机械球磨法制备纳米HATO及其性能测试  

Preparation of Nano-HATO by Mechanical Milling Method and Its Performance Test

作　　者：黎博 刘巧娥 高向东 肖磊[1] 郝嘎子 柯香[1] 张哲 李东楠 姜炜[1] LI Bo;LIU Qiao-e;GAO Xiang-dong;XIAO Lei;HAO Ga-zi;KE Xiang;ZHANG Zhe;LI Dong-nan;JIANG Wei(National Special Superfine Powder Engineer Research Center,Nanjing University of Science and Technology,Nanjing 210094,China;Research Institute of Gansu Yinguang Chemical Industry Group Co.,Ltd.,Baiyin Gansu 730900,China)

机构地区：[1]南京理工大学国家特种超细粉体工程技术研究中心,江苏南京210094 [2]甘肃银光化学工业集团有限公司科研所,甘肃白银730900

出　　处：《火炸药学报》2019年第1期97-102,I0006,共7页Chinese Journal of Explosives & Propellants

基　　金：国家安全重大基础研究项目

摘　　要：采用机械球磨法结合真空冷冻干燥技术制备了纳米5,5′-联四唑-1,1′-二氧二羟铵(HATO,又名TKX-50),用激光粒度仪分析其粒度分布,并通过扫描电子显微镜(SEM)观察其颗粒大小和形貌;采用傅里叶变换红外光谱(FT-IR)、X射线衍射(XRD)对其晶型、成分及纯度进行分析;采用热重(TG)和差示扫描量热法(DSC)分析其热分解特性,同时测试了工业微米级及纳米HATO的摩擦感度和撞击感度。结果表明,制备的纳米HATO颗粒大小均匀,形貌规则呈类球形,平均粒径小于100nm,且引入的杂质极少;纳米HATO的热分解峰温较工业微米级HATO稍有提前,最大热失重温度降低2.46℃,表观活化能下降2.02kJ/mol,自发火温度提高2.95℃,表明热力学稳定性基本不变,安定性有所提高;纳米HATO的撞击感度和摩擦感度分别为44.5cm和48%,与工业微米级HATO相比分别降低了44%和16%,表明机械感度明显降低,安全性得到提高。Nano-sized dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate(HATO,also known as TKX-50)was prepared by mechanical milling method combined with vacuum freeze-drying technology.Its particle size distribution was analyzed by a laser particle size analyzer,and its particle size and morphology were observed by scanning electron microscopy(SEM).The crystal form,composition and purity were analyzed by Fourier transform infrared spectroscopy(FT-IR)and X-ray diffraction(XRD).Its thermal decomposition characteristics were analyzed by thermogravimetry(TG)and differential scanning calorimetry(DSC),and the friction sensitivity and impact sensitivity of industrial micron-sized HATO and nano-HATO were tested.Results show that the prepared nano-HATO particles are uniform in size,spherical in shape,with an average particle size of less than 100 nm and few impurities.The thermal decomposition peak temperature of nano-HATO is slightly advanced compared with that of industrial micron-sized HATO.The maximum thermal mass loss temperature is reduced by 2.46℃,the apparent activation energy is decreased by 2.02 kJ/mol,and the self-ignition temperature is increased by 2.95℃,indicating that the thermodynamic stability is basically unchanged and the stability is improved.The impact sensitivity and friction sensitivity of nano-HATO are 44.5 cm and 48%,respectively,which are 44%and 16%lower than those of industrial micron-sized HATO,indicating that the mechanical sensitivity is significantly reduced and the safety is improved.

关 键 词：高能量密度材料 纳米HATO 机械球磨 纯度 热分解 感度 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O642[理学—物理化学]