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V. L. Kuznetsov O. Shenderova
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Abstract—A novel lightweight onion-like carbon (OLC)-based polymer composites find large-scale applications as antistatic
polymer composite with high electromagnetic (EM) shielding prop- materials, in printed electronics, supercapacitors, organic solar
erties is presented. OLC have been produced via the large-scale cells, biosensors, flexible transparent displays, etc. [1]. In spite
production technology based on the annealing of detonation nan-
odiamond under vacuum conditions (or in inert atmosphere). EM of the practical limitations of use because of their confined pro-
shielding effectiveness has been tested in the frequency range of cessability and manufacturing cost, dc and ac conductive com-
26–37 GHz. The highest EM attenuation at 36.6 GHz reaching posites are rapidly gaining attention in new applications such as
−34 dB was observed for polymethylmethacrylate films compris- packaging for electronics and chemical industry, metal replace-
ing 20 wt.% of OLC. The shielding effectiveness data collected ment, heating elements and fuel cells, and for EM shielding and
for microwave frequencies were found to correlate well with the
electrical resistivity measurements by four-probe method as well absorption in gigahertz and terahertz frequency ranges, where
as conductivity measurements provided by the broadband dielec- traditional radar materials [2], if not completely inapplicable,
tric spectroscopy (20 Hz–3 GHz). It was proved experimentally lose their attractiveness due to rising consumer wants.
that OLC EM shielding capacity can be optimized by varying the Among different fillers, the nanosized forms of carbon, such
nanoonion cluster size and nanodiamond annealing temperature as carbon black, carbon fibers, carbon nanotubes (CNTs) and
so that effective EM coatings can be produced. Both the experi-
mental observations and theoretical simulations demonstrate that their mixtures, exfoliated graphite, graphene related materials,
even small (smaller than percolation threshold) additions of OLC onion-like carbon (OLC), turned out to be especially attrac-
particles to a polymer host can noticeably modify the composite tive for the design of EM materials giving the benefit of both
response to EM radiation. lightweight and chemical inertness (see [3]–[13]). Note also that
Index Terms—Composites, electromagnetic shielding, nanoelec- in gigahertz and terahertz ranges, due to increasing utilization in
tromagnetics, onion-like carbon (OLC). EM materials of novel nanostructures, the classical electromag-
netic compatibility (EMC) faces new problems, while traditional
EM methods gain new life in their application to new objects.
I. INTRODUCTION On the way to new advanced EMC materials, the goal is to
HE current state of the art in the development of submil- achieve the synergy of well-known properties of host polymers,
T limeter, millimeter, and microwave electromagnetic (EM)
materials is determined, in many respects, by the success in the
e.g., polymethylmethacrylate (PMMA), polyurethane (PU),
epoxy resin, etc., with new potentialities originating from the
design, fabrication, and tailoring of artificial composite materi- fillers and providing the multifunctionality of the coatings and
als. Such materials, constituted by variously shaped electrically tailoring their properties. For example, CNTs, with their extraor-
small inclusions embedded in a host medium, can often exhibit dinary mechanical properties and unique electronic structure,
pronouncedly properties (chirality, anisotropy, and nonlinearity) being incorporated into the polymer matrix demonstrate impres-
unattainable on such a high level in natural media. Conductive sive shielding (see [5] and [12]). Due to the high aspect ratio of
CNTs, a low percolation threshold is expected to be observed,
which is important issue for producing effective EM coatings
with extremely low content of nanocarbon inclusions provided
Manuscript received May 12, 2011; revised July 16, 2011 and September 9, the maximal values of EM reflection/absorption. And indeed, a
2011; accepted October 11, 2011. Date of publication November 21, 2011; date number of papers (see [7] and [12]) have already reported a low
of current version February 17, 2012. This work was supported in part by the percolation threshold of CNT-based polymer composites.
