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Carbon onions for electromagnetic applications

Article · August 2010


DOI: 10.1109/URSI-EMTS.2010.5637245

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6 IEEE TRANSACTIONS ON ELECTROMAGNETIC COMPATIBILITY, VOL. 54, NO. 1, FEBRUARY 2012

Carbon Onion Composites for EMC Applications


Polina P. Kuzhir, Alesia G. Paddubskaya, Sergey A. Maksimenko, Vladimir L. Kuznetsov, Sergey Moseenkov,
Anatoly I. Romanenko, Olga A. Shenderova, Jan Macutkevic, Gintaras Valušis, and Philippe Lambin

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

governed by electron tunneling through the contact potential


barrier (multichannel in general case), which is irrelevant in the
macroscopic case (see [14] for the case of tunneling in mul-
tiwalled CNTs). Hence, adequate physical analysis of such a
composite is possible only by utilizing the nanoelectromagnet-
ics approach [15], where the boundary-value problem is raised
and solved in accordance with the quantum transport problem.
One more principal peculiarity of the nanocomposites is their
structural disorder: the shape, size, and spatial localization of
the individual fillers fluctuate and the fluctuations must be ac-
counted for both at the simulations of the nanocomposite EM
response and at the engineering of composites properties.

II. TARGET SETTING


There are many possibilities to control EM properties of
nanocarbon-based composites and, therefore, to manage their
EM shielding abilities, ranging from the alteration of the topol-
ogy and polarizability of individual constituents to control elec-
tromagnetism of assemblies of nanocarbon clusters, dielectric
response of the host matrix and its affinity to carbon fillers. In
this paper, we focus on the EM properties of novel technological
material—OLC [16]–[19] and OLC-based polymer composites.
Recently, several results have been arguing for promising
shielding capabilities of OLC at microwave frequencies (see [8],
[20], and [21] for experimental observations and [22]–[24]
for the theory). These articles demonstrated that OLCs (see
Fig. 1)—stable defected multishell fullerene obtained by ther-
mal transformation of nanodiamonds (ND)—are promising
nanostructures for the use as fillers for the manufacture of wide-
band EM composite materials. In this paper, we summarize our
experience in dealing with this new innovative material—onion
synthesis technology, composites fabrication, dc, and dielectric
analysis—and, on the basis of new experimental data collected
in low-frequency and microwave ranges, give systematic view
on how to utilize OLC for producing effective EM coating.
An interesting feature specific to OLCs comes from their abil-
ity to form agglomerates, often covered by common graphitic
mantle, leading to a so-called pod-of-peas geometry [23]. Typ-
ical size of the OLC agglomerates, depending on the method of
OLC preparation, lies within 100–200 nm (see Fig. 2).
Quantum-chemical calculations, together with features ob-
served in the X-ray emission spectra of OLCs [18], indicate that
onions produced by ND annealing at an intermediate temper-
atures (1400–1800 K) have holes in their internal shells. That
structure can be explained by deficiency of carbon atoms ar-
ranged to the diamond cubic structure in order to be transformed
into perfect spherical graphitic shells during annealing. As a re-
sult, nonperfect fullerene-like inner shells are formed. Hence, Fig. 1. HRTEM image of OLC (Dd series) produced at (a) 1400-, (b) 1600-,
structural defects (sp-hybridized carbon atoms constituted the and (c) 1800-K annealing temperature.
boundaries of holes in the spherical graphitic shells and dangling
bonds) are concentrated in the inner cores of the OLCs and are
well protected from the ambient by the outer, more defect-free carbon nanoonions produced, for example, by electric arc dis-
shells and interact with an external EM field, contributing to the charge in water, with average size of primary particles of 25–
overall EM attenuation. 30 nm [19]. We expect that OLC due to their lightness will allow
Since the average size of a primary OLC particle is about reducing significantly the weight of the coatings while keeping
4–7 nm, OLC possesses higher dispersability as compared with high EM attenuation efficiency.
8 IEEE TRANSACTIONS ON ELECTROMAGNETIC COMPATIBILITY, VOL. 54, NO. 1, FEBRUARY 2012

Fig. 2. Volumetric size distribution of OLC sample of the De-series in DMF


(photon correlation spectroscopy data (see Section III).
Fig. 3. Scheme of formation of sp3 /sp2 composites and OLC [8].

