以KPS起始劑合成之PS球爲模板製備TiO2中空球之研究

Preparation and Characterization of TiO2 Hollow Spheres Using KPS-initiated PS Spheres as Templates

詹志潔(C.C. Chan) ； 張忠傑(C.C. Chang) ； 朱慧娟(H.C. Chu) ； 陳靜誼(C.Y. Chen) ； 鄭凱云(K.Y. Cheng) ； 王仕凱(S.K. Wang)

《材料科學與工程》 38卷1期 (2006/03) Pp. 33-38

https://doi.org/10.6409/JMSE.200603.0033

摘要

本研究利用無乳化聚合法，以陰離子起始劑KPS合成粒徑爲137.9±16.0nm的聚苯乙烯球(PS)，將之作爲模板，再利用田口方法中的L9表，搭配鈦的前驅物異丙基醇鈦(TTIP)，以sol-gel法製備PS(下標 (core))/TiO2(下標 (shell))的核殼粒子，最後經高溫鍛燒移除PS球以得到TiO2中空球。藉由田口分析方法，分析TiO2殼層厚度以獲得最佳條件及最佳調控因子，在最佳條件下控制最佳調控因子（因子A）進行驗證實驗，可得到TiO2中空球之殼層厚度，隨著因子A（TTIP濃度）的增加而變厚。
利用熱分析儀檢測PS球與PS(下標 (core))/TiO2(下標 (shell))核殼粒子，得知PS球的熱裂解溫度爲400℃至450℃，並且在相同鍛燒時間下隨著殼層厚度增加PS球移除的溫度也隨之增加。經X光粉末繞射儀分析顯示，PS(下標 (core))/TiO2(下標 (shell))核殼複合微粒經過300℃熱處理後其晶相爲非晶相，400℃熱處理其晶相爲銳鈦礦相，600℃熱處理其晶相爲銳鈦礦相和金紅石相混晶。

關鍵字

二氧化鈦 ； 中空球 ； 核殼微粒 ； 聚苯乙烯球 ； 模板

並列摘要

Polystyrene (PS) with the size of 137.9±16.0nm, prepared by emulsion-free polymerization using potassium persulfate (KPS) as an anionic initiator, was used as a template to synthesize TiO2 hollow spheres. Sol-gel method and Taguchi L9 experimental design were adopted in this study. With PS templates and titanium tetraisopropoxide (TTIP) precursor, PS(subscript (core))/TiO2(subscript (shell)) core-shell particles were prepared. After removing the PS by calcination, TiO2 hollow spheres were obtained. Analysis by the Taguchi method, optimum preparation conditions was achieved. It was found that the shell thickness of the TiO2 hollow spheres depended significantly on the concentration of TTIP precursor (Factor A).
Characterization of PS(subscript (core))/TiO2(subscript (shell)) core-shell particles by TGA analysis, it is found that PS can be removed by calcination under 400℃~450℃. The thicker the shell thickness is, the higher the temperature is required. It is also found from XRD analysis that amorphous TiO2 was obtained under 300℃, anatase TiO2 was obtained at 400℃, and mixed phase of anatase and rutile was obtained at 600℃.

並列關鍵字

titanium dioxide ； hollow sphere ； core-shell particle ； polystyrene ； template