Specimen preparation is the first step that determines the quality of the microstructural information that can be obtained using optical microscopy. This chapter describes the sample preparation methods that are applicable to most types of composite materials containing short discontinuous or continuous fibers. The sample preparation methods cover documentation and labeling of samples, sectioning the composite, clamp-mounting composite samples, mounting composite samples in casting resins, and the addition of contrast dyes to casting resins. Information on the molds used for mounting composite materials is provided. The steps recommended to achieve a good mounted specimen without voids or specimen pull-out are also described. The chapter discusses the processes for clamping mounted composite samples in automated polishing heads and mounting composite materials for hand polishing. A summary of the mounting technique is also included.

Transmitted-light methods reveal more details of the morphology of fiber-reinforced polymeric composites than are observable using any other available microscopy techniques. This chapter describes the various aspects relating to the selection and preparation of ultrathin-section specimens of fiber-reinforced polymeric composites for examination by transmitted-light microscopy techniques. The preparation steps covered are a selection of the rough section, preparation of the rough section for preliminary mounting, grinding and polishing the primary-mount first surface, mounting the first surface on a glass slide, and preparing the second surface (top surface). The optimization of microscope conditions and analysis of specimens by microscopy techniques are also covered. In addition, examples of composite ultrathin sections that are analyzed using transmitted-light microscopy contrast methods are shown throughout.