A potential advantage of OLC is the availability of relatively


low-cost fabrication technology. However, in order to succeed in OLC structure. Due to the aggregation of primary ND, its an-
the design and fabrication of OLC-based polymer films as effec- nealing products (OLC particles) are organized into aggregates
tive EM coatings, specific scientific and engineering problems with joint defective graphene shells covering several primary
must be solved, such as technology optimization of the OLC OLC cores. Content of iron impurities in OLC does not exceed
incorporation into host matrix and their dispersing in specific 0.1 wt%.
solutions, achieving evaluation of the affinity of carbon particles OLC of Dd and De types were produced as follows. First, ND
with corresponding polymer molecules. This paper reports also powder was heated with rate 5◦ /min in argon flow 35 cm3 /min
on the dielectric spectroscopy of OLC-based polymer films as a up to 850 ◦ C and was annealed at this temperature for 1 h. Then,
tool for exploring these particular problems while developing a the sample was annealed at high vacuum (10−6 torr) at tempera-
new family of effective wideband EM materials with improved tures 1400 K (De-1400, Dd-1400), 1600 K (De-1600, Dd-1600),
thermal stability as a main task. and 1800 K (De-1800, Dd-1800), correspondingly. Cooling was
That is why various homogenization procedures taking into done at a rate 20◦ /min down to 500 ◦ C using diffusion pump.
account all the mentioned factors should be applied. Here, along Packed density of OLC powder samples changes from 0.306 to
with the experimental results collected for OLC-based compos- 0.530 g/cm3 as compared to initial ND sample.
ites in different frequency ranges, a theoretical simulation is NDs for producing OLC of Db-1650 type were purchased
presented, comprising semiempirical microscopic calculations from New Technologies, Chelyabinsk, Russia. Average primary
of the OLC polarizability and a Maxwell–Garnett homogeniza- particle size of ND was 4 nm and average volumetric aggregate
tion procedure aimed at accounting for the OLC size distribu- size was 120 nm. To achieve fully transformed ND into OLC,
tion [24]. NDs were heated in vacuum 10−4 torr at 1650 K for 3 h. Size of
primary OLC particles is around 6–7 nm, while average aggre-
gate size is 130 nm for OLC dispersed in N -methylpyrrolidone
III. EXPERIMENTAL DETAILS (NMP) as measured by dynamic light-scattering technique.
The precursor NDs were synthesized at high-pressure and The size (volumetric) distribution of particles in OLC
high-temperature conditions within a shock wave during deto- samples presented in Fig. 2 has been measured in N, N-
nation of carbon-containing explosives with a negative oxygen Dimethylformamide (DMF) by means of photon correlation
balance. The particles were extracted from the detonation soot spectroscopy using Nicomp 380 ZLS PCS Spectrometer. High
by oxidative removal of nondiamond carbons using strong ox- dispersion state of OLC particles in DMF was achieved for
idizers. Following the procedure described in [16], OLC ma- 1 mg/ml concentration by sonication for 10 min. During the
terials were produced by annealing of ND powder in vacuum measurements, this suspension was diluted down to 0.05 mg/ml
at high temperature. Controllable graphitization in vacuum of concentration. In Fig. 2, one can see that the volumetric size
the explosive ND within the temperature range 1200–1800 K distributions of particles in the investigated OLC samples are
allows us to produce the sp2 /sp3 composites (see Fig. 3). ND unimodal. The average size of the OLC aggregates is 143, 147,
with the size of primary particle ∼8–10 nm (De series) and and 85 nm for Dd-series (for annealing temperature 1400, 1600,
4–5 nm (Dd series) were obtained from “Alit” (Kiev, Ukraine and 1800 K, respectively) and 95, 162, and 190 nm for De-1400,
[http://www.alit.kiev.ua/products.htm]) and FGUP ALTAI De-1600, and De-1800 correspondently. Db-1650 effective clus-
(Biysk, Russia [http://www.frpc.risp.ru/uda/index.shtml]), cor- ter diameter is 130 nm. For OLC, DMF can be considered as the
respondingly. As annealing temperature is increased, the ra- universal solvent. Thus, the observations of larger aggregates
tio between diamond core and outer defective curved graphitic for De-series of OLC as compared to Dd-series reflect the real
shells (sp2 /sp3 nanocomposites) decreases, finally resulting in difference in size of the aggregates.
KUZHIR et al.: CARBON ONION COMPOSITES FOR EMC APPLICATIONS 9

