Improved ball milling method for the synthesis of nanocrystalline TiFe compound ready to absorb hydrogen

Abstract

In this study, we propose a method to produce nanocrystalline TiFe powder by high-energy ball milling, in order to avoid the common sticking problem of the material to the milling tools, assuring a material prompt to absorb hydrogen as well. The method consists of making a preliminary milling operation with the elemental powders (50:50 stoichiometric ratio) to form a strong adhered layer of the milled material on the surfaces of the vial and balls. The main milling operation is then performed with a new powder charge (same composition as before), but now adding a process control agent (stearic acid). Various processing times - 2, 6, 10 and 20 h - were used in the milling experiments. Nanocrystalline TiFe was synthesized in this way with low oxygen contamination, full yields for milling times of 6 h or over, requiring no heat treatments for the first hydrogen absorption. Hydrogen storage capacity of 1.0 wt% at room temperature under 20 bar was attained by the sample milled for 6 h. Kinetic data from samples milled for 2 h and 6 h agreed with Jander model for the rate limiting step of the hydriding reaction, which is based on diffusion with constant interface area.