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Novel Method for Preparing Transmission Electron Microscopy Samples of Micrometer-Sized Powder Particles by Using Focused Ion Beam

Part of: Micrographia Collection

Published online by Cambridge University Press:  13 September 2017

Tae-Hoon Kim ,
Min-Chul Kang ,
Ga-Bin Jung ,
Dong Soo Kim  and
Cheol-Woong Yang
Tae-Hoon Kim
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
Min-Chul Kang
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
Ga-Bin Jung
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
Dong Soo Kim
Affiliation:
Powder & Ceramics Division, Korea Institute of Materials Science, Changwon 51508, Korea Metals Technology Research Department, Convergence Research Center for Development of Mineral Resources, Korea Institute of Geoscience and Mineral Resources, Daejeon 34132, Korea
Cheol-Woong Yang*
Affiliation:
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
*
*Corresponding author. [email protected]
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Abstract

The preparation of transmission electron microscopy (TEM) samples from powders is quite difficult and challenging. For powders with particles in the 1–5 μm size range, it is especially difficult to select an adequate sample preparation technique. Epoxy is commonly used to bind powder, but drawbacks, such as differential milling originating from unequal milling rates between the epoxy and powder, remain. We propose a new, simple method for preparing TEM samples. This method is especially useful for powders with particles in the 1–5 μm size range that are vulnerable to oxidation. The method uses solder as an embedding agent together with focused ion beam (FIB) milling. The powder was embedded in low-temperature solder using a conventional hot-mounting instrument. Subsequently, FIB was used to fabricate thin TEM samples via the lift-out technique. The solder proved to be more effective than epoxy in producing thin TEM samples with large areas. The problem of differential milling was mitigated, and the solder binder was more stable than epoxy under an electron beam. This methodology can be applied for preparing TEM samples from various powders that are either vulnerable to oxidation or composed of high atomic number elements.

Keywords

TEM sample preparationsolderFIB millingpowderoxidation
Type
Micrographia
Information
Microscopy and Microanalysis , Volume 23 , Issue 5 , October 2017 , pp. 1055 - 1060
Copyright
© Microscopy Society of America 2017 

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References

Ayache, J., Beaunier, L., Boumendil, J., Ehret, G. & Laub, D. (2010). Sample Preparation Handbook for Transmission Electron Microscopy: Techniques. New York, NY: Springer.Google Scholar
Benslim, N., Mehdaoui, S., Aissaoui, O., Benabdeslem, M., Bouasla, A., Bechiri, L., Otmani, A. & Portier, X. (2010). XRD and TEM characterizations of the mechanically alloyed CuIn0.5Ga0.5Se2 powders. J Alloys Compd 489, 437–440.Google Scholar
Chung, K.H., Lee, J., Rodriguez, R. & Lavernia, E.J. (2002). Grain growth behavior of cryomilled INCONEL 625 powder during isothermal heat treatment. Metall Mater Trans A 33, 125–134.CrossRefGoogle Scholar
Danaie, M. & Mitlin, D. (2009). TEM analysis and sorption properties of high-energy milled MgH2 powders. J Alloys Compd 476, 590–598.Google Scholar
Hashemi-Sadraei, L., Mousavi, S.E., Vogt, R., Li, Y., Zhang, Z., Lavernia, E.J. & Schoenung, J.M. (2011). Influence of nitrogen content on thermal stability and grain growth kinetics of cryomilled Al nanocomposites. Metall Mater Trans A 43, 747–756.Google Scholar
He, J.H., Chung, K.H., Liao, X.Z., Zhu, Y.T. & Laveria, E.J. (2003). Mechanical milling-induced deformation twinning in fcc materials with high stacking fault energy. Metall Mater Trans A 34, 707–712.Google Scholar
Hoffmann, J., Klimenkov, M., Lindau, R. & Rieth, M. (2012). TEM study of mechanically alloyed ODS steel powder. J Nucl Mater 428, 165–169.Google Scholar
Kim, T.H., Oh, J.S., Cha, H.R., Lee, J.G., Kwon, H.W. & Yang, C.W. (2016). Direct observation of texture memory in hydrogenation–disproportionation–desorption–recombination processed Nd-Fe-B magnets using electron backscatter diffraction. Scr Mater 115, 6–9.Google Scholar
Kitano, Y., Fujikawa, Y., Kamino, T., Yaguchi, T. & Saka, H. (1995). TEM observation of micrometer-sized Ni powder particles thinned by FIB cutting technique. J Electron Microsc 44, 410–413.Google Scholar
Lin, J.H., Liu, S.F., Cheng, Q.M., Qian, X.L., Yang, L.Q. & Su, M.Z. (1997). Preparation of Nd-Fe-B based magnetic materials by soft chemistry and reduction-diffusion process. J Alloys Compd 249, 237–241.Google Scholar
Litynska-Dobrzynska, L., Dutkiewicz, J., Maziarz, W. & Rogal, L. (2010). TEM and HRTEM studies of ball milled 6061 aluminium alloy powder with Zr addition. J Microsc 237, 506–510.Google Scholar
Prenitzer, B.I., Giannuzzi, L.A., Newman, K., Brown, S.R., Irwin, R.B., Shofner, T.L. & Stevie, F.A. (1998). Transmission electron microscope specimen preparation of Zn powders using the focused ion beam lift-out technique. Metall Mater Trans A 29, 2399–2406.Google Scholar
Rea, K.E., Agarwal, A., Mckechnie, T. & Seal, S. (2005). FIB cross-sectioning of a single rapidly solidified hypereutectic Al-Si powder particle for HRTEM. Microsc Res Tech 66, 10–16.Google Scholar
Thornton, J.J., Han, B.Q. & Lavernia, E.J. (2007). Grain growth in cryomilled Ni powder during degassing. Metall Mater Trans A 38, 1343–1350.Google Scholar
Wei, L.Y. & Li, T. (1997). Ultramicrotomy of powder material for TEM/STEM study. Microsc Res Tech 36, 380–381.Google Scholar
Wen, H., Dong, S., He, P., Wang, Z., Zhou, H. & Zhang, X. (2007). Sol-gel synthesis and characterization of ytterbium silicate powders. J Am Ceram Soc 90, 4043–4046.Google Scholar
Wen, H., Lin, Y., Seidman, D.N., Schoenung, J.M., van Rooyen, I.J. & Lavernia, E.J. (2015). An efficient and cost-effective method for preparing transmission electron microscopy samples from powders. Microsc Microanal 21, 1184–1194.Google Scholar
Williams, D.B. & Carter, C.B. (2009). Transmission Electron Microscopy—A Textbook for Materials Science. New York, NY: Springer.Google Scholar
Zhou, F., Lee, J., Dallek, S. & Lavernia, E.J. (2001). High grain size stability of nanocrystalline Al prepared by mechanical attrition. J Mater Res 16, 3451–3458.CrossRefGoogle Scholar
Zhou, F., Liao, X.Z., Zhu, Y.T., Dallek, S. & Lavernia, E.J. (2003 a). Microstructural evolution during recovery and recrystallization of a nanocrystalline Al-Mg alloy prepared by cryogenic ball milling. Acta Mater 51, 2777–2791.CrossRefGoogle Scholar
Zhou, F., Nutt, S.R., Bampton, C.C. & Lavernia, E.J. (2003 b). Nanostructure in an Al-Mg-Sc alloy processed by low-energy ball milling at cryogenic temperature. Metall Mater Trans A 34, 1985–1992.CrossRefGoogle Scholar