OLC/PMMA composites were prepared via coagulation tech-


nique described in [20] and [25]. NMP and DMF were chosen
as solvents for dispersion of OLC due to their high ability to
solvate nanocarbon particles and stabilize corresponding sus-
pension during ultrasonication. A calculated amount of OLC
was dispersed in 60 ml of NMP using horn sonicator with fre-
quency 22.5 kHz and power up to 900 W (InLab Il-6.3, Russia)
during 10 min. After sonication, 40 ml of the PMMA/DMF so-
lution with PMMA concentration 0.05 g/l was added to OLC
suspension and the mixture was additionally sonicated during
10 min. After this procedure, black dispersion of OLC (100 ml)
was quickly poured into 800 ml of distilled water (50–60 ◦ C) un-
der vigorous stirring using magnetic stirrer. Immediately after
mixing with water, PMMA began to precipitate from solution
forming amorphous deposit with color varying from light-gray
to intensively black (depending on OLC content in composite).
Precipitated deposit was filtered using Buchner funnel with pa-
per filter, washed with distilled water for 5–7 times, and dried on
Fig. 4. Optical microscope image of 5 wt% concentration of OLC (a) in epoxy
filter in air. Composites were additionally dried using vacuum and (b) in PMMA for Dd-1800 type of OLC inclusions. (c) Optical microscope
pump and water bath, milled and used for the preparation of image of a thin slice of OLC/PMMA composite with 2 wt% concentration of
polymer films with a hot-pressing technique. Composite films OLC of De-1800 type. SEM images of OLC/PU composites for 3.8 wt% of OLC
inclusions (Db-1650 series). (d) Arrows indicate locations of OLC aggregates.
were produced via hot-pressing of milled powders of dried com-
posites at 200 ◦ C using hydraulic pressing apparatus with load-
ing up to 2 tons. Finally, produced films were uniformly black
regardless of OLC content with thickness 0.5 mm and diameter one pair of contacts and the voltage drop is measured on the
up to 60 mm. second pair. This allows for elimination of the resistance of
OLC/epoxy samples were prepared as follows. Epoxy resin contacts from a measured value, as the measuring current does
was dissolved with acetone (1:10) and calculated amount of not pass through potential contacts. The OLC powders were
OLC powder was distributed in resulting mixture using ultra- pressed into a glass tube (dint = 2 mm) until the resistivity
sonicator for 10 min. Produced suspension was placed in dry- ceased to depend on the degree of compression. A silver wire
ing oven and heated at 40–45 ◦ C overnight for removal of ace- with a diameter of 0.1 mm provided the electric contact. The
tone residues. Dried epoxy resin was mixtured with hardener sample temperature was measured using an iron–rhodium resis-
(1:1) and pressed between polished Teflon disks with 0.5-mm tance thermometer [8].
spacer. Produced plates were removed from Teflon surface, cut Complex dielectric permittivity ε∗ = ε − iε was measured
in pieces, and used for future investigations without additional as a function of frequency and temperature using an HP4284A
treatments. precision LCR meter in the frequency range 20 Hz–1 MHz and
OLC/PU samples were produced as follows. OLCs of by vector network analyzer Agilent 8714ET in frequency range
Db-1650 type were mixed at different mass ratios with commer- 1 MHz–3 GHz. The sample was placed in the coaxial line be-
cial formulation of oil-based PU minwax clear satin containing tween the inner conductor and short end, which were fresh
60% of volatile compounds. After mixing with the OLC pow- polished for each measurement for better electrical contact. Sil-
der, the polymer suspension was stirred at 400 r/min overnight at ver paste has been used for contacting. The real part of complex
40 ◦ C. Then, the suspension was casted on a Teflon substrate and electrical conductivity σ  was calculated via σ  = 2πνε0 ε , with
dried at ambient conditions at 45 ◦ C overnight. The thicknesses ε0 being the permittivity of vacuum.
of OLC/PU films varied between 250 and 700 μm. The microwave measurements were provided by scalar net-
The uniformity of distribution of the OLC fillers in the OLC- work analyzer R2-408R (ELMIKA, Vilnius, Lithuania) set in-
based polymer samples was studied by optical microscopy cluding a sweep generator, a waveguide reflectometer, and an
(magnification 100) and SEM JSM-6460 LV (see Fig. 4). Fabri- indicator unit (personal computer). The EM response of sam-
cated coatings demonstrate good quality and nanocarbon inclu- ples as ratios of transmitted/input (S21 ) and reflected/input (S11 )
sions are reasonably well dispersed. While the size of OLC ag- signals has been measured within 26–37 GHz frequency range
glomerates in highly dissolved suspension is lower than 200 nm, (Ka-band). The frequency stability of the oscillator was con-
coagulation, e.g., of PMMA and OLC solution in DMF with trolled by frequency meter and was as high as 10−6 . The
higher concentration, leads to the formation of larger agglomer- power stabilization is provided on the level of 7.0 mW ±
ates with the size up 5 to 20–30 μm, which are clearly observed 10 μW. Measurement range of EM attenuation is from 0 to
as dark contrast objects on optical micrographs. −40 dB. Basic measurement errors of EM attenuation over the
Four-point probe dc measurements of resistance versus tem- range 0–25 dB and −25–40 dB are δA = ±(0.6 + 0.06A) and
perature at 4.2–300 K with an error of about 0.1% were per- δA = ±(−0.4 + 0.1A) correspondingly, where δA is the mar-
formed. According to this method, the current flows through gin of error and A is the measured EM attenuation. The accuracy
10 IEEE TRANSACTIONS ON ELECTROMAGNETIC COMPATIBILITY, VOL. 54, NO. 1, FEBRUARY 2012

