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On a Bimodal Distribution of Grain Size in Mechanically Alloyed Bulk Tungsten Heavy Alloys
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Elemental W and Ni powders were mechanically alloyed in a SPEX mill with WC grinding media for durations ranging from 5 to 50 hours, then compacted samples were sintered in hydrogen to generate bulk tungsten heavy alloys with 2, 4 and 6 wt.% Ni. Evidence of a bimodal grain size distribution was seen in X-ray diffractograms of sintered samples and confirmed by scanning electron microscopy. Grain sizes in the small-grained regions ranged from 200–600 nm; those in the large-grained regions ranged from 1–2 µm. Furthermore, the volume fraction of the small-grained region increased linearly as milling time increased. A slice from a sintered sample was prepared for examination by TEM, in which particles 30–100 nm in diameter were regularly observed on the boundaries of the 200–600 nm grains. EDS point analysis showed that the particles are WC. Therefore it is concluded that heterogeneously distributed contamination from the grinding media is continually incorporated during mechanical alloying and, during sintering, inhibits grain growth through Zener pinning. Densities of sintered samples increased as milling time increased to a maximum of almost 96% of the theoretical value. Density increases with respect to milling time were initially great but diminished upon further milling. While the samples with 4 and 6 wt.% Ni both approached 96% of the theoretical density value by 50 hours of milling, densities in the samples with 2 wt.% Ni were considerably lower. Thus it appears that the Ni that becomes incorporated into the bcc W structure during mechanical alloying activates W diffusion during sintering, though there is a limit to the amount of Ni that the W structure can accommodate. This is evinced in W lattice parameter values from the as-milled powders; while the lattice parameter drops considerable from 2 to 4 wt.% Ni, the difference between 4 and 6 wt.% Ni is much smaller and the Ni content limit surely falls between the two values. Otherwise-equivalent samples with added WC powder were also produced, but did not increase the volume fraction of the small-grained region – probably because the particles remained large and were homogeneously distributed.
- Doctoral Dissertations