1070-4272/03/7603-0457$25.00C2003 MAIK [Nauka/Interperiodica]
Russian Journal of Applied Chemistry, Vol. 76, No. 3, 2003, pp. 457! 459. Translated from Zhurnal Prikladnoi Khimii, Vol. 76, No. 3,
2003, pp. 472! 474.
Original Russian Text Copyright + 2003 by Ginzburg, Smirnov, Filatov, Shibaev, Melenevskaya, Novoselova, Shepelevskii.
AND POLYMERIC MATERIALS
Aggregates in Polymethyl Methacrylate Films
B. M. Ginzburg, A. S. Smirnov, S. K. Filatov, L. A. Shibaev, E. Yu. Melenevskaya,
A. V. Novoselova, and A. A. Shepelevskii
Institute of Machine Science, Russian Academy of Sciences, St. Petersburg, Russia
St. Petersburg State University, St. Petersburg, Russia
Institute of Macromolecular Compounds, Russian Academy of Sciences, St. Petersburg, Russia
Received July 31, 2002
Abstract-The structure of aggregates of fullerene C
introduced into films of radical polymethyl methacry-
late in the stage of solution preparation was studied by wide-angle X-ray diffraction.
Previously, we have studied the effect of small ad-
ditions of fullerene C
on thermal degradation of
polymers . Preparation of fullerene3polymer
compositions can be accompanied by microphase
segregation with formation of fullerene aggregates in
the polymer matrix. In turn, the structure of such
aggregates can affect the composition properties .
In this work, we studied the structure of fullerene C
aggregates in a film of atactic polymethyl methac-
rylate (PMMA) prepared by radical polymerization.
Atactic PMMA with the molecular weight M =
85000 was dissolved in o-dichlorobenzene to obtain
10 wt % concentration. The same solution of fullerene
was also prepared. Then, these solutions were
mixed in proportions required to obtain the fullerene
concentration in the PMMA film of 1 and 10%. Films
were prepared by casting on a cover glass. The solvent
was evaporated from the PMMA and PMMA + ful-
lerene solutions at room temperature in air. The film
thickness was about 70 mm.
A study with a MIN-8 polarization optical micro-
scope showed that the films were transparent, i.e., they
were homogeneous on the optical level (<0.5 mm).
Wide-angle X-ray diffraction patterns of films
was measured on a DRON-2.0 diffractometer with
graphite crystal monochromator in CuK
The powder pattern of fullerene C
a glass support is shown in Fig. 1. The reflections
are indexed in the face-centered cubic crystal lattice of
. The fullerene reflections are narrow
and intense, so that the scattering from the support
can be neglected. The relative reflection
intensities and the corresponding interplanar spacings
(with the error of 0.0130.02 A) are in good agreement
with the reference data .
The average crystallite dimensions L
direction were calculated by the Scherrer formula 
using measured widths of the reflection profiles.
The minimal crystallite size (neglecting the effects of
the lattice distortion and primary beam width) calcu-
lated from the width of a series of the most intense
reflections is 3003400 A.
Fullerene aggregates in the PMMA matrix show no
similar ordering. The diffraction patterns of PMMA
films with fullerene on a glass support are shown in
Fig. 2. To take into account the scattering from the
support, the scattering pattern was subtracted from the
difraction patterns. The difference patterns allowed re-
finement of the position and shape of diffuse maxima.
Fig. 1. Wide-angle powder pattern of C
(I) intensity and (2q) Bragg angle; the same for Fig. 2. In-
dices of the face-centered crystal lattice are indicated.
Bragg angle corresponding to peak maximum, deg:
(1) 10.83, (2) 17.77, (3) 20.91, (4) 21.82, (5) 27.63,
(6) 28.30, (7) 31.01, and (8) 32.94.