Fig. 5. The temperature dependence of OLC conductivity σ(T ), annealed at


temperature 1400, 1600, and 1800 K. Continuous lines correspond to depen-
dence (1) [8].

has been controlled by repetitive measurements for different ori-


entations of the sample in the waveguide cross section. When
polymer films have been analyzed, the cured specimens were
cut precisely to the waveguide cross section 7.2 × 3.4 mm.
S-parameters were measured by subsequent inserting specimen
into waveguide. The measurements were performed with free-
standing polymer films.

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

[28]. The percolation effect theories give a phenomenologi-


cal equation for the conductivity (resistivity) of a composite
medium close to the metal–insulator (conductor to perfect con-
ductor) transition. Although largely developed in the context of
regular lattices, these theories are widely used to describe the
conductivity of continuum systems such as metal—metal–oxide
and graphite–polymer mixtures.
The size and shape effect on the complex permittivity are
understood to make a major contribution along with the volume
fraction to the EM response of the mixture. That is why the
adequate modeling of the EM properties of composite materials
with complex inclusions embedded (such as, e.g., OLC) is ex-
tremely important before manufacturing, sometimes expensive,
of new EM materials those EM parameters are strongly affected
by the fillers geometry.
Fig. 7. Temperature dependence of the dielectric permittivity of OLC
In this section, we briefly dwell on modified effective medium (Db-1650)/PU composites at ν = 129 Hz (theoretical predictions and ex-
approach taking into account the shape anisotropy and size dis- perimental data for (a) 1.9, (b) 3.8, and (c) 7.8 wt% concentration of OLC
persion of nanosized fillers. A polymer composite containing inclusions).
well-dispersed nanoparticles is equivalent to an effective ho-
mogeneous medium if inclusions are electrically small, i.e., for As a next step, we introduce a continuous distribution of parti-
EM wavelengths much larger than the length scale that charac- cles by radius R given by the distribution function ϕ(R) normal-

