TEM Specimen Preparation by Crushing Bulk Crystals
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Some TEM specimens can be prepared by crushing bulk crystals. For instance:          
          i) TiO2 TEM specimens were prepared by crushing bulk single crystals into fine fragments in an agate mortar, dispersing in ethyl alcohol and finally by putting drops of ethyl alcohol on a carbon-film grid. [1]
          ii) TEM specimens of Be borides were prepared by crushing the materials in methanol in a boron carbide mortar and pestle that allowed a drop of the sample in suspension to dry on a lacey C coated Cu TEM grid. [2]
          iii) TEM specimens were prepared by crushing Pb(Zr0.3Ti0.7)O3 (PZT) powder in propanol in a pestle and mortar. Drops of the resulting suspensions were placed on holey carbon films on copper (Cu) grids. [3]

On the other hand, electropolishing is a well-known technique, mostly used to prepare (inter)metallic samples, because these materials are conducting, too soft for crushing, and easily damaged by conventional ion milling.

Then, different fragments with a thin wedge-shaped region can be analyzed with TEM.

 

 

 

 

 

 

 

 

 

 

 

[1] Susumu Yamada and Michiyoshi Tanaka, Structure of a stacking fault in the (-101) plane of TiO2, Journal of Electron Microscopy 1: 67-74 (1997).
[2] Laurence A. J. Garvie, Peter R. Buseck, and Peter Rez, Characterization of Beryllium–Boron-Bearing Materials by Parallel Electron Energy-Loss Spectroscopy (PEELS), Journal of Solid State Chemistry 133, 347 - 355 (1997).
[3] Harkins, P. and MacKenzie, M. and Craven, A.J. and McComb, D.W., Quantitative electron energy-loss spectroscopy (EELS) analyses of lead zirconate titanate. Micron, 39 (6). pp. 709-716, (2008).

 

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