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]
          iv) TEM specimens of superconductive YBa2Cu3O7-y (YBCO) crystals were prepared by crushing method, which did not generate point defects (vacancies and interstitials), while Ar milling created point defects. (see page1286)
          v) A bulk is crushed under methanol and the slurry is dispersed ultrasonically to separate out the finest particles. The samples is then floated on to Be microscope grids that has previously been coated with Formvar and carbon.
          vi) Microtome for specimen-sectioning (see page3334).

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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