"Study of UV-Curable Rubber-Toughened Epoxy Systems"
Abhijeet Godbole
M.S. Thesis, May 2002
Abstract
Rubber-toughened epoxy resins are
used extensively in various structural applications. Current thermal curing
processes limit the possible structural designs and require higher inputs in
terms of pressure, temperature and time. UV and electron beam curing offers
almost instantaneous curing of even complex structural shapes using minimal
inputs. Various formulations were quenched from single phase at high temperatures
to various temperatures below the corresponding cloud point temperatures, before
being allowed to cool to room temperature. These quenched formulations were
then cured using UV and thermal energy. The cured material toughness increases
with decreasing particle size by over 150%. The rate of cooling affects the
particle size achieved during phase separation. Particle size decreases with
faster cooling rates. Particle size of rapidly cooled samples changes with time
at room temperature. This is thought to be due to Ostwald ripening in which
densely populated small-sized particles coalesce together forming small number
of large-sized particles. This phenomenon is predicted to reduce the intended
shelf life of the B-stage resin. Triaryl sulphonium hexafluoroantimonate (TASHFA)
cured two phase and three component samples were partly uncured even after curing
under UV radiation for 15 minutes. Additional thermal curing step in a conventional
oven resulted in complete cure. FT-IR studies of the samples confirmed the presence
of unreacted epoxide rings in the UV cured samples. Additional short-time thermal
curing step, without any additional peroxide catalyst, was found to be sufficient
for complete cure. DMA results showed that some amount of rubber remains dissolved
in the epoxy matrix. This dissolved rubber contributes to the observed shift
of 30C in the epoxy tan [delta] peak for the fastest cooled sample. The amount
of the particulate rubber, dispersed in the matrix, reduced with an increase
in the cooling rate.