摘要
本论文分三个层次进行论述,一是研究SiO2从非晶态到晶态的相变行为；二是在乳突形微/纳米SiO2和支化形微/纳米SiO2(包括蜈蚣状、树枝状和珊瑚状微/纳米SiO2)的制备和表征、生长机理以及影响微/纳米SiO2形貌结构的因素等方面展开了较深入的研究；三是对用水热法、化学气相沉积法、共混法制备的微/纳米SiO2核壳式复合材料和复合薄膜作了应用性探索。研究内容既考虑了微米技术的前沿性和现实性,又着眼于纳米科技的前瞻性和基础性,因此,此研究具有重要的理论意义和广泛的应用前景
首先,以稻壳为原料,制备微.纳米SiO2粉末,SEM、TEM和HRTEM表明,焙烧温度小于570℃时,微.纳米SiO2为非晶态；当焙烧温度达到1080℃时,非晶态SiO2转化为柱形晶态纳米SiO2。焙烧温度不仅是SiO2晶型转变的关键因素,而且对其纯度和形貌结构也影响很大。用有序原子集团切变沉积机制解释了SiO2相变行为。
其次,特殊形貌的微/纳米SiO2的制备。一是采用酸碱两步法从稻壳中提取了原生原位的乳突形微/纳米SiO2。研究结果表明,原生原位的乳突形微/纳米SiO2为非晶态,并整齐有序地排列着在稻壳的外表面上,分为双峰乳突、单峰乳突和瘤峰乳突三种类型；Si含量呈现递增梯度。二是采用水热法制备了不同形貌的支化形(包括蜈蚣状、树枝状和珊瑚状)微/纳米SiO2。研究结果表明,支化形由基体和分枝组成,分枝的各向平均生长速率和各向平均特征长度各不相同,具有各向异性特征；原材料、压力、温度以及保温时间等因素对支化形微/纳米SiO2形貌有很大的影响。气相沉积-悬键辅助生长机理解释了支化形微/纳米SiO2的生长过程。
最后,采用不同的方法制备了三种微/纳米SiO2复合材料。用水热法制备了核-壳-支C@SiO2@SiO2三层结构的复合材料,核心碳纳米线为单晶结构,壳层非晶态SiO2分两层包覆碳纳米线,最外层微/纳米SiO2的形貌是支化形状,悬键辅助沉积生长机理解释C@SiO2@SiO2的成形过程；用化学气相沉淀法制备了制备SiC@SiO2核壳式复合材料,直径约为25-50nm.,而长度约为几百微米,最长可达几个厘米。核心SiC纳米线存在“凹洞”填隙缺陷和“凸结头”缺陷。在438nm和464.5nm处有较强的PL性能。气态Si02沉积速率与SiC纳米线生长速率是否相匹配是调控微／纳米SiC@SiO2结构形貌的关键；通过共混法制备了SiO2/PI、 CNT@SiO2/PI和SiC@SiO2/PI三种复合薄膜。微/纳米SiO2在PI基体中分散均匀,具有较好的相容性,提高了复合薄膜的热稳定性能,降低了介电常数。CNT@SiO2/PI复合薄膜的热性能、硬度、耐磨性能、断裂强度和电性能的测试结果表明,CNT@SiO2的加入能提高复合薄膜的各项性能,特别是耐磨性能的提高更为显著。SiC@SiO2的加入,提高了SiC@SiO2/PI复合薄膜的热稳定性,体积电阻的下降致使导电性增强,机械性能,如断裂强度和断裂伸长率,硬度、耐磨性,得到有效的提高。SiC@SiO2主要通过裂纹偏转、SiC@SiO2拔出和桥接来实现增强补韧。
微/纳米SiO2包覆碳纳米管(CNT)和SiC纳米线,进行表面修饰,不仅改善了CNT和SiC纳米线的分散性,而且还整合优化了它们的性能。将微/纳米SiO2、核壳CNT@SiO2和SiC@SiO2有效地分散在PI基体中,可以提高复合薄膜综合性能指标。SiO2/PI复合薄膜的介电常数得到降低,CNT@SiO2/PI复合薄膜的耐磨性能的提高较为显著,SiC@SiO2/PI复合薄膜的断裂强度和韧性的增加更为突出。
This manuscript was discussed in three aspects:Firstly, the transition of amorphous SiO2to crystalline state was investigated. Secondly, the mastoid-like and the branch-like micro/nano SiO2were prepared and characterized, the growth mechanisms were researched in detail, and the factors that affecting the morphologies of micro/nano-SiO2were analyzed more in-depth. Thirdly, hydrothermal method, chemical vapor deposition and blending method were developed to prepare the micro/nano SiO2core-shell composite materials and composite films. Both the micron technology frontier and reality are concerned but also the forward-looking and foundation of nanotechnology are focused in this study. Therefore, this research is valuable in theory and application.
