Synthesis of HfB2 Powders by Carbothermal Reduction

M. Shirvani, M. Mashhadi, M. Yosofi
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Abstract

: In this research, solid state carbothermal synthesis of HfB 2 Nano powders was investigated. For this purpose, HfO 2 , H 3 BO 3 , carbon active or phenolic resin were used as raw materials for carbothermal reaction. After 2-4 hours of milling the raw materials by a planetary ball in an ethanol media, the mixture was heat dried and pressed in to disks under pressure of 20-30 bar. The disks were then placed in a graphite crucible and heat-treated at 1500–1600 °C for 1 hour under flowing Ar atmosphere. The powder product was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and backscattered electron (BSE) imaging. The heat treatment temperature, amount of boric acid, milling and heat treatment time were recognized as four factors influencing synthesis and size of HfB 2 powder particles. SEM images reported irregular morphologies with a particle size of about 2-4 µm for HfB2 powder. The best sample was obtained at a molar ratio of HfO 2 : phenolic resin carbon: boric acid = 1:5:5 at 1600 °C after 1 hour of heat treatment. XRD results confirmed synthesis of pure HfB 2 with a crystallite size of about 60 nm.
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碳热还原法合成HfB2粉末
本研究采用固相碳热法合成了HfB2纳米粉体。为此,使用HfO2、H3BO3、碳活性树脂或酚醛树脂作为碳热反应的原料。在乙醇介质中用行星球研磨原料2-4小时后,将混合物加热干燥并在20-30巴的压力下压入盘中。然后将圆盘放置在石墨坩埚中,并在流动的Ar气氛下在1500–1600°C下热处理1小时。通过X射线衍射(XRD)、扫描电子显微镜(SEM)、能谱仪(EDS)和背散射电子(BSE)成像对粉末产物进行了分析。热处理温度、硼酸用量、研磨和热处理时间是影响HfB2粉末颗粒合成和尺寸的四个因素。SEM图像报道了HfB2粉末的颗粒尺寸约为2-4µm的不规则形态。热处理1小时后,在1600°C下,HfO2:酚醛树脂碳:硼酸的摩尔比为1:5:5时,获得了最佳样品。XRD结果证实合成了晶粒尺寸约为60nm的纯HfB2。
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