terizes the nonhomogeneities—the typical size of nanoparticles ized as 0 ϕ(R)dR = 1. And we come to the expression for the
and distance between them. For OLC or OLC clusters, this effective dielectric function of the multicomponent composite
condition is certainly fulfilled for far infrared and lower fre- with quasi-spherical inclusions
quencies. Thus, the Maxwell Garnet homogenization procedure ∞
can be applied. 1 + 23 f 0 ϕ(R)α(ω, R)dR
εeff (ω) = εh ∞
Consider a composite medium formed by identical electri- 1 − 13 f 0 ϕ(R)α(ω, R)dR
cally small particles embedded in a homogeneous isotropic di- which can be used for estimating the EM response of OLC-based
electric host with the permittivity εh . The spatial distribution of polymer composite.
nanocarbon inclusions is assumed to be random. The fillers can For the numerical estimate, we have used the static polar-
be considered as point-like objects with a given polarizability izability α(0, R) calculated in [23] for icosahedral fullerenes
calculated according to [22] and [23]. The complex effective C1280 , C720 , C240 , and C60 , for Stone–Wales rounded fullerenes
permittivity of this mixture depends not only on volume frac- C2000 , C1280 , and C720 ; and for pod-of-peas fullerene C5540
tion of scatters, but also on their size and shape since the scatter containing three “peas” of spherical C720 . The frequency depen-
polarizability depends on both these parameters: icosahedral dence of the permittivity of nanocarbon-based polymer compos-
fullerenes, spherical onions, pod-of-pies structures [23], collec- ite at a given temperature is approximated using the electrostatic
tions of multishell fullerenes, model real agglomerated OLC interaction model developed in [29] for the frequency-dependent
material, etc. molecular polarizability and valid for the low-frequency range
We shall consider a composite material with some size dis- below the terahertz and optical resonances
tribution as multicomponent composite material. Let the OLC
cluster shape be close to spherical and let the composite com- α(ω, R) = α(0) + c(R)ω 2
prises N components enumerated further by the index j = 1,
where the coefficient c(R) increases with the mean fullerene
2, . . . , N, and fj be the volume fraction of jth component. Fur-
radius as c(R) = 0.419 · 10−32 R 3.469 .
ther, we assume fj  1 for arbitrary j. Then, we model the
We can suppose that the multishell fullerenes (OLC) are ther-
composite as a single-component one comprising particles of
mally stable at least up to the matrix melting temperature [24].
the j type; all other N − 1 components are tentatively included
The results of theoretical modeling of EM response of OLC/PU
into the host with the dielectric function ε̃h1 . Next, the host
films with the different content of nanocarbon inclusions are
medium is considered as a single-component composite com-
presented in Fig. 7. The theoretical predictions are supported
prising particles of the j = 2 type; all other N − 2 components
well by the experimental data collected for 129 Hz in wide tem-
are tentatively included into the host with the dielectric func-
perature range for a series of prepercolative PU samples with
tion ε̃h2 . Then, recurrence transformation leads to the effective
OLC embedded (up to 7.8 wt%).
dielectric function expressed in terms of the dielectric func-
tion of the host medium εh and polarizabilities and densities of
inclusions VI. MICROWAVE ANALYSIS
 The permittivity of the investigated composites were recon-
1 + 23 N j =1 fj αj (ω) structed, as presented in Table I, from the transmittance and
εeff (ω) = εh N .
1 − 3 j =1 fj αj (ω)
1
reflectance measured in a rectangular waveguide with a cross
12 IEEE TRANSACTIONS ON ELECTROMAGNETIC COMPATIBILITY, VOL. 54, NO. 1, FEBRUARY 2012

