多孔硅的制备、含能化填充及活性保持研究

发布时间：2018-03-25 11:47

本文选题：含能材料　切入点：多孔硅　出处：《南京理工大学》2017年硕士论文

【摘要】：本文以P型掺杂单晶硅片为原料,采用双槽电化学腐蚀法制备了结构稳定的多孔硅,确定了适宜装填氧化剂的最优制备条件;分别通过真空压差法、超声振荡法、三次滴加法对其进行含能化填充,分析了多孔硅制备条件和氧化剂填充方法对制得的纳米含能材料发火性能影响,并采用高速摄影对样品的燃烧过程进行了对比分析;以丙烯酸甲酯为原料对制备的多孔硅样品进行了氢化硅烷化改性,对比了改性前后样品的活性保持情况。获得的研究结果如下:(1)在一定腐蚀条件下,时间对样品的影响主要表现在腐蚀深度和多孔硅质量方面,电流密度的影响主要表现在孔径大小和孔隙率方面。在腐蚀时间30min、电流密度90 mA·cm-2的条件下制备的样品具有较好的多孔形貌和稳定的结构,其多孔硅层厚度约70μm,孔隙率达80%。(2)采用真空压差法填充氧化剂的综合效果最优,超声振荡法效果次之,三次滴加法效果最差。此外,真空压差法适用于超声振荡法所不能填充的高孔隙率样品,适用范围更广,装填效果优势明显。当样品电流密度为90mA·cm-2、腐蚀时间为45min时,制备的多孔硅含能材料氧化剂/燃料(O/F)摩尔比达0.44。高速摄影显示该样品发火时能产生猛烈的发火现象,形成长宽约为4cm的蘑菇云状火焰并持续13 ms。(3)采用丙烯酸甲酯对多孔硅进行氢化硅烷化改性有一定保持活性的效果。热分析和加速氧化实验结果表明,改性后进行含能化填充的样品具有一定的点火能力且保持较好,加速氧化后的样品点火性能优于同条件下未改性的样品。
[Abstract]:In this paper, porous silicon with stable structure was prepared by double cell electrochemical etching with P doped single crystal silicon wafer as raw material, and the optimum preparation conditions for filling oxidant were determined, respectively by vacuum pressure difference method, ultrasonic oscillation method, The preparation conditions of porous silicon and the effect of oxidant filling method on the pyrogenicity of the nano-energetic materials were analyzed, and the combustion process of the samples was analyzed by high-speed photography. The hydrosilane modification of porous silicon samples was carried out using methyl acrylate as raw material, and the activity of the samples before and after modification was compared. The results obtained are as follows: 1) under certain corrosion conditions, The influence of time on the sample is mainly reflected in the corrosion depth and the quality of porous silicon. The effect of current density is mainly on pore size and porosity. The samples prepared at corrosion time of 30 min and current density of 90 Ma cm-2 have good porous morphology and stable structure. The thickness of porous silicon layer is about 70 渭 m, and the porosity reaches 80 渭 m.) the comprehensive effect of using vacuum pressure difference method to fill oxidant is the best, the ultrasonic oscillation method is the second, and the third drop addition method is the worst. The vacuum pressure difference method is suitable for high porosity samples which can not be filled by ultrasonic oscillating method. The range of application is wider and the loading effect is obvious. When the current density of the sample is 90mA cm-2 and the corrosion time is 45min, The prepared porous silicon energetic material, oxidant / fuel / O / F molar Prida 0.44. High-speed photography shows that the sample can produce a violent combustion phenomenon when it fires. A mushroom cloud flame with length and width of about 4cm was formed and continued for 13 ms.3) the hydrosilanation modification of porous silicon by methyl acrylate has a certain activity. The results of thermal analysis and accelerated oxidation test show that, The modified samples filled with energetic materials have a certain ignition ability and keep good, and the accelerated oxidation samples have better ignition performance than the unmodified samples under the same conditions.
【学位授予单位】：南京理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ127.2;TQ560.1

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