SEM analysis of DC magnetron sputtered beryllium films

Columnar structures produced by DC magnetron sputtering can be altered by using RF biased sputtering or by exposing the film to nitrogen pulses during sputtering, and these techniques are being evaluated to refine the grain structure in sputtered beryllium films deposited on fused silica substrates. Beryllium is brittle, and fractures in sputtered beryllium films tend to be intergranular; therefore, a convenient technique to analyze grain structure in these films is to fracture the coated specimens and examine them in an SEM. However, fine structure in sputtered deposits is difficult to image in an SEM, and both the low density and the low secondary electron emission coefficient of beryllium seriously compound this problem. Secondary electron emission can be improved by coating beryllium with Au or Au-Pd, and coating also was required to overcome severe charging of the fused silica substrate even at low voltage. The coating structure can obliterate much of the fine structure in beryllium films, but reasonable results were obtained by using the high-resolution capability of an Hitachi S-800 SEM and either ion-beam coating with Au-Pd or carbon coating by thermal evaporation.