We tested forward recoil spectrometry (FRES) as a method to determine misci
bility by measuring coexistence compositions in binary polymer blends. In t
his study, equilibrium phase compositions were determined for a composition
ally symmetric poly(styrene-ran-methyl methacrylate) random copolymer (S-0.
49-r-MMA) and two homopolymers, deuterated polystyrene (dPS) and deuterated
poly(methyl methacrylate) (dPMMA). Sample preparation, film dewetting, and
beam damage were addressed, and the results for these polymer blends were
in good agreement with those obtained through other experimental techniques
. Deuteration had a strong effect on the miscibility of the dPS/S-0.49-r-MM
A and dPMMA/S-0.49-r-MMA blends, to the extent that the asymmetric miscibil
ity observed separately for the PS/S-0.49-r-MMA and PMMA/S-0.49- r-MMA blen
ds was not found. Although this deuteration effect may limit the applicabil
ity of FRES for some polymer systems, the accuracy with which phase composi
tions can be determined with FRES makes it an attractive alternative to oth
er less quantitative methods for investigating blend miscibility. (C) 2000
John Wiley & Sons, Inc.