TABLE I mer coat cannot interact effectively with EM field. In contrast,


DIELECTRIC PERMITTIVITY AT 30 GHZ FOR THE DD-SERIES OLC ANNEALED
AT DIFFERENT TEMPERATURES AND INCORPORATED INTO PMMA IN
polarizability of OLC aggregates annealed at 1800 K is high
DIFFERENT CONCENTRATIONS enough [23] and this screening effect of matrix is not exhibited.
Reflectance (R), absorbance (A), and transmission (T ) of
the EM radiation on the sample can be determined as follows:
R = S11 2 2
; T = S21 ; A = 1 − R − T.
The thicknesses of OLC/polymer samples used for microwave
analysis were between 0.4 to 2 mm. All results collected using
scalar analyzer for transmitted/input (S21 ) and reflected/input
(S11 ) signals within 26–37 GHz were recalculated through the
procedure of dielectric permittivity reconstruction (2), (3) for
the same thickness in 2 mm of EM coating.
Finding a way to manage the high-frequency conductivity of
section a × b (in x- and y-directions correspondingly) using the OLC fillers and their possibility to attenuate the EM signal in
following procedure developed in [30]: microwave frequency range as much as possible, the series of
polymer samples with 2–20 wt% of OLC inclusions annealed at
2(kz 2 /kz )
T = (2) different temperatures were analyzed.
2(kz 2 /kz ) cos(kz 2 τ ) + i[(kz 2 /kz )2 + 1] sin(kz 2 τ ) The maximal values of EM attenuation S21 in −34 and
−j[(kz 2 /kz )2 − 1] sin(kz 2 τ ) −32 dB were observed for Dd-1800 and De-1800 series of
R= (3) OLC correspondently embedded in PMMA in 20 wt%. It has
2(kz 2 /kz ) cos(kz 2 τ ) + i[(kz 2 /kz )2 + 1] sin(kz 2 τ )
been found (see Fig. 8) that raising the annealing temperature
where τ is the thickness of the nanocarbon-based layer, kz is leads to enhanced absorption ability of OLC-based composites,
the longitudinal wave number, z isthe direction along the wave- which is in perfect agreement with the results for dc conduc-
guide, numbers kz (1,3) = (π/λa) 4a2 − λ2 , λ is the free space
 tivity measurements presented in Fig. 5. Indeed, OLC annealed
wavelength, kz 2 = (π/λa) 4εa2 − λ2 , and ε is the complex at 1400 K do not demonstrate valuable EM attenuation: even
permittivity of the investigated sample ε = ε − iε . The real 20 wt% of OLC provide only 19% of microwave signal absorp-
(imaginary) part of dielectric permittivity of neat PMMA mea- tion and 26% of reflection. At the same time, Dd-1600 produced
sured at 30 GHz is 2.12 (0.01) correspondently. at 1600 K absorbs already 40% of microwaves being incorpo-
Microwave probing of OLC composites (see Table I) shows rated in PMMA within the same percentage. Dd-1800 fabri-
that ND annealed at any of three temperatures, being incorpo- cated at 1800 K absorbs practically 60% of microwave energy
rated into polymer in a small concentration (2–5 wt%, i.e., far at 20 wt% concentration. This property of OLC correlates with
from the percolation threshold [31]) does not affect essentially the observed increase of density states of conductive electrons
the dielectric permittivity of composite in comparison with the in OLC material produced at high temperature [8]. The reason is
permittivity of neat matrix. Starting from 10 wt% of OLC con- that OLC with the dielectric diamond core inside, being sp3 /sp2
centration, the OLC/PMMA composites demonstrate some in- composite (samples annealed at 1400 K at 1600 K), transforms
crease of both real and imaginary parts of permittivity for OLC step-by-step into onions, when annealing temperature is 1800 K.
prepared at 1600 and 1800 K. The increase in annealing temperature does not only promote
Significant growth of permittivity is inherent to 20 wt% ND core graphitization but also results in the formation of more
content of OLC annealed at intermediate (1600 K) and high perfect prolonged conductive tracks within OLC agglomerates.
(1800 K) temperature in favor of OLC-1800: the rise of ε (ε ) The reflection ability of OLC annealed at different temper-
from 2.12 (0.01) to 7.01 (1.39) takes place for OLC/PMMA ature is actually the same on the level of 20% demonstrat-
with 20 wt% of OLC in comparison with neat PMMA. This ing slightly nonmonotonous dependence on concentration for
result is in good agreement with the data collected in dc exper- OLC annealed at intermediate temperature 1600 K [see Fig. 8(a)
iment (see Fig. 5), where substantial increase of conductivity and (b)].
has been observed with the rise of the annealing temperature of As was shown in [20], EM attenuation in Ka-band provided
precursor ND. At the same time, due to high screening effect of by 0.8-mm-thick layer of OLC powders is strongly dependent
the host the permittivity of prepercolated composites fabricated on the OLC cluster size, being significantly higher for longer
with OLC annealed at small (1400 K) and intermediate (1600 K) nanoonions clusters (De series, which is characterized by the
temperatures can be even slightly lower than permittivity of pure larger average cluster size). This conclusion is in good agree-
polymer (e.g., for 2 wt% of Dd-1600 in PMMA) or can demon- ment with our theoretical prediction for OLC polarizability to
strate minor nonmonotonous dependence on concentration (e.g., be dependent linearly on the OLC cluster volume [23]. Both
for 5 and 10 wt% of Dd-1400 inclusions). This is because the experimental results and theoretical estimates coincide with the
dielectric diamond core inside just-formed onion annealed at increase in conductivity of OLC powder produced from NDs
1400 and 1600 K (see scheme of formation of sp3 /sp2 compos- having larger average size of the nanocarbon aggregates [8].
ites, Fig. 3) is in the nature of relatively low polarizability of This behavior can be described as follows: the increase in
individual OLC particle formed at 1400 and 1600 K [32]. Such OLC mean aggregate diameter results in the formation of more
sp3 /sp2 particles and their clusters being preserved by poly- perfect prolonged conductive tracks within OLC material. At the
KUZHIR et al.: CARBON ONION COMPOSITES FOR EMC APPLICATIONS 13

