用电流在约 1 分钟内快速烧结铼

Emmanuel A. Bamidele, Alan W. Weimer, Rishi Raj
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摘要

我们的研究表明,通过向狗骨形试样直接注入电流,可以将铼从粉末烧结到接近全密度(99.96%)。电流以 1 A s-1 的速度增加。约 30 秒后,当试样温度升至 900 ℃ 时,试样突然烧结。实验是在手套箱内的氩气环境中进行的,没有加热炉。报告了以下操作过程中的测量结果:(i) 用快速照相机测量收缩应变;(ii) 用电压和电流测量电阻率;(iii) 用高温计测量温度;(iv) 用光谱仪测量电致发光光谱。在第一个烧结周期中,样品烧结到了全密度,随后用同一样品又进行了两个闪光周期。在第一个周期中,电阻的变化呈现出一个峰值,这是由于颗粒间的界面电阻减弱引起的;而在第二和第三个周期中,该峰值消失了。快速烧结的原因是产生了空位-间隙(Frenkel)对形式的缺陷。Frenkels 的浓度是通过原位量热法估算出来的,输入的电能与辐射、对流和比热损失的能量之间的差值被归因于缺陷生成的内热反应。通过这种方法,我们计算出 Frenkel 对的浓度为 10 mol pct。闪速烧结试样的电阻值高于文献值,这可能是这些缺陷造成的。极低的烧结温度和匿名的高缺陷浓度意味着金属的闪蒸烧结是一种远非平衡的现象。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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Flash Sintering of Rhenium in About 1 Minute with Electrical Current

We show that rhenium can be sintered from powders to nearly full density (99.96 pct) by directly injecting electrical current into dogbone shaped specimens. The current was increased at a rate of 1 A s−1. The specimen sintered abruptly after about 30 seconds when its temperature had risen to 900 °C. The experiments were carried out without furnace heating, within a glove box in Ar atmosphere. The following in-operando measurements are reported, (i) shrinkage strain with a rapid rate camera, (ii) resistivity measured by voltage and current, (iii) temperature measured with a pyrometer, and (iv) electroluminescence spectra measured with a spectrometer. The sintering cycle, the first, during which the sample sintered to full density, was followed by two more flash cycles with the same specimen. In the first cycle, the change in resistance exhibited a peak arising from abatement of interparticle interface resistance; the peak was absent in the second and third cycles. The rapid sintering is attributed to the generation of defects in the form of vacancy-interstitial (Frenkel) pairs. The concentration of the Frenkels was estimated from in-situ calorimetry, where the difference between the electrical input energy, and the energy lost to radiation, convection and specific heat, was attributed to an endothermic reaction for defect generation. In this way we calculated a concentration of ∼ 10 mol pct of Frenkel pairs. The resistance of the flash sintered specimens was higher than literature values, presumably due to these defects. The very low sintering temperature and the anonymously high defect concentrations mean that flash sintering of metals is a far-from-equilibrium phenomenon.

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