Institute of Metals Division - Grain-Growth and Recrystallization Characteristics of Zirconium (With Discussion)

Grain-growth and recrystallization characteristics of a commercially pure zirconium prepared by the iodide process are reported. Grain growth from 640° to 800°C was continuous once initiated and obeyed D = kt". Recrystallization of zirconium occurred at temperatures of 450° to 550°C after deformations of 20 and 50 pct. Hardening from partially soluble inclusions prevented determination of the absolute rates of recrystallization, but the relative rates of recrystallization obtained are useful as a guide in fabrication practice. BASIC information needed as a guide in the hot and cold working and annealing of metals includes recrystallization and grain-growth data. A search of the literature revealed no such information for pure zirconium. This is a report of practical grain-growth and recrystallization results obtained for a commercial grade of pure zirconium on a project sponsored by the Office of Naval Research. In this work, isothermal grain-growth curves were obtained at five temperatures from 640" to 800°C inclusively; while recrystallization curves have been determined at 450°, 500°, and 550°C for the metal at the deformation levels of 20 and 50 pct. In addition to the usual variables of temperature, time, and deformation, distribution of the second phase found in all commercial grades of iodide zirconium is also treated as an important factor in these grain-growth and recrystallization studies. In conducting this work, two properties of zirconium were particularly pertinent in dictating experimental conditions. First, since zirconium undergoes a transformation from the a close-packed hexagonal form to the ß body-centered cubic form at 862°C, no recrystallization or grain-growth studies were made above 800°C. Second, because dissolved gases (oxygen, nitrogen and/or hydrogen) increase the hardness and lower the ductility of the solid metal, all annealing treatments in this investigation were carried out in vacuum or in a helium atmosphere. Materials and Methods The zirconium used in this investigation was prepared by the Foote Mineral Co. by deposition from its iodide. A spectrochemical analysis of the metal showed the following composition in weight pct: Hf, 2.1; Mg, 0.012; Fe, 0.035; Si, 0.095; Ti, 0.023; Al, 0.037; Mo, trace; Ni, trace; Cr, trace; Ca, 0.006. Conventional metallographic procedures involving hand polishing on wet metallographic papers, followed by final polishing on fine, levigated alumina on gamal cloth and a medium speed wheel were used throughout this investigation. Grain boundaries were revealed with modified Tucker's etch containing 20 parts glycerine, 2 parts hydrofluoric acid, and one part nitric acid. Grain-Growth Procedure: Three lots of zirconium, designated here as series A, B, and C were prepared for the grain-growth studies as follows: Series A was prepared by cold swaging the % in. as-deposited rod to a 3/16 in. final diameter, followed