MgB_2的制备及工艺优化
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摘要
采用机械合金化和热处理相结合的方法制备了MgB_2化合物;采用振动式高能球磨机进行球磨,研究了磨球尺寸、球磨时间、热处理温度、保温时间等对合金化效果的影响,获得了最佳制备工艺参数。结果表明,在保持磨球质量与粉末物料质量比不变的情况下,采用大尺寸不锈钢球(Φ10mm)代替小尺寸球(Φ2mm,Φ5mm),可以提高球磨时的撞击能量,加速Mg-B粉末的机械合金化;热处理温度不宜超过Mg的熔点,否则Mg粉易发生氧化和挥发;热处理保温时间越长,对产物MgB_2物相形成越有利;MgB_2的最佳制备工艺参数为:Mg粉和B粉按摩尔比1∶2混合,球磨介质为Φ10mm的不锈钢球,磨球质量与粉末物料质量比20∶1,球磨时间12min,再将粉末在真空管式炉中进行热处理,升温速率为5℃/min,并在580℃下保温10h。
The MgB_2 compound was prepared by a combination method of mechanical alloying and heat treatment.The ball mill was carried out by a vibrating type high-energy ball grinder mill.The influence of grinding ball size,ball grinding time,heat treating temperature and heat preservation time on the alloying effect was studied.The optimum preparation technology parameters were obtained.The results show that the use of large-size stainless steel balls(Φ10 mm)instead of small-size balls(Φ2 mm,Φ5 mm)can increase the impact energy during ball milling and accelerate the mechanical alloying of Mg-B powder in the case of keeping the mass ratio of grinding ball and powder material unchanged.The heat treaing temperature should not exceed the melting point of Mg,otherwise Mg powder will be oxidized and volatilized easily.The longer the heat treatment holding time,the better the phase formation of the product MgB_2.The best preparation process parameters obtained is Mg powder and B powder mixed uniformly in mole ratio of 1∶2,ball mill medium asΦ10 mm stainless steel ball,the mass ratio of grinding ball and powder material as 20∶1,grinding time 12 min,heat treatment of powder in vacuum tube furnace,heating rate as5℃/min,heat preservation at 580℃for 10 h.
The MgB_2 compound was prepared by a combination method of mechanical alloying and heat treatment.The ball mill was carried out by a vibrating type high-energy ball grinder mill.The influence of grinding ball size,ball grinding time,heat treating temperature and heat preservation time on the alloying effect was studied.The optimum preparation technology parameters were obtained.The results show that the use of large-size stainless steel balls(Φ10 mm)instead of small-size balls(Φ2 mm,Φ5 mm)can increase the impact energy during ball milling and accelerate the mechanical alloying of Mg-B powder in the case of keeping the mass ratio of grinding ball and powder material unchanged.The heat treaing temperature should not exceed the melting point of Mg,otherwise Mg powder will be oxidized and volatilized easily.The longer the heat treatment holding time,the better the phase formation of the product MgB_2.The best preparation process parameters obtained is Mg powder and B powder mixed uniformly in mole ratio of 1∶2,ball mill medium asΦ10 mm stainless steel ball,the mass ratio of grinding ball and powder material as 20∶1,grinding time 12 min,heat treatment of powder in vacuum tube furnace,heating rate as5℃/min,heat preservation at 580℃for 10 h.
引文
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[2]陈冰虹,刘建忠,梁导轮,等.硼颗粒的包覆机理及工艺研究进展[J].火炸药学报,2016,39(5):13-21.CHEN Bing-hong,LIU Jian-zhong,LIANG Dao-lun,et al.Research progress in coating mechanism and technology of boron particles[J].Chinese Journal of Explosives&Propellants(Huozhayao Xuebao),2016,39(5):13-21.
[3] Shoshin Y L,Mudryy R S,Dreizin E L.Preparation and characterization of energetic Al-Mg mechanical alloy powders[J].Combustion and Flame,2002,128:259-269.
[4] Shtessel E,Dreizin E.High energy metallic mechanical alloys for new explosives and incendiary devices with controllable explosion parameters,ADA397097[R].Camden:Exotherm Corporation,2001.
[5] Aly Y,Schoenitz M,Dreizin E L.Ignition and combustion of mechanically alloyed Al-Mg powders with customized particle sizes[J].Combustion and Flame,2013,160:835-842.
[6] Whittaker M L,Sohn H Y,Cutler R A.Effect of synthesis atmosphere,wetting,and compaction on the purity of AlB2[J].Journal of Solid State Chemistry,2013,207:163-169.
[7]贾艳军.铝钛硼合金产品的作用机理和生产技术现状[J].有色金属加工,2017,46(4):33-34.JIA Yan-jun.Status of production technology and function mechanism of Al-Ti-B alloy products[J].Nonferrous Metals Processing,2017,46(4):33-34.
[8] Maisam Jalaly,Francisco JoséGotor.A new combustion route for synthesis of TaB2nanoparticles[J].Ceramics International,2018,44(1):1142-1146.
[9] Guo Yang,Zhang Wei,Zhou Xing,et al.Magnesium boride sintered as high-energy fuel[J].Journal of Thermal Analysis and Calorimetry,2013,133(2):787-791.
[10]郭洋.改性硼的制备、燃烧性能及应用研究[D].长沙:国防科技大学,2014.GUO Yang.Study on preparation,combustion property and application of modified boron[D].Changsha:National University of Defense Technology,2014.