ISTC Project B-1708, the NATO Grant CBP.EAP.CLG 983910, the EU FP7
BY-NanoERA Project FP7-266529 and Ministry of Education and Science of Also, it is important that individual nanocarbon inclusions
RF Grants RNP. 2.1.1/10256, and the RF state Contracts P339, P898. could display nonmonotonic frequency dependence of the EM
P. P. Kuzhir, A. G. Paddubskaya, and S. A. Maksimenko are with response in some frequency ranges coursed by the finite-size ef-
the Institute for Nuclear Problems, Belarus State University, 220030
Minsk, Belarus (e-mail: polina.kuzhir@gmail.com; paddubskaya@gmail.com; fects and provide, therefore, a resonant EM response of the com-
sergey.maksimenko@gmail.com). posite as a whole (for CNTs, see [11] and references therein).
V. L. Kuznetsov, S. Moseenkov, and A. I. Romanenko are with the It means that the individual inclusions cannot be regarded as
Boreskov Institute of Catalysis SB RAS, Novosibirsk 630090, Russia (e-mail:
kuznet@catalysis.nsk.su; moseenkov@catalysis.ru; air@che.nsk.su). producing a small perturbation of the EM field. Even more,
O. A. Shenderova is with the International Technology Center, Raleigh, NC the individual inclusion interaction within the nanocomposite
27715 USA (e-mail: oshenderova@itc-inc.org). is not limited to the multiple EM scattering as in the case of
J. Macutkevic and G. Valušis are with the Center for Physical Sciences and
Technology, LT-01108 Vilnius, Lithuania (e-mail: jan@pfi.lt; valusis@pfi.lt). macroscopic systems. Quantum mechanical effects come into
P. Lambin is with the Department of Physics, University of Namur, 5000 play, drastically influencing the polarizability of the constituting
Namur, Belgium (e-mail: philippe.lambin@fundp.ac.be). particles, and thus modifying the classical picture of the com-
Color versions of one or more of the figures in this paper are available online
at http://ieeexplore.ieee.org. posite EM response. In addition, the interelement conductivity
Digital Object Identifier 10.1109/TEMC.2011.2173348 and, consequently, the percolation effect in nanocomposites are
0018-9375/$26.00 © 2011 IEEE
KUZHIR et al.: CARBON ONION COMPOSITES FOR EMC APPLICATIONS 7
IV. ELECTRON TRANSPORT PROPERTIES OF OLC: Fig. 6. Frequency dependence of complex dielectric permittivity and electrical
DIELECTRIC ANALYSIS conductivity of OLC/PU composites at room temperature.
OLC demonstrates variable range hopping conductivity
(VRHC). For comparison with the quasi-1-D VRH model, the The broadband dielectric spectroscopy has been applied
temperature dependence of the dc conductivity σ(T ), is shown to study electrical conductivity and dielectric permittivity of
in Fig. 5 plotted as ln(σ) versus T−1/2 : OLC/polymer prepercolative and percolative composites in a
wide frequency (20 Hz–3 GHz) range at room temperature
1/2
T0
σ(T ) = σVRH (T ) = A exp − (1) (see [21] and references therein).
T The frequency dependence of the room-temperature dielectric
permittivity and conductivity of Db-1650/PU composites with
for the OLC samples produced at different temperatures. In (1),
different OLC concentration is shown in Fig. 6. The dielectric
A is a constant, T0 = CT a/k B N (EF ), CT ∼ 16, and a is
permittivity and conductivity for films with OLC concentration
the inverse length on which the amplitude of wave function
up to 7.8 wt.% are very low; their values are very close to that
falls down (a ∼ 60 Å for OLC). The slope of the temperature
of pure PU. However, dielectric permittivity and electric con-
dependences of conductivity with VRHC as given by (1) is
ductivity are very high for composites with 15 wt.% of OLC
determined only by the density of states at Fermi level N (EF ).
inclusions at low frequencies, ε is in order of 102 –104 , and σ
Estimation of density of states of carriers at Fermi level
is about 0.03–4 S/m. The complex dielectric permittivity value
N (EF ) in OLC was based [8] on the approximation of the tem-
is very similar to that for multiwalled CNTs nearly percolation
perature dependence of conductivity expression (1) was carried
threshold [12]. The loss tangent is also very high at low frequen-
out for different series of OLC produced from ND of differ-
cies (approximately 103 ), indicating a high absorption ability of
ent vendors. The increase of the annealing temperature from
EM waves by percolatiove composite (with 15 wt.% of OLC).
