SummaryIn situ composites were prepared via melt blending of a liquid crystalline polymer (LCP) and polycarbonate using a twin screw extruder. The structure and morphology of these composites were analysed using both transmission electron microscopy (TEM) and scanning electron microscopy. The LCP phases were able to orientate and form in situ submicrometre fibres during the extrusion and postextrusion drawing. TEM images as well as selected-area diffraction patterns were obtained from the materials. The effects of both composition, i.e. LCP content, and postextrusion draw-down ratio on the development of the in situ formed LCP fibres were studied in detail. A skin-core morphological differentiation is observed in these materials where well-defined LCP fibres of higher aspect ratios were formed in the skin region. However, a significant amount of unelongated LCP particles were found coexisting with the less well-defined fibres in the core region of the extrudates. This skin-core differentiation was found to be dependent on the composition and the processing conditions, e.g. draw ratio. In this instance, electron microscopy is proven to be a powerful technique not only for direct observation of the formation, dimensions and morphology of the in situ LCP fibres, but also for the qualitative and quantitative characterization of the molecular orientation and crystalline structures in these fibres using selected-area electron diffraction. It is observed that the skin-core differentiation becomes more distinct in the in situ composites containing a higher percentage of LCP but diminishes when the material is processed at higher post-extrusion draw ratio.