Abstract: | Blends of poly(acrylic acid) (PAA) and poly(p‐vinylphenol) (PVPh) were prepared from N,N‐dimethylformamide (DMF) and ethanol solutions. The DMF‐cast blends exhibited single Tg's, as shown by modulated differential scanning calorimetry, whereas the ethanol‐cast blends had double Tg's. Fourier transform infrared spectroscopy showed that there was a specific interaction between PAA and PVPh in the DMF‐cast blends. The single‐Tg blends cast from DMF showed single‐exponential decay behavior for the proton spin–lattice relaxation in both the laboratory frame and the rotating frame, indicating that the two polymers mixed intimately on a scale of 2–3 nm. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 789–796, 2003 |