Institute of Metals Division - Preparation of Beryllium Thin Films (TN)

THE production of thin films of beryllium became essential early in the irradiation program at Harwell in order to study the fundamentals of irradiation damage in this metal. In common with other metals, electron-microacope specimens of beryllium can be produced by different techniques. The techniques used to produce thin-film specimens varied according to the starting material. Most of the starting material was -0.060 in. thick. Large-area specimens (1 in. long by 0.5 in. wide) were chemically thinned to -0.005 in. thick in a solution containing 85 pct orthophosphoric acid, 10 pct chromium trioxide, and 5 pct sulfuric acid at 70°C prior to electropolishing. Small-area specimens, Fig. 1, had to be mechanically thinned prior to electropolishing because chemical thinning considerably reduces the area as well as the thickness. Mechanical thinning tends to produce a worked layer about 0.002 in. deep and hence this method cannot be used to thin bulk specimens below about 0.005 in. thick. Mechanical thinning is carried out by mounting the specimen on perspex then carefully polishing on wet grinding papers. Polishing is continued until about half the initial thickness is removed; the reverse side is then polished in a similar manner. After the bulk specimens have been mechanically or chemically thinned to -0.005 in. they are elec-tropolished in the solution shown in able I at 50" to 80°C. This solution should be prepared by adding the chromium trioxide to the orthophosphoric acid and then the glycerol last. The glycerol should be added slowly because a vigorous effervescence can occur. Electropolishing is carried out by holding the specimen in stainless-steel tweezers and gently agitating in the solution. Masking or "window" techniques are not required for beryllium, good microscope specimens being obtained from the edges of elec-tropolished foils. A stainless-steel beaker should be used, acting as the cathode and solution container. A closed circuit voltage of 30 v is used for polishing. Too low a voltage produces a matt surface and pitting occurs when it is too high. The solution temperature is important. If it is too low, the solution is viscous and bad polishing results and, if too high, etching of the specimen occurs. After electropolishing, the foils are thoroughly