Aspects regarding measurement of thickness of intergranular glassy films

Materials such as Si(3)N(4), SiC and SrTiO(3) can have grain boundaries characterized by the presence of a thin intergranular amorphous film of nearly constant thickness, in some cases (e.g. Si(3)N(4)) almost independent of the orientation of the bounding grains, but dependent on the composition of the ceramic. Microscopy techniques such as high-resolution lattice fringe imaging, Fresnel fringe imaging and diffuse dark field imaging have been applied to the study of intergranular glassy films. The theme of the current investigation is the use of Fresnel fringes and Fourier filtering for the measurement of the thickness of intergranular glassy films. Fresnel fringes hidden in high-resolution micrographs can be used to objectively demarcate the glass-crystal interface and to measure the thickness of intergranular glassy films. Image line profiles obtained from Fourier filtering the high-resolution micrographs can yield better estimates of the thickness. Using image simulation, various kinds of deviation from an ideal square-well potential profile and their effects on the Fresnel image contrast are considered. A method is also put forth to objectively retrieve Fresnel fringe spacing data by Fourier filtering Fresnel contrast images. Difficulties arising from the use of the standard Fresnel fringe extrapolation technique are outlined and an alternative method for the measurement of the thickness of intergranular glassy films, based on zero-defocus (in-focus) Fresnel contrast images is suggested. The experimental work is from two ceramic systems: Lu-Mg-doped Si(3)N(4) and SrTiO(3) (stoichiometric and nonstoichiometric). Further, a comparison is made between the standard high-resolution lattice fringe technique, the standard Fresnel fringe extrapolation technique and the methods of analyses introduced in the current work, to illustrate their utility and merits. Taking experimental difficulties into account, this work is intended to be a practical tool kit for the study of intergranular glassy films.