The effects of processing conditions on the morphology of molecular composite films are examined by optical and electron microscopy. During coagulation processing from solutions in methanesulfonic acid (MSA), rigid‐rod polymer, such as poly(p‐phenylenebenzobisoxazole) (PBO), phase separates into undesirable aggregates. The coagulant and the method of its introduction have been found to exert a strong impact on the final film morphology. A quench of a PBO solution in MSA into a water bath results in a…
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