1400 K up to 1800 K leads to increase of the density of states
It means that we can expect significant EM shielding ability of
at Fermi level and consequently increasing of the carrier con-
OLC-based composites.
centration. Some variation of density of states at the Fermi level
was observed for OLC of different size of agglomerate, being
V. MODELING
slightly larger for larger aggregates. Thus, we can operate den-
sity of states at Fermi level N (EF ) in investigated samples via The classical instrument for the composite EM response mod-
variation of the annealing temperature, choice of background of eling is the Maxwell Garnet effective medium approach and its
preparation of initial NDs and using of the specific fractions of modifications accounting for additional influencing factors, such
OLC. as composite’s nonhomogeneity [26] or percolation effect [27],
KUZHIR et al.: CARBON ONION COMPOSITES FOR EMC APPLICATIONS 11
TABLE III
EM ABSORPTION, REFLECTION, AND TRANSMISSION OF OLC/PMMA
AND OLC/EPOXY COMPOSITES AT 30 GHZ AND DIFFERENT
CONCENTRATIONS OF OLC OF Dd-1800 Type
adhesion could lead to increase of the contact resistivity and [12] P. Kuzhir, A. Paddubskaya, D. Bychanok, A. Nemilentsau, M. Shuba,
decrease conductivity of composite as a whole [34]. A detailed A. Plushch, S. Maksimenko, S. Belucci, L. Coderoni, F. Micciulla,
I. Sacco, G. Rinaldi, J. Macutkevic, D. Seliuta, G. Valusis, and J. Banys,
dielectric analysis within the wide temperature range is needed “Microwave probing of nanocarbon based epoxy resin composite films:
to study the problem of interactions between the fillers and the Toward electromagnetic shielding,” Thin Solid Films, vol. 519, pp. 4114–
polymer molecules; structural relaxation process in the given 4118, Apr. 2011.
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[14] M. V. Shuba, G. Ya. Slepyan, S. A. Maksimenko, C. Thomsen, and
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dimensional structures,” in The Handbook of Nanotechnology: Nanome-
The reported results demonstrate that OLC is an interesting ter Structure Theory, Modeling, and Simulation, A. Lakhtakia, Ed.
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KUZHIR et al.: CARBON ONION COMPOSITES FOR EMC APPLICATIONS 15
[32] V. L. Kuznetsov, Y. V. Butenko, A. L. Chuvilin, A. I. Romanenko, and Vladimir L. Kuznetsov received the Diploma de-
A. V. Okotrub, “Electrical resistivity of graphitized ultra-disperse diamond gree in chemistry from Novosibirsk State Univer-
and onion-like carbon,” Chem. Phys. Lett., vol. 336, pp. 397–404, Mar. sity, Novosibirsk, Russia, in 1973, and the Ph.D.
2001. degree from the Boreskov Institute of Catalysis,
[33] T. Xiao, H. L. Yang, and G. P. Zhang, “The influence of carbon nanotube Novosibirsk, in 1978.
structure on complex permittivity and determination of filler density by He started his career at Boreskov Institute of
microwave techniques,” J. Appl. Phys.,, vol. 110, pp. 024902-1–024902-5, Catalysis in 1973, where he was a Junior Research
2011. Scientist, Senior Research Scientist. In 1986–1991,
[34] Y. Zeng, P. Liu, J. Du, L. Zhao, P. M. Ajayan, and H.-M. Cheng, “Increasing he was a Scientific Secretary of the Boreskov Institute
the electrical conductivity of carbon nanotube/polymer composites by of Catalysis, where he was the Head of laboratory,
using weak nanotube–polymer interactions,” Carbon, vol. 48, pp. 3551– and the Head of Information Center in 1994–2003.
3558, 2010. In 1978–1979, he was a Postdoctoral Researcher at the University of California,
Berkeley. He was also a Visiting Scientist at Case Western Reserved University,
Drexel Universtity, and the Swiss Federal Institute of Technology Lausanne.
