PART V - Communications - Chemical Etchants for Dislocations in Alpha Brass

TO the author's knowledge, only one satisfactory high-resolution technique for etch-pitting dislocations in Cu-Zn alloys has been published.' In that account, pits in 70/30 brass single crystals were produced by etching electrolytic ally in a 30 pct orthophosphoric acid bath. Thereafter, observations were made from surface replicas by electron microscopy. The method of pitting and observation permitted the high resolution necessary for the distinction of individual dislocations in arrays of pile-ups. However, no comment was offered concerning the possibility of obtaining pits which are amenable to optical resolution. Moreover, for adequate results, the electrolytic pitting process is invariably preceded by a polishing stage which could obscure the surface features of interest. Consequently, it would be desirable to be able to delineate, by solely chemical means, dislocations which could be detected by both optical and electron metallo-graphic techniques. This was achieved by the simple expedient of modifying two etchants reported by young2 to reveal dislocations on the (100) planes of pure copper. Single crystals of 70/30 a brass, described previously,3 were sectioned to provide a surface parallel to a set of {100) planes, mechanically polished, and subsequently electropolished at 2.4 v in a solution comprised of 2 parts H3PO4, 4 parts ethanol, and 3 parts water. The inclusion of ethanol tended to inhibit nonuniform surface attack. Etch-pitting was effected by a 2 to 3 sec immersion in a 70 pct aqueous solution of HNO3. The samples were then washed in a fast-flowing stream of water, and rinsed further in distilled water, and ethanol, before drying. It is important to note that this reagent should be either used immediately after mixing, or, if allowed to cool, reheated to about 35°C prior to use. No pitting was obtained at room temperature. Typical results are shown in Fig. 1 where (a) is an optical view of the pitted surface and (b) is an electron micrograph of a silicon monoxide replica shadowed with tungsten oxide. The former is characteristic of a somewhat longer etching time (-6 to 8 sec) which varied with bath temperature. Similar pits accrued from a 1/10 aqueous dilution of another of Young's solutions2—2 M FeC1,6H20 and 7.8 M HBr.