With the advent of “designed damping” in composite materials, and modern computer design tools, accurate three-dimensional material properties information is critically important. Further, design of advanced composite structures often requires knowledge of material properties over a range of temperatures. Conventional testing approaches for the determination of material properties present difficulties related to specimen preparation, fixturing and test apparatus. Consequently, engineers frequently make use of micromechanics generated properties. Unfortunately, micromechanics approaches do not usually account for manufacturing and temperature variations, which affect material properties. This research focuses on developing approaches to allow experimental characterization of elastic and viscoelastic properties of fiber reinforced composite laminae, over a range of temperatures. In addition to investigating the temperature dependence of the three-dimensional material properties, for the viscoelastic characterization, the effect of loading frequency is also addressed. A technique for the determination of the three-dimensional elastic coefficients of transversely isotropic laminae has been developed, using a combination of laminate coefficient of thermal expansion (CTE) measurements and two elastic properties measured from a standard tensile test. The CTE measurements have been conducted in a laboratory thermo mechanical analyzer (TMA), using samples of simple geometry. PEEK/IM7 laminae were used to verify this approach and the computed room temperature elastic properties are in good agreement with quoted elastic material properties measured by standard techniques.