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Development of multiceramics compornent and monodispersed particle preparation by new emulsion method for practical precess

新型乳液法制备多陶瓷组分和单分散颗粒的开发及实用化工艺

基本信息

批准号：
07555669
负责人：
MIZUTANI Nobuyasu
金额：
$ 0.9万
依托单位：
Tokyo Institute of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (A)
财政年份：
1995
资助国家：
日本
起止时间：
1995 至 1996
项目状态：
已结题

项目摘要

This study was carried out for preperation and size control of sperical and monodispersed particles by hydrolysis reaction in acetnitril-n-octanol mixed solvent. To understand the solution condition before and after hydrolysis reaction we decided the solubility of Ti (OC_4H_9)_4. The solubility of Ti (OC_4H_9)_4 was decreased accompanied by the increase of acetnitril concentration. Above 60vol% of acetnitril concentration it becomam 0 and alcoxide were sedimented forming emulsion or solution under that condition. Stability of the emulsion was influenced by HPC concentration. There was critical and minumam HPC concentration for emulsion existing in stable condition.We came to abel to get monodispersed spherical particles by using homogeneous solution and emulsion method by the ultrasonic waves at the high acetnitril concentration, in which monodispersed particle could not synthesized before. Several parameters which influence the size of the particels were investigated. When composition of the mixed solvent was changed the size of the particles were changed between 0.5-6mum ([Ti (OC_4H_9)_4] =0.1mol/l, [H_2O] =0.5mol/l, [HPC]=0.2g/l). And when concentratio of HPC was changed the size of the particles were changed between 0.5-200mum ([Ti (OC_4H_9)_4] =0.1mol/l, [Acetonitril] =80vol%, [H_2O] =0.5mol/l, ). And at the same time in-situ observation of hydrolysis reaction in the particle of 100mum in diameter.Internal structure and thermal change of the particles about 10-100mum in diameter. The inside of the as-prepared particle was homogenious and packed thoroughly Sometimes hole was existed at the center of the particle. By thermal analyzes they were proved that the over 50wt% of organic materials were remained in the as-prepared particles in which the non-reacted alcoxid could by aging more long time. The shapes of the particles were maintained up to 900ﾟC.

本文研究了在乙腈-正辛醇混合溶剂中，通过水解反应制备球形单分散粒子及其粒径控制。为了了解水解反应前后的溶解状态，我们测定了Ti（OC_4H_9）_4的溶解度。随着乙腈浓度的增加，Ti（OC_4H_9）_4的溶解度降低。乙腈浓度大于60vol%时，乙腈0和醇盐在此条件下沉降形成乳状液或溶液。HPC浓度对乳液稳定性有影响。在稳定条件下，HPC存在临界浓度和最小浓度，在乙腈浓度较高时，采用均相溶液法和超声波乳化法，可以得到单分散的球形粒子，而在此条件下，单分散的球形粒子是不能合成的。研究了影响颗粒尺寸的几个参数。当混合溶剂的组成改变时，颗粒的尺寸在0.5- 6 μ m之间变化（[Ti（OC_4H_9）_4] =0.1mol/l，[H_2O] =0.5mol/l，[HPC]=0.2g/l）。当HPC浓度变化时（[Ti（OC_4H_9）_4] =0.1mol/l，[乙腈] = 80vol%，[H_2O] =0.5mol/l），颗粒尺寸在0.5- 200 μ m之间变化。同时对粒径为100 μ m的颗粒进行了水解反应的原位观察，并对粒径为10- 100 μ m的颗粒的内部结构和热变化进行了研究。所制备的纳米粒子内部均匀、致密，有时在粒子中心存在孔洞。热分析结果表明，所制得的颗粒中有机物的含量超过50wt%，其中未反应的醇类物质可以通过较长时间的老化而得到保留。颗粒的形状在高达900摄氏度的温度下保持不变。