Transmission electron microscope specimen preparation of Zn powders using the focused ion beam lift-out technique

• Published in: Metallurgical and materials transactions. A, Physical metallurgy and materials science Vol. 29; no. 9; pp. 2399 - 2406
• Main Authors: PRENITZER, B. I, GIANNUZZI, L. A, NEWMAN, K, BROWN, S. R, IRWIN, R. B, SHOFNER, T. L, STEVIE, F. A
• Format: Conference Proceeding Journal Article
• Language: English
• Published: New York, NY Springer 01.09.1998; Springer Nature B.V
• Subjects: Applied sciences; Argon ions; Cross-disciplinary physics: materials science; rheology; Electron microscopes; Exact sciences and technology; Grain size; Ion beams; Materials science; Materials synthesis; materials processing; Metals. Metallurgy; Optical microscopy; Physics; Powder processing: powder metallurgy, compaction, sintering, mechanical alloying, and granulation; Scanning electron microscopy; Specimen preparation; Transmission electron microscopy; Sample preparation; Metal powder; Metallography; SEM; Metallographic method; Experimental study; Microstructure; TEM; Zinc
• ISSN: 1073-5623; 1543-1940
• DOI: 10.1007/s11661-998-0116-z

Particles of Zn powder have been studied to show that high-quality scanning electron microscope (SEM) and transmission electron microscope (TEM) specimens can be rapidly produced from a site-specific region on a chosen particle by the focused ion beam (FIB) lift-out technique. A TEM specimen approximately 20-µm long by 5-µm wide was milled to electron transparency, extracted from the bulk particle, and micromanipulated onto a carbon coated copper mesh TEM grid. Using the FIB lift-out method, we were able to prepare a site-specific TEM specimen from a difficult material in under 3 hours. The TEM analysis of the lift-out specimen revealed a large amount of thin area free from characteristic signs of damage that may be observed as a result of conventional argon ion milling. The overall microstructure of the specimen prepared by the FIB lift-out method was consistent with samples prepared by conventional metallographic methods. A grain size of ∼10 to 20 µm was observed in all specimens by both TEM and SEM analysis. Light optical microscopy revealed the presence of internal voids in ∼10 to 20 pct of all particles. The SEM analysis showed the voids to extend over ∼70 pct of the particle volume in some cases.