The crystaIIinity, particle size and morphology of polyphenylene sulphide synthesized under various conditions have been investigated by X-ray diffraction and scanning electron microscopy. It was found that crystaIIinity decreased from 71 to 66% with increase of reaction time. The growth of particle size as well as total polymer mass followed a time dependence of the form X =X0 (1 -e-αt) The particle size distribution curve was noted to be sharp centring at 3 μn for short reaction time, high speed of stirring and also for low concentration of reactants. The particle morphology showed very strong dependence on various reaction parameters. Intricate sheaf-like morphology was noted for the particles at long reaction times or low stirring speeds while oblong platelet type two-dimensional morphology was noted when a low concentration of reactants was used. © 1986 Chapman and Hall Ltd.