Highly cross-linked
inorganic and organic hybrid cyclomatrix-polyphosphazenes
microspheres (C-PPZs) have been successfully synthesized by a one-pot
polymerization technique between hexachlorocyclotriphosphazene and p-phenylenediamine in the presence of triethylamine (TEA),
and they were used for enhancing the flame retardancy of epoxy resins
(EPs). A thermoset EP was prepared by incorporating different percentages
(2, 5, and 10%) of C-PPZs into diglycidyl ether of bisphenol A (DGEBA).
The results reveal that the size and morphology of the microspheres
can be tuned by varying the synthesis temperature. The average size
of C-CPPZs gradually increased from 3.1, 4.9, to 7.8 μm as the
temperature was increased from 100, 120, to 200 °C, respectively.
The thermogravimetric analysis showed that the C-CPPZ microspheres
have good thermal stability up to 900 °C with about ∼10
wt % mass loss for C-CPPZs formed at 200 °C compared to ∼30
wt % mass loss for those obtained at 100 and 120 °C. The 10%
loss at 900 °C is much lower than the previous research concerning
the thermal stability of cyclophosphazene, in which more weight losses
were observed at lower temperatures. The resulting C-CPPZ microspheres
were characterized by spectroscopic and imaging techniques including
Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray
diffraction, scanning electron microscopy, energy-dispersive X-ray
spectroscopy, elemental mapping, and X-ray photoelectron spectroscopy.