Effects of foil thickness on measurement of grain boundary segregation with FEG-TEM/EDS in austenitic stainless steels

Abstract
In order to clarify the effects of foil thickness on spatial resolution of energy dispersive X-ray spectroscopy (EDS), segregation in a nano-order width near a grain boundary was measured by an energy dispersive X-ray spectrometer attached to an FEG-TEM. The materials used were commercial types 316 and 304 stainless steels, which were solution-annealed at 1373 or 1323K, followed by slow cooling in air. Prior to the EDS measurement, the electron beam diameter was determined to be 1 nm using the lattice image of gold. The mean free path of inelastic scattering for stainless steels was determined, and used to obtain local foil thickness in the analysed area by the EELS technique. Spatial resolution of the EDS analysis was little sensitive to the foil thickness of less than 200 nm, and the resolution of at least 1.5 nm was kept even at the thickness of 200 nm. Segregation of solutes due to thermal heat treatment was not dependent on the misfit angle of the grain boundary as far as high-angle random boundaries were concerned.

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