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Thesis Advisor曹竹友
Degree Grantor中国科学院研究生院
Abstract本文研究了在小型流化床反应器中通过三异丁基铝热分解CVD反应在平均粒径80μm的高折射率玻璃微珠表面淀积铝的过程,重点考察了操作条件-铝膜微结构-铝膜性质间的关系。目的是探索在流化床CVD 反应器中控制铝膜微结构的方法,从而生冰出具有和真空蒸镀铝膜同样性能的包铝微珠,以满足反光材料生产的需求。发现床层温度、微珠的反应时间和三异丁基铝的进料组成是决定铝膜微结构的关键因素。SEM观察表明和三异丁基铝的进料组成是决定铝膜微结构的关键因素。SEM观察表明所得到的铝膜有三种不同结构,即:三维岛状结构、孔洞结构和连续致密的铝膜。对于一定的进料组成(三异丁基铝分压约5-6mmHg)和包覆时间(30 min),在280-390℃范围中随着温度的升高,淀积最终得到的铝膜逐渐由三维岛状结构(大约280-320℃),变为孔洞结构(大构320-340℃),最后得到连续致密的铝膜。通过测定不同温度下的平均包覆速率,确定在流化床反应器中三异丁基铝在玻璃微珠上淀积反应的表观活化能为90.6 kJ/mol。用得到的包铝微珠反光膜,并检验反光膜的反光能力,结果表明用有连续致密铝膜的包铝微珠制成的反光膜的反光能力比起用其它两种结构的包铝微珠的反光膜 有极大改进,已经很接近于用传统的真空镀铝工艺得到的反光膜的反光能力。
Other AbstractIn this paper, aluminum film coating on high refractive index glass microsphears was studied, using the chemical vapor deposition (CVD) technique in a small size of fluidized bed, where triisobutylaluminum was used as the aluminum precursor. The purpose in to find the methods to control the microstructure of the aluminum film in the fluidized bed CVD reactor. We also wish to get aluminum film coating on glass microsphears having the same quality with that manufactured by physical vapor deposition method satisfying the manufacture of retroreflective material. Experiments were majorly studied the relationship between operation condition, film microstructure and film quality. It was found that there are three key parameters controlling the microstructure of the aluminum film ,which are bed temperature, resident time of the particle in the fluidized bed and the partial pressure of triisobutylaluminum in the fluidized bed. Three kinds of film microstructures were found with the scan electronic mirror (SEM) observation. They are: three dimensional island structure, micropore structure and continuous film. With a certain inlet composition condition, triisobutylaluminum partial pressure about 5-6 mmHg and a certain reaction time about 30 minutes, three kinds of microstructures could be observed by improving the deposition temperature from 280 ℃ to 390 ℃. Three dimensional island structure could be observed from about 280 ℃ to 320 ℃; micropore structure could be observed from about 320 ℃ to 340 ℃ and the continuous film could be observed from about 340 ℃ to 390 ℃. By measuring the mean coating rate at different deposition temperature, we got the value of apparent activation energy of triisobutylaluminum depositing on the high refractive index glass microsphears in the fluidized bed 90.64 kJ/mol. Retroreflective film was made with the glass microsphears coated by aluminum film, and the retroreflective activity was checked. The result was that the film with the mircorsphears having continuous aluminum film has much better retroreflective intense than that having other kinds of microstructure aluminum film. And the retroreflective intense of the film is very close to that made by physical vapor deposition (PVD) technique.
Document Type学位论文
Recommended Citation
GB/T 7714
施大新. 包铝玻璃微珠成膜质量控制的研究[D]. 中国科学院研究生院,1998.
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