Examples of evolution of microstructure in ceramics and composites

In this article we describe a number of studies involving the direct observation of microstructural evolution. In general these investigations were carried out to establish the mechanistic paths involved. The materials studied range from fibers being evaluated for use in high-temperature ceramic composites to energetic materials used as propellants. In particular we discuss the room temperature imaging of materials difficult to image by conventional means and the use of the chamber atmosphere to influence microstructural evolution. Imaging of hydroxyapatite formed by chemical means is briefly described as an example of a difficult microstructure. Microstructural evolution during calcium aluminate cement hydration relies on the chamber atmosphere to control moisture loss from the hydrating specimens. In some instances microstructural evolution with heating occurred independently of the chamber atmosphere. Grain growth in PZT films formed by sol-gel processes depends strongly on temperature but does not appear to depend on the chamber atmosphere. This is also the case for the combustion of nitroamine propellants in that their combustion does not depend on access to an external source of oxygen. In other studies, the chamber atmosphere played an indirect role in determining microstructure. However, the mechanistic path driving microstructural evolution in copper-based inks used as conductive paths on electronic substrates is atmosphere dependent. These inks are formulated from copper powder, glass, and an organic binder, and the interaction of the binder with an oxidizing atmosphere allows it to be burned out before significant interaction occurs between the copper powder and the glass. Finally, the microstructural variations during the oxidation of structural composites at high temperature were used to allow assessments of their likely failure mechanisms.