多孔硅的制備、含能化填充及活性保持研究
發(fā)布時(shí)間:2018-03-25 11:47
本文選題:含能材料 切入點(diǎn):多孔硅 出處:《南京理工大學(xué)》2017年碩士論文
【摘要】:本文以P型摻雜單晶硅片為原料,采用雙槽電化學(xué)腐蝕法制備了結(jié)構(gòu)穩(wěn)定的多孔硅,確定了適宜裝填氧化劑的最優(yōu)制備條件;分別通過(guò)真空壓差法、超聲振蕩法、三次滴加法對(duì)其進(jìn)行含能化填充,分析了多孔硅制備條件和氧化劑填充方法對(duì)制得的納米含能材料發(fā)火性能影響,并采用高速攝影對(duì)樣品的燃燒過(guò)程進(jìn)行了對(duì)比分析;以丙烯酸甲酯為原料對(duì)制備的多孔硅樣品進(jìn)行了氫化硅烷化改性,對(duì)比了改性前后樣品的活性保持情況。獲得的研究結(jié)果如下:(1)在一定腐蝕條件下,時(shí)間對(duì)樣品的影響主要表現(xiàn)在腐蝕深度和多孔硅質(zhì)量方面,電流密度的影響主要表現(xiàn)在孔徑大小和孔隙率方面。在腐蝕時(shí)間30min、電流密度90 mA·cm-2的條件下制備的樣品具有較好的多孔形貌和穩(wěn)定的結(jié)構(gòu),其多孔硅層厚度約70μm,孔隙率達(dá)80%。(2)采用真空壓差法填充氧化劑的綜合效果最優(yōu),超聲振蕩法效果次之,三次滴加法效果最差。此外,真空壓差法適用于超聲振蕩法所不能填充的高孔隙率樣品,適用范圍更廣,裝填效果優(yōu)勢(shì)明顯。當(dāng)樣品電流密度為90mA·cm-2、腐蝕時(shí)間為45min時(shí),制備的多孔硅含能材料氧化劑/燃料(O/F)摩爾比達(dá)0.44。高速攝影顯示該樣品發(fā)火時(shí)能產(chǎn)生猛烈的發(fā)火現(xiàn)象,形成長(zhǎng)寬約為4cm的蘑菇云狀火焰并持續(xù)13 ms。(3)采用丙烯酸甲酯對(duì)多孔硅進(jìn)行氫化硅烷化改性有一定保持活性的效果。熱分析和加速氧化實(shí)驗(yàn)結(jié)果表明,改性后進(jìn)行含能化填充的樣品具有一定的點(diǎn)火能力且保持較好,加速氧化后的樣品點(diǎn)火性能優(yōu)于同條件下未改性的樣品。
[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.
【學(xué)位授予單位】:南京理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類(lèi)號(hào)】:TQ127.2;TQ560.1
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