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

OLC particles characterized by smaller average cluster size (the


average size of the OLC aggregates is 85 nm for Dd-1800 sam-
ple and 190 nm for De-1800) demonstrates significantly lower
percolation threshold [31]. It also agrees with the results for
multiwalled CNT of different mean diameter [33]: the EM atten-
uation in microwaves was observed to be higher for the samples
with the finest CNT embedded within the same percentage and
do not depend directly on the electrical conductivity of individ-
ual filler. That is Dd-1800 and De-1800 fillers within 10 wt%
in PMMA demonstrate the same EM attenuation (see Table II),
but Dd-1800-based polymer sample with 20 wt% of nanocarbon
inclusions being close to a percolation threshold corresponding
to this type of OLC demonstrates maximal possible EM absorp-
tion, whereas De-1800/polymer will reach maximal values of
EM attenuation when OLC content will reach approx. 25 wt%.
This peculiarity of OLC and OLC-based composites has to
be taken into account when effective EM shielding materials
fabricated.
Nevertheless, the qualitative dependence of EM attenuation
on OLC concentration provided by the same types of OLC
embedded into different polymers (PMMA, PU, epoxy, cellu-
lose, etc.) are similar to each other [8], [20], [21], [23] because
EM constitutive parameters of OLC/polymer composites are
Fig. 8. EM absorption (A), reflection (R) and transmission (T) of OLC/PMMA
composites at 30 GHz versus OLC concentration. OLC of Dd-type were an-
determined mostly by type of OLC (first of all by ND anneal-
nealed at (a) 1400, (b) 1600, and (c) 1800 K. ing temperature and OLC average cluster size) as seen from
Tables I and II. In order to reveal the influence of the host poly-
TABLE II mer on the EM properties of OLC-based coatings in Ka-band,
EM ABSORPTION, REFLECTION, AND TRANSMISSION OF OLC/PMMA the EM response of the same type of OLC (Dd-1800) incorpo-
COMPOSITES AT 30 GHZ FOR OLC OF Dd- and De-series, Annealed
at 1800 K and Different Concentrations of the Inclusions rated into epoxy and PMMA within the same weight percentage
was compared in Table III.
One can see that the EM reflection provided by OLC is slightly
higher when they are embedded into PMMA host matrix, but EM
absorption increases when OLC are incorporated into epoxy.
Finally, 10 wt% of nanoonions provide the same attenuation
of microwave signal being embedded into both PMMA and
epoxy resin, but the contribution of reflection and absorption
mechanisms is different. That is OLC of different types, de-
pending on the synthesis conditions (first of all on the sur-
same time, the increase in the average cluster size of nanocarbon face chemistry), have different affinity for the host polymer: we
inclusions into polymer in large concentration (20 wt%) did not suppose that higher adhesion of polymer and OLC agglomer-
result in increase of EM absorption (see Table II). ates provide formation of more homogeneous distribution of
Indeed, on one hand, OLC with larger mean cluster size OLC within polymer matrix resulting in higher reflection abil-
demonstrate slightly higher conductivity [8]. On the other hand, ity of OLC-based polymer composite. At the same time, high
14 IEEE TRANSACTIONS ON ELECTROMAGNETIC COMPATIBILITY, VOL. 54, NO. 1, FEBRUARY 2012

