The Application of Chemical Polishing in TEM Sample Preparation of Zirconium Alloys

Hydride artefacts are commonly induced by the TEM sample preparation process in Zirconium alloys as hydrogen-sensitive metals, including electron polishing and focused ion beam (FIB) technology. In the research, we present the application of chemical polishing with a solution of 10HF:45HNO3:45H2O to prepare the disk samples for TEM observation in zirconium alloys. The thinning efficiency of chemical polishing is 25 μm per minute. XRD patterns indicate that the chemical polishing actually eliminates the macro- and micro-stress induced by mechanical grinding. TEM observation demonstrates that chemical polishing reduces the amount of hydride artefacts, especially hydrides with large size. It is proposed that induced stress provides driving force for hydride artefact formation. Compared with traditional mechanical grinding, the advantages of chemical polishing are high efficiency, free of induced stress, less induced hydride artefacts and bend contours.