An evaluation of Ar ion milling in TEM sample preparation by energy-filtered TEM technique

Abstract

Irradiated materials impose unique challenges when it comes to sample preparation for transmission electron microscopy (TEM) analysis. After the preparation of TEM samples by electrolytic polish, Ar ion milling was usually used to remove the surface contamination, as well as to thin the samples to desired thickness. Therefore, it is necessary to evaluate the advantages and limitations of Ar ion milling technique. In this work, the optimum milling condition with minimal surface artifacts was determined by Ar ion milling with various incident angles and beam energies, and the high-resolution TEM (HR-TEM) examinations confirmed the optimum condition to be 4.0keV Ar ions with incident angles of ±4°. In addition, Ar ion milling and subsequent thickness measurement by energy-filtered TEM (EF-TEM) were conducted to determine the thinning rate. It is found that electrolytic polished TEM lamella has a wedge-shape structure with a very sharp edge, and the thinning rates varied from 9.7±1.4nm/minute to 5.0±2.3nm/minute across the TEM lamella for 4.0keV Ar ions. However, the thinning rates for 2keV and 1keV Ar ions were under the examination limit, and they were supposed not sufficient to thin the tungsten samples. Even though the exact thinning rate varies for different materials, the general trends for the Ar ion milling observed in this study can be used as a guidance.