球磨法制备高氯酸铵基分子钙钛矿微纳米颗粒及安全性能分析

Preparation and Safety Performances of Ammonium Perchlorate-based Molecular Perovskite Micro/nano Particles by Ball Milling

为了改善高氯酸铵基分子钙钛矿((H2dabco)[NH4(ClO4)3],DAP)作为含能材料的安全性能,用球磨法制备出微纳米级DAP颗粒材料,采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、傅里叶红外光谱仪(FT-IR)以及Raman光谱仪分别对其形貌、结构进行表征。采用热重分析-差示扫描量热(TG-DSC)对其热分解性能进行表征,按GJB770B-2005爆炸概率法测试其撞击感度。结果表明,球磨法得到的细化DAP为0.5~10μm的微纳米级椭球颗粒,球磨后颗粒表面近似光滑,展现了良好的晶型稳定性;细化后DAP热分解峰温度为370.6℃,与原料DAP(热分解峰温度385.4℃)相比明显降低;与原料DAP(撞击感度为56%)相比,细化后DAP的撞击感度(28%)大幅降低。

In order to improve the safety performances of ammonium perchlorate-based molecular perovskite((H2dabco)[NH4(ClO4)3],DAP),DAP with micro/nano particles were prepared by ball milling.The morphology and structure of the as-obtained samples were characterized by scanning electron microscopy(SEM),X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FT-IR)and Raman spectroscopy(Raman).Thermal decomposition and impact sensitivity was investigated by thermo-gravimetric analysis-differential scanning calorimetry(TG-DSC)and GJB770B-2005 explosion probability method,respectively.The DAP obtained by ball-milling were micro/nano with ellipsoidal particles of 0.5-10μm,which had relatively smooth surface and good phase stability.The peak temperature of thermal decomposition of micro/nano DAP was 370.6℃,which obviously decreased as compared with raw DAP(385.4℃).Futhermore,the impact sensitivity of micro/nano DAP(28%)was much lower than that of raw DAP(56%).