In this present study, the micro/nano SiO2was prepared from rice hull. The results of SEM, TEM and HRTEM show that the SiO2is amorphous when the roasting temperature is lower than570℃; the columnar-like SiO2appeared when the temperature rise to1080℃. The roasting temperature is critical factor for phase transformation of SiO2, it also decides the purity, morphology and structure of SiO2. These phenomena were explained by the change of deposition model of the ordered atomic clusters.
Then, the micro/nano SiO2with different morphologies were prepared by two different methods. The native in-situ mastoid SiO2can be purified by acid and alkali pretreatment from rice husk. Studies have shown that the mastoid SiO2is amorphous, is place in an orderly arrangement on the outer surface of the rice husk, and is divided into three types of bimodal mastoid, unimodal mastoid and tumor peak mastoid. Si content is increasing from the outer surface to the inner surface of the husk. In other side, three branch-like micro/nano SiO2with different morphologies (including centipede-like, arborization and coral-like) were prepared by hydrothermal method, and was constructed by the main body and dendrtics, The growth rate and length of these dendrtics are different from each other. The raw materials, pressure, temperature and the temperature keeping time have great effects on the morphologies of SiO2. The growth mechanism of branch-like micro/nano SiO2can be explained by the vapor deposition and dangling bonds-assisted growth.
At last, three kinds of micro/nano SiO2composites were prepared by different methods. C@SiO2@SiO2composites with core-shell-branch structure were prepared by hydrothermal method. The carbon nanowires are single crystal structure, and two SiO2shells are amorphous, the outer SiO2shell is branch-like structure. The formation of C@SiO2@SiO2can be explained by dangling bonds-assisted growth and the vapor deposition. SiC@SiO2composites with core-shell structure were prepared by chemistry vapor deposition. Its diameter is25-50nm, while its length is about hundreds of micrometers, even up to several centimeters. The defects of'convex knot'and'concave hole'exist on the SiC nanowires. There is a PL peak in438nm and464.5nm. The matching of deposition rate of the gaseous SiO2and the growth rate of SiC nanowires can control the morphology of SiC@SiO2. Three kinds of composite films, including SiO2/PI, CNT@SiO2/PI and SiC@SiO2/PI, were prepared by blending method. The heat stabilities of SiO2/PI were greatly increased and the dielectric constant was reduced by adding micro/nano SiO2which has better dispersion and compatibility in the PI matrix. The heat stability, rigidity, wear resistance, fracture strength, and electricity properties of CNT@SiO2/PI were improved by adding CNT@SiO2, especially the wear resistance property. By adding SiC@SiO2, the heat stabilities of SiC@SiO2/PI were greatly increased, and its volume resistivity was reduced to improve its conductivity. The mechanism properties, including fracture strength, rigidity, and wear resistance, were improved effectively. SiC@SiO2can enhance the strength and toughness by the crack deflexion, SiC@SiO2pulled out and bridged.
When the carbon nanotubes (CNT) and SiC nanowires were coated by the micro/nano SiO2to modify its surface, they can not only be improved its dispersion but also be integrated and optimized its performance. Micro/nano SiO2, the core-shell CNT@SiO2and SiC@SiO2dispersed in the PI matrix, can improve the performances of the composite film. A dielectric constant of SiO2/PI was reduced, the improving wear resistance of CNT@SiO2/PI is more distinguished, and the increasing fracture strength and toughness of SiC@SiO2/PI are more prominent.
引文
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