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.