Comparison Between the Thermal and Microwave Curing
of Bismaleimide Resin
Ismail Zainol,
1
Richard Day,
2
Frank Heatley
3
1
Advanced Materials Research Centre, SIRIM Berhad, Lot 34, Jalan Hi-Tech 2/3, Kulim Hi-Tech Park, 09000 Kulim,
Kedah, Malaysia
2
Manchester Materials Science Centre, UMIST, Grosvenor Street, Manchester M1 7HS, United Kingdom
3
Department of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom
Received 16 July 2002; accepted 2 April 2003
ABSTRACT: Microwave energy was used to cure
Matrimid 5292A bismaleimide resin. The degree of cure at
different cure times was determined with differential
scanning calorimetry. A comparison was made with the
same resin cured in a conventional oven. The resin cured
faster in the microwave oven than in the conventional
oven. The glass-transition temperature (T
g
) depended on
the degree of cure. The samples cured with a conventional
oven showed slightly higher T
g
’s than the microwave-
cured samples at higher degrees of cure. At low degrees of
cure, the two heating methods yielded materials with
similar T
g
’s. Fourier transform infrared spectroscopy and
solid-state cross-polarity/magic-angle-spinning
13
C NMR
spectroscopy were used to investigate the cured struc-
tures. There was no difference in the chemical reactions
taking place during the microwave cure and the thermal
cure. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90:
2764 –2774, 2003
INTRODUCTION
The microwave processing of thermosetting materials
offers significant advantages over conventional heat-
ing, such as reduced cure cycles, more uniform curing,
and improved physical and mechanical properties.
1
Microwave heating takes place through dipolar inter-
actions between molecules and an alternating electric
field rather than through thermal conduction or con-
vection as in conventional heating. Microwave radia-
tion penetrates materials, and the heat is generated
internally. Studies on epoxy resin systems have shown
that microwave processing significantly reduces the
cure cycle without sacrificing the mechanical proper-
ties.
2,3
Bismaleimide (BMI) resins are presently the best
candidates to replace epoxy resins in high-perfor-
mance composites because of their high temperature
stability and resistance to hot and wet environments.
4
BMI resins contain reactive double bonds (CAC) in
the maleimide groups that can polymerize with or
without the presence of a catalyst. Various curing
reactions for BMI resin formulations have been sug-
gested.
5
The main reaction proposed is homopolymer-
ization via a free-radical mechanism.
6
Conventional
curing processes involve heating in an oven, auto-
clave, or compression mold, in which heat transfer to
the material is accomplished through conduction or
convection. Just as for other thermosetting materials,
the low thermal conductivity of these resins leads to
thermal gradients inside the resin, and the curing
cycle becomes longer.
Initial studies of the microwave processing of BMI
systems have been reported.
7,8
Researchers
8
found
that the reaction kinetics in conventional and micro-
wave ovens were identical under isothermal condi-
tions. They concluded that no microwave effect could
be observed. The term microwave effect implies the
possibility of altering the rate and path of a chemical
reaction to produce a different morphology and dif-
ferent physical and mechanical properties. The afore-
mentioned researchers used in situ fiber-optic Fourier
transform near-infrared spectroscopy to measure the
extent of the reaction. Liptak et al.
7
however, found
more rapid curing when microwave heating was used
than when a conventional oven was used. They used
extraction methods to determine the gel content in the
cured resin. The apparent contradiction between these
two reports is probably due to the different techniques
used to cure and characterize the samples. Neither
shows in detail the cure chemistry in microwave and
conventional ovens. It is important to study the curing
path because the final structure and mechanical prop-
erties of a network depend on the reaction path.
The objective of this study was to compare the cure
chemistry of a BMI resin when conventional and mi-
crowave heating were used. The cure reactions were
followed with spectroscopic techniques. The effect of
Correspondence to: I. Zainol (ismail@sirim.my).
Contract grant sponsor: SIRIM Berhad.
Journal of Applied Polymer Science, Vol. 90, 2764 –2774 (2003)
© 2003 Wiley Periodicals, Inc.