The LDEF M0003-5 Thermal Control Materials Experiment contains numerous thermal control coatings, metallized and nonmetallized polymeric films, adhesives, OSR's, and metallic foils. The materials were located on the leading and trailing edges of the satellite, therefore exposed to two different low earth orbital environments. Many specimens received a total exposure of 5.75 years and other received a limited exposure of 0.9 years to the complete environment. On-orbit and post flight photographic records are presented. The material's physical and optical performance are discussed as a function of location and duration of exposure. Data concerning specimen condition, degradation, contamination, optical reflectance and transmittance are discussed. The effect of atomic oxygen erosion on specific materials is also presented, The performance of adhesive bonds with polymeric films is reviewed.