Transmission electron microscopy sample preparation method for micrometer-sized powder particles using focused ion beam. (April 2021)

• Record Type: Journal Article
• Authors: Liu, Tong; Jin, Hongyan; Xu, Leilei; Huang, Zengli; Chen, Haijun; Niu, Mutong; Ding, Yanli; Ma, Yao; Ding, Sunan
• Is Part Of: Micron. Volume 143(2021)
• Publication Date: 2021-04
• Subjects: Micrometer-sized powder particles -- TEM sample preparation -- FIB -- Pt coating layers -- Layers -- EDX elemental mapping; Microscopy -- Periodicals; Electron Probe Microanalysis -- Periodicals; Microscopy -- Periodicals; Microscopie -- Périodiques; Microscopy; Periodicals; 502.82
• DOI: 10.1016/j.micron.2021.103030
• Languages: English
• ISSNs: 0968-4328

Abstract

Highlights: A TEM specimen preparation technique for micrometer-sized powder particle is proposed by using a FIB system. This novel technique reduces the TEM sample preparation time, allowing higher efficiency compared to embedding methods. This method enables the particles prepared for TEM sample with different size, shape or orientation to be easily selected. The TEM lamella of an individual particle can be fixed by the ion-beam-deposited Pt brackets on both sides. Both microstructure and EDX elemental mapping on the entire cross-section of the particle sample can be observed. Abstract: A TEM sample preparation technique for micrometer-sized powder particles in the 1−10 μm size range is proposed, using a focused ion beam (FIB) system. It is useful for characterizing elemental distributions across an entire cross-section of a particle. It is a simple and universal method without using any embedding agent, enabling the powder particles with different size, shape or orientation to be easily selected based on the SEM observations. The suitable particle is covered with Pt coating layers through an ion-beam-assisted deposition. The Pt coating layers provide sufficient support for the TEM lamella. A small piece of tungsten needle is used as a support under the particle by taking a series of operations using a micromanipulator. The particle can be precisely thinned by the ion beam to be suitable for both TEM observation and EDX elemental mapping. This novel technique reduces the TEM sample preparation time to a few hours, allowing much higher efficiency compared to complicated and time-consuming embedding methods.