This work investigates spontaneous gelatination of polysulfonamide in the solution of dimethylacetamide by nuclear magnetic relaxation, small‐angle light scattering, and refractive index measurement. Two stages of the gelatination process were found to occur. Spherulites are formed in the first stage while the mobility of the solvent molecules decreases sharply. The second stage is characterized mainly by perfection of the inside structure of spherulites without a change in their size. The degree of decreasing mobility of the solvent molecules is much less in this stage than in the first stage.

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