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Metal‐assisted SIMS for three‐dimensional analysis using shave‐off section processing

Three‐dimensional microanalysis of the microstructure of organic materials is important in the development and progress of analytical methods on the micro‐to‐nanometer scales. We have developed a novel three‐dimensional microanalysis method using focused ion beams for section processing (shave‐off scanning) and time‐of‐flight secondary ion mass spectrometry for mapping. Shave‐off scanning can effectively create an arbitrary section on a sample set against composites materials with a wide variety of shapes; three‐dimensional sample images are then obtained by alternately operating two focused ion beams. In this study, we adapted metal‐assisted secondary ion mass spectrometry for three‐dimensional microanalysis. We have devised a unique method whereby gold is deposited on a section to be analyzed after every shave‐off sectioning by setting a gold plate at the back of the sample. Consequently, gold was observed to be deposited on the created cross‐section concurrently with shave‐off sectioning, resulting in a substantially enhanced secondary ion intensity. Copyright © 2014 John Wiley & Sons, Ltd.