In this work, quantitative Atomic force acoustic microscopy (AFAM) was used to measure nanomechanical properties and to determine microstructural morphology in fiber reinforced composites and hard calcified tissue. In carbon fiber reinforced composites, the fiber-matrix interphase is of interest as it affects the primary load-transfer process and thereby bulk mechanical properties of reinforced composites. The study of properties in the interphase region is important for an understanding of the bulk mechanical properties, which have been shown affected by moisture-based environmental degradation. Single point AFAM testing has been used to quantitatively determine elastic properties at the fiber-matrix interphase by taking advantage of the high spatial scanning resolution capable of measuring interphase dimensions. Carbon-fiber epoxy composite samples were degraded in laboratory conditions by exposure to a accelerated hydrothermal degradation environment in deionized water and salt water. Composite degradation has been characterized by the change in the epoxy matrix contact stiffness and the interphase properties. A decrease in matrix stiffness was found to coincide with the environmental exposure and moisture absorption of the samples. Interphase stiffness measurements indicate a constant interphase thickness as a function of environmental exposure. Chemical analysis of the epoxy using FTIR and Raman spectroscopy indicate hydrolysis of the C-O-C and Epoxide bonds which contribute to the decrease in epoxy mechanical properties. Accelerated degradation by salt water and deionized water both resulted in degradation of the epoxy, though the presence of sodium chloride showed less degradation. From SEM, debonding of the fiber-matrix interface was observed to be more severe when exposed to a salt water environment. In performing quantitative AFAM measurements, the effects of tip shape on the contact mechanics at the epoxy interface were found to influence the reported results significantly, and new, power-law body of revolution models of the probe tip geometry have been applied. Due to the low yield strength of polymers compared with other engineering materials, elastic-plastic contact is considered to better represent the epoxy surface response and was used to acquire more accurate quantitative measurements. Visco-elastic contact response was introduced in the boundary condition of the AFAM cantilever vibration model, due to the creep nature of epoxy, to determine time-dependent effects. These methods have direct impact on the quantitative measurement capabilities of near-filler interphase regions in polymers and composites and the long-term influence of environmental conditions on composites. In addition, quantitative AFAM scans were made on distal surfaces of human bicuspids and molars, to determine the microstructural and spatial variation in nanomechanical properties of the enamel biocomposite. Single point AFAM measurements were performed on individual enamel prism and sheath locations to determine spatial elastic modulus. Mechanical property variation of enamel is associated to the differences in the mineral to organic content and the apatite crystal orientations within the enamel microstructure. Also, variation in the elastic modulus of the enamel ultrastructure was observed in measurements at the outer enamel versus near the dentine enamel junction (DEJ).