Currently, he is the Head of research group at the Boreskov Institute of Cataly-
sis and a lector of the course Molecular Design of Catalysts in Novosibirsk State
Polina P. Kuzhir received the M.S. degree in theoret- University. His research interests include tailor-made catalysts; synthesis and
ical physics from Belarusian State University, Minsk, investigation of surface compounds; ultradisperse materials (cluster derived cat-
Belarus, in 1991, and the Ph.D. degree in high en- alysts, aerogels of SiO2 , detonation soot, nanodiamond, and onion-like carbon,
ergy physics from the Institute of Physics, Belarus carbon nanotubes); and growth and characterization of SiC whiskers, carbide-
Academy of Science, Minsk, in 1996. derived nanocarbons, carbon nanotubes, composites containing nanocarbons.
She is currently a Senior Researcher at the Re- He is the author or coauthor of more than 160 articles in refereed journals,
search Institute for Nuclear Problems, Belarus State nearly 200 conference papers, and five book chapters.
University. She has been working in Particle Physics
and Quantum Field Theory for more than 15 years.
She is actively involved in the theoretical and ex-
perimental research of electromagnetic response of
nanocarbon composite materials. At the same time, she contributes to the pio-
neering investigation of the potential of nanotubes and graphene as monomolec-
ular light emitters in the terahertz frequency range.
Olga A. Shenderova received the Ph.D. degree Gintaras Valušis received the Diploma degree from
in computational materials science from the St. the Faculty of Physics, Vilnius University, Vilnius,
Petersburg State Technical University, Petersburg, Lithuania, in 1985, where he received the Ph.D. de-
Russia, in 1991. gree in 1992.
She has been a Senior Scientist and the Head of the He was a Postdoctoral Researcher at the Insti-
Nanodiamond Laboratory, International Technology tute of Applied Photo Physics, Dresden University
Center, Raleigh, NC, since 2001. During her appoint- of Technology in 1995–1996. In 2000, he was an
ment at North Carolina State University in 1995– Alexander von Humboldt Fellow at Physics Institute,
2001, she performed atomistic simulations of me- J. W. Goethe University, Frankfurt, Germany. Cur-
chanical and electronic properties of carbon nanos- rently, he withholds positions of a Deputy Director
tructures. She is the author or coauthor of more than for development in the Center for Physical Science
100 papers in peer-reviewed journals, including more than ten chapters in the and Technology, Head of the Terahertz Photonics laboratory, and Professor in
books. She is an Editor of four books on Nanodiamond. Her research interests Semiconductors Physics Department, Physics Faculty, Vilnius University.
include nanodiamond (ND) and onion-like carbon (OLC) particles modification
and fractioning, development of ND and OLC composites with polymers, and
optical and biological applications of ND and OLC.
Jan Macutkevic was born in Vilnius, Lithuania, in Philippe Lambin received the M.S. degree in phys-
1980. He received the B.S. degree in electronic en- ical engineering from the University of Liège, Liège,
gineering in 2000, the M.S. degree in 2002, and the Belgium in 1976, and the Ph.D. in physical sciences
Ph.D. degree in physics in 2006 from Vilnius Univer- in 1981, from the same university.
sity, Vilnius. After joining the University of Namur, Namur,
He is currently with Terahertz Photonics Labo- Belgium, he went to the IBM Research Center, San
ratory, Center for Physical Science and Technology Jose, CA, as a Visiting Scientist in 1983–1984. He
and Dielectric Spectroscopy Laboratory, Vilnius Uni- then joined the University of Namur as a Research
versity as a Senior Research Associate. His current Associate of the Foundation for Scientific Research
research interests include dielectric properties of fer- of Belgium, where he became a Professor in 1995 and
roelectric relaxors, carbon nanotubes, onion-like car- a Full Professor in 2004. He was successively a Dean
bon, and composites based on these materials in very wide frequency range from of the Faculty of Sciences in 2005–2008 and a Vice-Rector of the University of
hertz to terahertz. His recent research has also focused on developing active and Namur in 2008–2011. His research interests include theoretical physics of the
passive device for terahertz applications. condensed matter and nanomaterials.