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Microwave Absorption Properties in Epoxy Resin Multi

Walled Carbon Nanotubes Composites


M. Giorcelli1, P. Savi2, A. Delogu3, M. Miscuglio2, Y.M. Hajj Yahya 2, A. Tagliaferro1

Abstract − In the ongoing search for new materials for chosen among other polymers because it is thermoset
microwave absorption applications, carbon nanotubes (CNTs) and can withstand temperatures comparable to those
deserve a special consideration due to their outstanding
properties. In this paper, the microwave absorbing properties of reached when microwave absorption applications are
epoxy resin based composites containing three different types targeted. The characteristics of commercial MWCNTs
of commercial Multi Walled Carbon Nanotubes (MWCNTs) (Cheaptubes, Nanothinx) are summarized in Table 1.
used as fillers have been analyzed. The complex permittivity of They are selected in order to understand the influence
the composites has been experimentally determined. These data
were used to simulate the absorbing properties in the frequency
of parameters (length, diameters) on the microwave
band 3-18 GHz of a single-layer absorber backed by a metallic behaviour.
plate considering several concentration of CNTs.
MWCNTs Diameter Length Purity
filler (nm) (ȝm) (%)
1 INTRODUCTION 1 30-50 0,5-2 >95
2 25-45 >10 >98
There is an increasing demand for lightweight and 3 6-10 >10 >90
Radar Absorbing Material (RAM) in both commercial Tab. 1: Multi walled carbon nanotubes used.
and military applications. Carbon Nano Tubes (CNTs)
and graphene have already been investigated for 2.1 Samples preparation
microwave absorption applications [1-4] due to their
great thermal stability, reluctance toward chemical MWCNTs have been dispersed in Epilox in desired
agents and excellent mechanical and electrical concentration using the following procedure [7]:
properties. CNTs are much more attractive for the 1. MWCNTs and Epilox quantities are weighted via
preparation of RAMs with respect to graphene [1] and digital balance and preliminary mixed together with
graphene oxide [5] because their large scale production a metallic spatula
is more economical and they are less troublesome to 2. The mixture is dispersed using an UltraTurrax®
disperse in host polymers. As a matter of fact CNTs mixer for 10 minutes in order to create a well
have been used as polymer fillers for a number of years dispersed solution
in order to improve polymer characteristics [6]. Even 3. Curing agent (Epilox® Hardner H 10-31: liquid,
at low filler contents, they can improve the mechanical colourless, modified cycloaliphatic polyamine
and electrical performances of the host polymer. apoxide adduct) is added to the mixture in 6:10
Moreover, CNTs have aspect ratios (i.e. length vs ratio and a 10 minutes mechanical stirring
diameters ratio), that can exceed 1000. These special performed
properties make CNTs excellent candidates for high 4. The mixture is slowly poured in 27 mm in diameter
strength and electrically conductive polymer nano- cylindrical moulds
composite applications. 5. Nanocomposite is degassed in a vacuum chamber
for 20 minutes
2 CNTs COMPOSITES CHARACTERISTICS 6. Final product is dried in oven for 3 hours at 70°C
Samples have been prepared starting from a
commercial epoxy resin and a number of commercial
MWCNTs having different lengths and diameters. The
commercial epoxy resin (Epilox®, T 19-36/700) used
in this work is a modified, low viscosity epoxy resin Figure 1: Samples compared with one euro coin.
with reduced crystallization tendency. It has been
1
Department of Applied Science and Technology (DISAT), Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino, Italy,
mauro.giorcelli@polito.it, alberto.tagliaferro@polito.it.
2
Department of Electronic and Telecommunication (DET), Politecnico di Torino, C.so Duca degli Abruzzi 24, 10129 Torino, Italy,
patrizia.savi@polito.it.
3
Selex ES, Caselle (TO), Italy, andrea.delogu@selex-es.com

978-1-4673-5707-4/13/$31.00 ©2013 IEEE

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2.2 Morphological analysis

Field Emission Scanning Electron Microscopy


(FESEM Zeiss Supra-40) images of cryo fractured
samples are shown in Fig. 2. They show the dispersion
degree of the filler inside polymeric matrix (a,b,c) and
the outer CNTs structure. CNTs, because of Van der
Waals forces, are usually bundled (see fig.1 d). Figure 3: Measurement set up.
Bundles are broken by applying a strong shear force.
3 RESULTS AND DISCUSSION

In Fig. 4 the real part of the permittivity and tanį for


a) b)
nanocomposite of type 3 are shown. Results for three
different MWCNTs concentrations (1-3-5 wt%) are
shown and compared with pure Epilox resin.

c) d)

Figure 2: FESEM analysis on nanocomposite at 3%


of MWCNTs: a) type 1, b) type 2, c) type 3, d)
bundle of MWCNTs type 3 as it is.

2.4 Permittivity measurements

The complex permittivity e = e'+ je ' ' of pure


Epoxy resin and of the three different composites was
measured in the frequency range 3 -18 GHz. The real
part e' of the complex permittivity is related to the
polarization characteristics of the material. The
imaginary part e ' ' is related to the effective electrical
conductivity ( ı = Ȧİ 0 İ ' ' , İ 0 being the free-space
permittivity and Ȧ the angular frequency of the em
wave). Samples were measured using a commercial
capacitive sensor (Agilent 85070D) and a Network
Analyzer (E8361A) (see Fig.3).
This measurement system has been chosen because Figure 4: Type 3 characteristics at 1%, 3%, 5%
it allows a wide-band characterization and it can be MWCNTs wt% compared with pure Epilox resin.
used on samples of small dimension. Free-space
measurements require at least 15 cm x 15 cm samples, In type 3 composite the values of the complex
whereas waveguides method needs an accurate permittivity increase with the increase of the
manufacturing of the sample to be inserted in the concentration of CNTs more than in types 1 and 2.
waveguide. Hence, this type appears more suitable for radar
A standard calibration short/air/water was absorbing material applications.
performed before each measurement. Several Starting from the knowledge of the permittivity, the
measurements were performed on each sample absorbing properties of polymers with different
changing the sensor position. The final value has been contents of MWCNTs have been analyzed considering
reported after an accurate average for each type. one-layer of thickness d, backed by a metallic plane.

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The reflection coefficient of this structure was Acknowledgments
analyzed by considering an incident plane wave with
parallel, TM, and perpendicular, TE, polarization and Authors would like to thank Nanothinx for material
applying a transmission line approach [8]. supply. Dr. S. Guastella for FESEM analysis, W.
Ferrarese and M. Mwanya of Selex ES for the RCS
measurements. Thermalskin project (Revolutionary
surface coatings by carbon nanotubes for high heat
transfer efficiency, FIRB 2010 - Futuro in Ricerca)
for economical support.

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