World Journal of Nano Science and Engineering, 2012, 2, 213-218
http://dx.doi.org/10.4236/wjnse.2012.24029 Published Online December 2012 (http://www.SciRP.org/journal/wjnse)
Microstructural Characterization of Large Area C
60
Films
Obtained by Conventional Microwave Oven Irradiation
Jacobo Martínez-Reyes
1
, Lucia Graciela Díaz Barriga-Arceo
2
, Luis Rendón-Vazquez
3
,
Reynaldo Martínez-Guerrero
4
, Néstor Romero-Partida
4
, Eduardo Palacios-González
5
,
Vicente Garibay-Febles
5
, Jaime Ortiz-López
1
1
National Polytechnic Institute (IPN), ESFM, UPALM, Mexico City, Mexico
2
National Polytechnic Institute (IPN), ESIQIE, UPALM, Mexico City, Mexico
3
Facultad de Ciencias, UNAM, Mexico City, Mexico
4
ROMFER S.A. de C.V., Mexico City, Mexico
5
IMP-Molecular Engineering Program, Mexico City, Mexico
Email: jacobomartinezreyes@gmail.com, luchell@yahoo.com
Received August 14, 2012; revised August 28, 2012; accepted September 5, 2012
ABSTRACT
In the present work the synthesis of C
60
produced in a conventional microwave oven from the decomposition of cam-
phor resin is reported. The polycrystalline structure of the sample was determined by X-Ray Diffraction (XRD), the sam-
ple showed several phases, the main phase corresponds to fullerene C
60
ordered in a Face-Centered Cubic structure (FCC),
with two more structures: one orthorhombic system and the other the monoclinic system coexisting also with graphite
2H phase. It was observed in a Scanning Electron Microscopy (SEM), that the sample formed thin films of stacked
carbon. Whereas in a High Resolution Transmission Electron Microscopy (HRTEM), measurements in Bright Field
mode revealed that the main phase of the material is C
60
ordered in FCC structure and the elemental composition and
atomic bonding state can be determined by analyzing the energy with the electron microscope by Elesctron Energy-
Loss Spectroscopy (EELS), technique allowed confirm all the phase C
60
established with XRD observations.
Keywords: Microwave-Assisted Synthesis; Carbon Film; Fullerene
1. Introduction
Carbon thin films are important for the development of
applications due to the physicochemical properties [1-5].
Several methods are currently used for the preparation of
carbon films such as: the condensation of steam to car-
bon, magnetron sputtering, mechanical peeling, chemical
vapor deposition, physical vapor deposition [6-11] among
others. In these methods the films are obtained in tem-
perature conditions at ranges of 950˚C - 1250˚C with
different energies from 100 to 1000 eV at pressure from
1 to 5 × 10
–7
Tor using inert atmospheres or carbon gases
as control atmospheres, flowing in a continuous way to
obtain small area films with thicknesses from 500 nm to
10 microns and crystalline or amorphous structure [12],
making this synthesis expensive. Comparing the chemi-
cal precursors used in the synthesis of carbon films, it
was observed that organic resins present more advan-
tages than the inorganic precursors because some of
these resins are environment friendly that is why cam-
phor resin was chosen [13-15]. It is important to mention
that camphor C
10
H
16
O resin has been successfully used in
carbon nanomaterial synthesis and also in carbon films
[16-20]. Therefore the Microwave Assisted Synthesis
(MAOS) [21-28], is a cost-effective alternative technol-
ogy which reduces the impact on the environment by
saving energy, being able to produce materials and mi-
crostructures that cannot be performed by other methods.
The aim of this work was to find the synthesis and mi-
crostructural of carbon films to characterization them
carbon films by microwave radiation a resins of com-
mercial camphor.
2. Experimental Details
2.1. Microwave Oven Preparation
The plate was removed from the microwave oven and the
samples were placed in a position where the microwave
radiation reaches the maximum. Determinations of max-
imum and minimum points were done as reported in lit-
erature [29]. Resin sample were located in one of the
points where microwave radiation has one maximum.
2.2. Sample Preparation
For this work 250 mg of camphor Sigma-Aldrich were
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