【作者】 张华；

【导师】 韩建军； 赵修建；

【作者基本信息】 武汉理工大学 ， 材料物理与化学， 2008， 硕士

【摘要】 本论文以锂铝硅玻璃为基础,在确定各组分比的前提下,研究了成核剂银的含量对制备空穴孔阵基板的影响,采用屏蔽光辐照工艺,制备高密度空穴孔阵基片,优化了空穴孔阵基板的制备工艺,为多孔玻璃粉注入提供空间。同时,采用硅烷偶联剂将多孔玻璃粉与空穴孔阵复合,先将玻璃粉热处理分相,填入空穴孔阵中,再进行酸浸析处理以得到所需要的纳米多孔结构,从而实现一个大孔里面分布着无数纳米小孔的要求,可用来固定或隔离生物和化学样本,满足生物样本分析的要求。其中的空穴孔阵玻璃基片载体是利用特定Li₂O-Al₂O₃-SiO₂光敏微晶玻璃基片晶化后对稀HF酸具有的选择性刻蚀效应制得的,即将一定配比的Li₂O-Al₂O₃-SiO₂体系玻璃,经过光掩模UV曝光,在适当的温度下进行热处理从而使得曝光区域玻璃微晶化生成偏硅酸锂晶体,然后将部分晶化后的玻璃浸入一定浓度的HF酸溶液中,将易溶的微晶相刻蚀掉,获得空穴孔阵玻璃基片。纳米多孔玻璃介质是利用Na₂O-B₂O₃-SiO₂玻璃分相原理及随后的酸处理制得,通过对玻璃组成、热处理温度和时间、酸处理制度的调整从而实现孔径可控。根据研究所得相关工艺条件和参数,采用KH570为偶联剂,将多孔玻璃粉和空穴点阵基板进行复合,可制备出不同规格的点阵格式玻璃生物芯片载体材料。主要采用了XRD、SEM等测试手段对基片样品的结构进行了表征,并结合了UV-Vis光谱分析、DSC/TG测试分析,探讨了各因素对玻璃基片制备性能的影响。采用了场发射扫描电镜分析热处理制度、酸处理工艺制度对复合载体基片中多孔玻璃平均孔径和孔径分布的影响。研究表明:1.合适的成核剂含量对空穴孔阵的形成具有重要的作用,含有2.1g（总900克）的AgNO₃,质量百分比为0.3%的锂铝硅玻璃制备的空穴孔阵最佳。2.最合适的处理工艺为曝光60min,热处理制度为核化580℃/1.0h,晶化610℃/1.0h,5%vol.HF酸刻30min。3.偶联剂选用KH570,浓度16.7%（质量比1:5）,PH=4.0,搅拌时间30min。4.利用孔径大小1.0mm的玻璃基片与多孔玻璃粉复合,制备出纳米孔径为70nm左右,点阵排布为9×9的生物样本载体装置。更多还原

【Abstract】 On basis of Li₂O-Al₂O₃-SiO₂ system photosensitive glass-ceramics,the influence of the content of nucleating agent Ag have been studied in this paper,the precondition are that the contents of the glass have been confirmed.Masking irradiation process is used to prepare glass substrate carrier material with high density holes array,the preparation process is also improved,which is provided condition for compounding with porous glass powders.At the same time,silane coupling agent is used for the compound.First let the porous glass powers phase splitting,infilling in the substrate holes,then leaching in sulfuric acid for getting nano-multiaperture structure,so can realized requirement of that one macropore contain incalculable nano-pores.The production had great market potential in medical treatment、biotechnology and gene analysis.The glass substrate carrier with holes array on basis of Li₂O-Al₂O₃-SiO₂ system photosensitive glass-ceramics have been prepared,on which there was a selective solution rate in HF acid aqua after crystallization.The glass substrate first was exposed in ultraviolet radiation under a quartz mask.Next,there was crystallization in the exposure areas of the substrates and lithium metasilicate microcrystal could be gained after heat treatment at appropriate temperature.Finally,the partial crystallization substrate was etched with a given concentration HF acid aqua and holes array was gained as the crystallization areas were dissolved.Na₂O-B₂O₃-SiO₂ system glass was used for preparing nanometer porous glass.It was prepared by phase separation and succedent acid leaching.Pore size could be controlled through adjusting glass composition、thermal treatment and acid leaching system.Porous glass powder integrated with cavity substrate and KH-570 was adopted as bonder.It is possible to gain different form of holes array on the glass substrates on the basis of appropriate component of glass and process parameters resulted from the investigation.The structure of glass substrate sample was charactered using XRD,SEM, FESEM etc.The analysis results of UV-Vis spectroscopic,DSC/TG were also utilized to discuss how the factors effect on the properties of glass substrates.Average pore size and pore size distribution was charactered using FESEM mainly.It provided routes to prepare pore size controllable porous glass with interconnected pore and narrow pore size distribution.It could conclude from the results of experiment and analysis that:1.Appropriate nucleating agent content is important for preparation glass substrate carrier,2.1g（900g）AgNO3,mass percent 0.3%（wt%）is the optimum percentage.2.The best condition is heat treated in 580℃for 1.0h,crystalline in 610℃for 1.0h, etched with a concentration of 5 vol.%HF acid aqua.3.KH570 is used for the integration,concentration is 16.7%（1:5 wt）,PH=4.0, stirring 30min.4.The glass cavity sbustrate withφ1.0mm was integrated with porous glass powder KH570 was adopted as bonder.A 9×9 matrix biology sample carrier device can be prepared,the nano-pore size is about 70nm.更多还原