(1.昆明理工大學(xué) 真空冶金國(guó)家工程實(shí)驗(yàn)室，材料與冶金工程學(xué)院，昆明 650093；2. 東北大學(xué) 材料冶金學(xué)院，沈陽(yáng) 110004)
摘 要: 以B2O3為原料，Mg粉為還原劑，通過(guò)自蔓延鎂熱還原反應(yīng)獲得還原產(chǎn)物，經(jīng)過(guò)對(duì)還原產(chǎn)物的鹽酸溶浸后，制備出超微細(xì)無(wú)定形硼粉。研究鎂熱還原工藝對(duì)產(chǎn)物的影響，利用激光粒度分析儀測(cè)定無(wú)定形硼粉的粒徑，用靜態(tài)表面吸附儀測(cè)定77.3 K下硼粉的氮吸附等溫曲線，通過(guò)XRD和SEM分別對(duì)還原產(chǎn)物和無(wú)定形硼粉的物相及形貌進(jìn)行分析。結(jié)果表明：在B2O3-Mg體系中，影響硼粉純度的雜質(zhì)主要是反應(yīng)過(guò)程中生成的酸不溶物MgBx、BxO、Mg2SiO4、FeBx及較難溶物xMgO∙B2O3等，在鎂熱還原過(guò)程中應(yīng)盡量抑制該類化合物的生成。通過(guò)優(yōu)化制備工藝，在w(B2O3)/w(Mg)為3.0的條件下，制備出硼含量為94.6%、比表面積8.2 m2/g、等效粒徑0.36 μm的形貌不規(guī)則的超微細(xì)硼粉。
關(guān)鍵字: 無(wú)定形硼粉；超微細(xì)；鎂熱還原法；比表面積；富燃料推進(jìn)劑
（1. Science and Technology State Key Laboratory of Vacuum Metallurgy,Faculty of Materials and Metallurgical Engineering, Kunming University ofTechnology, Kunming 650093, China;2. School of Materials and Metallurgy, Northeastern University,Shenyang 110004, China）
Abstract:B2O3 and Mg powders were used as raw materials and reductant respectively. The reductive products were prepared by the magnesiothermic reaction. The boron powders were obtained after the reductive products were leached by HCl. The effects of reductive techniques on products were systematically studied. The particle sizes of boron powders were measured by laser particle analyzer and static volumetric absorption analyzer at 77.3 K. The phases and morphology of the reductive products and boron powders were characterized by XRD and SEM. The results show that the main effects on the purity of boron powders are the insoluble matter MgBx, BxO, Mg2SiO4, FeBx and xMgO∙B2O3. So these compounds must be effectively restrained in the process of magnesiothermic reduction. The irregular ultra-fine amorphous boron powder with purity of 94.6%, specific surface area of 8.2 m2/g and equivalent particle size of 0.36 μm can be gotten when w(B2O3)/w(Mg) (ratio of mass fraction) is 3.0.
Key words: amorphous boron powder; ultra-fine; magnesiothermic reduction; specific surface area; fuel-rich propellant
