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超临界流体增强溶液扩散技术制备纳米CL-20及表征

     

摘要

采用超临界流体增强溶液扩散技术(SEDS法),以乙酸乙酯为溶剂,在9.0 MPa、40℃及溶液质量分数30%、溶液和反溶剂流速分别为5mL/min、8 kg/h的工艺条件下,制备了纳米六硝基六氮杂异伍兹烷(CL-20).用偏光显微镜与扫描电镜(SEM)、激光粒度分析仪、动态颗粒图像分析仪对细化前后的形貌、粒度、粒度分布和球形度进行表征,用傅里叶红外光谱仪(FT IR)和X射线衍射仪(XRD)对纳米CL-20的晶型进行了表征,测试了其热安定性和撞击感度.结果表明,所得CL 20边缘光滑且趋于球形,粒度均匀(1~2μm),所属晶型为β-型,与原料CL-20相比,晶型转变温度推后了约30℃,而分解峰温提前了6.74℃,撞击感度明显降低.%Nano-CL-20 was prepared with the solution of ethyl acetate through the process solution enhanced dispersion by supercritical fluids, and with the parameters of concentration 30%, pressure 9.0MPa, temperature 40℃ , solvent flow rate 5mL/min and CO2 flow rate 8kg/h. The morphology, particle size, size distribution and spherical degree of the sample before and after refinement were characterized by polarizing microscope, scanning electron mi-croscope(SEM), laser particle size analyzer and dynamic particle image analyzer. Crystal type of the refined CL-20 was identified by FT-IR and XRD. Thermal stability and impact sensitivity were measured. The results show that the edge of the refined particles is smooth and the shape is nearly spherical. The size distribution is uniform between l-2μm,and crystal type belongs to β. Compared with raw material, phase transformation temperatures postponed a-bout 30℃ , decomposition peak temperature advanced 6. 74℃ and impact sensitivity significantly reduced.

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