Micro-thermal analysis (micro-TA) is a new subsurface thermal analysis tech
nology. The average of the DC signal is a function of the thermal conductiv
ity, and the response to the AC modulation signal is a function of the ther
mal diffusivity of the subsurface. Using this technique, three images based
on topography, thermal conductivity, and thermal diffusivity are obtained
simultaneously. Specific areas and domains in these images can then be char
acterized by simply positioning the probe and performing a localized therma
l analysis experiment. The technique has been used to study the phase separ
ation process in a 50:50 (by weight) polystyrene (PS)-poly(vinyl methyl eth
er) (PVME) blend and natural rubber-nitrile rubber blends. For these polyme
r blends, considerable contrast between phases is obtained, based on therma
l conductivity, whereas optical and electron microscopy would show them as
being very similar. For example, it is difficult to image the morphology of
natural and nitrile rubber blends by means of transmission electron micros
copy, because of their similar chemical structures. Micro-TA gives an excel
lent image of the morphology of these natural-nitrile rubber blends. This o
pens a new way for rubber industries to study morphologies of rubber-rubber
blends in general. In the 50:50 PS-PVME blend, annealed at 125 degreesC, s
pinodal decomposition occurred. With increasing time, the domain size and t
he glass transition temperature of PS-rich domains increased, indicating th
at the concentration of PVME in the PS-rich phases decreases. The results i
mply that micro-TA can be used to image the composition in the near-surface
or surface regions in multicomponent materials, if the resolution is high
enough. (C) 2001 John Wiley & Sons, Inc.