3O4 particles: (A) — 0.5 g, (B) — 2.5 g, (C) — 5 g.
the nanofibers diameter tends to a narrower range between 200–350 nm
for sample (B) and 250–350 nm for sample (C). It seems that the presence
of the particles has a stabilizing effect for the fibers diameter which has to
be understood within the theory of the electrospinning process.
Ferromagnetic resonance (FMR) spectra were recorded and trans-
mission/reflection coefficients of the prepared composite nanofibers
were measured in order to investigate the behavior of these materials
in high frequency electromagnetic fields. The FMR curves were
recorded using a rectangular cavity working in TE 102 excitation
mode at 9.98 GHz ac magnetic field frequency, sweeping the static mag-
netic field up to 9000 Oe. From the FMR spectra presented in Fig. 2 it can
be seen a shift of the resonant absorption field accompanied by a
Fig. 2. Resonance spectra of composite nanofibers containing different amounts of
Fe3O4 nanoparticles: (A) — 0.5 g, (B) — 2.5 g, (C) — 5.0 g.
broadening of the resonance curve as the amount of Fe3O4 nanoparti-
cles dispersed into the PVC matrix increases. This broadening extends
the frequency range in which these materials can be used as microwave
absorbers.
The reflection/transmission coefficients of the investigated mate-
rials placed into a rectangular waveguide fixture were measured in
the X band frequency domain for various sample thicknesses. The mate-
rial samples under test fully fit the waveguide cross section. The
samples thickness was changed by increasing the number of nanofiber
membrane layers. A layer of as deposited nanofibers membrane had a
fixed thickness of 0.8 mm.
By increasing the number of layers a decreasing of transmission
coefficient (S12) values accompanied by an increase of reflection
coefficient (S11) was measured (Fig. 3). This means that by varying
the nanofibers sample thickness the ratio between reflected and
absorbed energy power from the incident electromagnetic wave is
modified. We can also see that, for the same number of material layers,
with increase of particles concentration embedded in PVC matrix, the
values of transmission coefficients decrease, being for sample C
around −9.5 dB. Certainly, the most concentration sample has the
lowest transmission coefficient value.
In order to investigate the effect of a uniform magnetic field on the
transmission/reflection properties of the materials prepared in our
work the waveguide containing the samples was placed between the
poles of an electromagnet. The thickness of each sample was 4.5 mm.
The measured values of the transmission/reflection coefficients for a
set of magnetic field values (0–8200 Oe) are presented in Fig. 4. In
case of sample A containing 0.5 g of Fe3O4 nanoparticles embedded in
PVC matrix, the transmission/reflection coefficient varies around
0.5 dB when the magnetic field increases from 0 to 8200 Oe. Increasing
the amount of Fe3O4 nanoparticles determine a linear variation of trans-
mission/reflection coefficients (2 dB for sample B and 6 dB for sample
C) in the same interval of applied magnetic field. The lowest value of
the transmission coefficient was observed in the case of sample C at
3300 Oe and 12 GHz. As expected, the samples with higher particle
 O. Chiscan et al. / Materials Letters 68 (2012) 251–254
Fig. 3. Transmission S12 and reflection S11 coefficients for: composite nanofibers with
different amount of Fe3O4 particles: (A) — 0.5 g, (B) — 2.5 g, (C) — 5 g.
loads (samples B and C) show higher absorption energies in the
presence of a uniform magnetic field.
4. Conclusion
Using the electrospinning method we prepared PVC/Fe3O4
composite nanofibers with the iron oxide nanoparticles completely
embedded in the PVC matrix. These materials demonstrated low
values of the microwave transmission coefficient.
253
Fig. 4. Transmission and reflection coefficients dependence on magnetic field for: com-
posite nanofibers with different amount of Fe3O4 nanoparticles: (A) — 0.5 g, (B) — 2.5 g,
(C) — 5.0 g.
By varying the amount of Fe3O4 nanoparticles embedded in the
PVC matrix one can control the absorption properties of these mate-
rials in the X band (8–12 GHz).
The transmission loss of PVC/Fe3O4 nanocomposites measured in the
microwave frequency range of X-band was found to be below −16 dB
proving that these materials can be used as electromagnetic radiation
protection material.
254 O. Chiscan et al. / Materials Letters 68 (2012) 251–254

Acknowledgment [4] Epstein AJ, Miller JS. Synth Met 1996;80:231–7.

This work was financial supported by POSDRU/89/1.5/S/49944
(The Sectorial Operational Programme for the development of Human
Resources) in Romania.
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