XRD Line Broadening Analysis with Ball Milled Palladium

Palladium powder was deformed by ball milling under an argon atmosphere in two types of mills for different milling times. Two methods for X-ray diffraction line profile analysis, the Williamson-Hall method and the Warren-Averbach method, yielded similar trends, but different quantitative results for crystallite sizes (column lengths) and microstrains. With both methods, from the anisotropic line broadening for planetary milled Pd smaller crystallite sizes and larger microstrains were obtained along the <100> direction than along <111>. Milling in a shaker mill causes microstrain higher by a factor of about two than milling in a planetary mill. The evolution of the crystallite size upon milling was discussed in terms of bimodal size distributions.