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.
[13] L. Liu, L. Kong, W. Yin, and S. S. Matitsine, “Characterization of single-
polymers composites, the influence of the OLC concentration and multiwalled carbon nanotube composites for electromagnetic shield-
on the dielectric properties and how it is effected by the per- ing and tunable applications,” IEEE Trans. Electromagn. Compat., DOI:
colation phenomena, interactions inside OLC aggregates, and 10.1109/TEMC.2011.2159798. (Jul. 29, 2011). [Online].
[14] M. V. Shuba, G. Ya. Slepyan, S. A. Maksimenko, C. Thomsen, and
structure of the interface between OLC and polymer matrix. A. Lakhtakia, “Theory of multiwall carbon nanotubes as waveguides and
antennas in the infrared and the visible regimes,” Phys. Rev. B, vol. 79,
pp. 155403-1–155403-17, Apr. 2009.
VII. CONCLUSION [15] S. A. Maksimenko and G. Ya. Slepyan, “Nanoelectromagnetics of low-
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.
candidate for EMC material applications in the microwave fre- Bellingham, WA: SPIE, 2004, pp. 145–206.
[16] V. L. Kuznetsov, A. L. Chuvilin, Yu. V. Butenko, I. Yu. Malkov, and
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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.

Sergey Moseenkov was born in Mgachi (Sakhalin),


Russia, in 1984. He received the Diploma de-
Alesia G. Paddubskaya was born in Potsdam, gree in chemistry from Novosibirsk State Univer-
Germany, in 1986. She received the M.S. degree sity, Novosibirsk, Russia, in 2006, the Ph.D. de-
in laser physics from Belarusian State University gree in physical chemistry from Boreskov Institute of
(BSU), Minsk, Belarus, in 2010, where she is cur- Catalysis SB RAS, Novosibirsk, in 2010.
rently working toward the Ph.D. degree. He is currently a Research Associate at the
She is also a Junior Researcher at the Institute Boreskov Institute of Catalysis. He is the coauthor
for Nuclear Problems, BSU. Her current research of more than 20 articles in peer refereed journals and
interests include dielectric properties of composites nearly 40 conference papers related to studies of car-
with different forms of nanocarbon (single- and mul- bon materials. His current research interests include
tiwall carbon nanotubes, carbon black, and onion-like developing composites materials containing nanocarbons (nanodiamond, onion-
carbon) in very wide frequency range from hertz to like carbon, and carbon nanotubes).
terahertz.

Sergey A. Maksimenko received the M.S. degree


in physics of heat and mass transfer in 1976, the
Ph.D. degree in theoretical physics in 1988, both from
Belarus State University (BSU), Minsk, Belarus, and
the Doctor of Science degree in theoretical physics in
1996 from the Institute of Physics, Belarus National Anatoly I. Romanenko was born on September 10,
Academy of Science. 1950 in Omsk, USSR. He received the Diploma de-
Since 1992, he has been the Head of the Labora- gree in physics from Novosibirsk State University,
tory of electrodynamics of nonhomogeneous media, Novosibirsk, Russia, in 1973, the Ph.D. degree from
Research Institute for Nuclear Problems, BSU. He the Institute of Semiconductor Physics, Novosibirsk,
also teaches at the BSU physical department. He is Russia, in 1986, and Doctor of Science degree from
the author or coauthor of more than 150 conference and journal papers. His the Institute of Inorganic Chemistry, Novosibirsk, in
current research interests are electromagnetic wave theory and electromagnetic 2000.
processes in quasi-one- and zero-dimensional nanostructures in condensed mat- He was a Professor of Low Temperature Chair
ter and nanocomposites with the focus on nanocarbon. in 2006. He started his career at the Institute of In-
Dr. Maksimenko co-chaired conferences “Nanotubes and nanowires,” organic Chemistry in 1974, where he was a Junior
“Nanomodelling” and “Nanomodelling II” as parts of SPIE’s 48th and 49th Research Scientist, Scientist, Senior Research Scientist, and Scientific Leader.
Annual Meetings, and SPIE’s Optics & Photonics, in 2003, 2004, and 2006, He is currently with the Boreskov Institute of Catalysis SB RAS, Novosibirsk.
respectively. He is a Chair of the International conference “Fundamental and He is the author or coauthor of more than 100 articles in major refereed journals
Applied Nanoelectromagnetics,” Minsk, May 2012. He is SPIE Fellow and is and nearly 200 conference papers. His research interests include investigation of
the Associate Editor of the Journal of Nanophotonics. He participates in a num- electron transport properties of carbon whiskers, carbide-derived nanocarbons,
ber of international research projects, and is a coordinator of EU FP7 project carbon nanotubes, and composites containing nanocarbons.
FP7-226529 BY-NANOERA.
16 IEEE TRANSACTIONS ON ELECTROMAGNETIC COMPATIBILITY, VOL. 54, NO. 1, FEBRUARY 2012

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.

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