本研究主要為探討冷凍解凍(Freeze/Thaw)程序強迫二氧化矽漿料聚集的應用價值，吾人討論此法與傳統的量測漿料穩定性的方法比較，並探討pH和高分子保護劑聚乙烯吡咯烷酮(Polyvinylpyrrolidone, PVP)對二氧化矽聚集的影響。
實驗結果發現，若干二氧化矽漿料會於冷凍解凍後凝聚，使用雷射粒徑儀量測其直徑至少有二十倍的增加。除了肉眼可見漿料從透明轉成乳白色會沉澱的漿料，光學顯微鏡與電子顯微鏡也可看到聚集顆粒在漿料中產生。電子顯微鏡可看到聚集體多數呈圓形，推想這是從四面八方均勻受力擠壓的結果，因為在冷凍過程中，冰晶成長排擠二氧化矽顆粒，強制顆粒互相靠近而發生聚集。
二氧化矽漿料在高pH值和高PVP含量能抵抗因為冷凍解凍引發的聚集效果，pH=6時至少需添加0.075 (g/g Silica)的PVP能完全抵抗凝聚，隨著pH值增加，可以添加較少PVP就能抵抗凝聚，當pH=10時，僅需0.025就可以完全抵抗凝聚。然而在pH<4時，加入PVP反而會直接導致凝聚，不需要經過冷凍解凍程序。冷凍解凍所得的聚集體形狀是緊密的球形，但加入PVP而直接凝聚的聚集體結構鬆散不規則，因此猜測是PVP成二氧化矽之間的架橋，而導致凝聚。
二氧化矽與PVP的吸附平衡也被建立，初期結果發現有多層吸附現象，熱重分析(TGA)中有些仍維持原來的燃燒溫度(450℃)，而有些PVP燃燒溫度因為吸附而改變(350℃)。PVP以氫鍵吸附的強度必定大於外圍PVP的吸附強度，因此以水清洗多餘的PVP即可得到單層吸附曲線。
另外研究冷凍解凍法應用於造粒，溶膠的二氧化矽冷凍解凍造粒後震實密度(tap density) 比冷凍乾燥法大上五倍。燃燒法製造的粉末(fumed silica)經過冷凍造粒後，震實密度也提高至五倍。造粒成功的粉末在壓錠成型後並以高溫燒結，兩種樣品經可達一定的透明度，然而燒結效果除與堆積有關外，基本粒子的大小也有密切的關係，不過經由冷凍解凍程序強迫奈米粒子聚集成為自由流動的micron等級之粒子確為可行的簡易替代方法。

Berne, B.J., R. Pecora, Dynamic Light Scattering. Courier Dover Publications, U.S.A. (2000)
Chang F. C., S. Tanawade and R. K. Singh, "Effects of Stress-Induced Particle Agglomeration on Defectivity during CMP of Low-k Dielectrics", Journal of the Electrochemical Society, 156, H39, (2009)
Chang F. C., P. Kumar, R. Singh, K. Balasundaram, J. Lee, J. Lee and R. K. Singh, "Role of interparticle forces during stress-induced agglomeration of CMP slurries", Colloids and Surfaces a-Physicochemical and Engineering Aspects, 389, 33, (2011)
Christian P., F. Von der Kammer, M. Baalousha and T. Hofmann, "Nanoparticles: structure, properties, preparation and behaviour in environmental media", Ecotoxicology, 17, 326, (2008)
Dhenge R. M., K. Washino, J. J. Cartwright, M. J. Hounslow and A. D. Salman, "Twin screw granulation using conveying screws: Effects of viscosity of granulation liquids and flow of powders", Powder Technology, 238, 77, (2013)
Despert G. and J. Oberdisse, "Formation of micelle-decorated colloidal silica by adsorption of nonionic surfactant", Langmuir, 19, 7604, (2003)
Lan Y. Q. and Y. Z. Li, "Effect of pump-induced particle agglomeration on CMP", Solid State Technology, 51, 40, (2008)
Kim H. J., J. K. Choi, M. K. Hong, K. Lee and Y. Ko, "Contact Behavior and Chemical Mechanical Polishing (CMP) Performance of Hole-Type Polishing Pad", ECS Journal of Solid State Science and Technology, 1, P204, (2012)
Kim J., U. Paik, Y. G. Jung, T. Katoh and J. G. Park, "The stability of nano fumed silica particles and its influence on chemical mechanical planarization for interlayer dielectrics", Japanese Journal of Applied Physics Part 1-Regular Papers Short Notes & Review Papers, 41, 4509, (2002)
Overbeek, J. T. G. "Recent Developments in Understanding of Colloid Stability." Journal of Colloid and Interface Science, 58, 408, (1977)
Oliver, M. R. "Chemical-Mechanical Planarization of Semiconductor Materials" Springer, U.S.A. (2004)
Palla B. J. and D. O. Shah, "Stabilization of high ionic strength slurries using surfactant mixtures: Molecular factors that determine optimal stability", Journal of Colloid and Interface Science, 256, 143, (2002)
Peethala B. C., D. Roy and S. V. Babu, "Controlling the Galvanic Corrosion of Copper during Chemical Mechanical Planarization of Ruthenium Barrier Films", Electrochemical and Solid State Letters, 14, H306, (2011)
Reed J. S. "Principles of Ceramics Processing" John Wiley & Sons, Incorporated, U.S.A. (2000)
Remsen E. E., S. Anjur, D. Boldridge, M. Kamiti, S. T. Li, T. Johns, C. Dowell, J. Kasthurirangan and P. Feeney, "Analysis of large particle count in fumed silica slurries and its correlation with scratch defects generated by CMP", Journal of the Electrochemical Society, 153, G453, (2006)
Richardson J. F. and W. N. Zaki, "Sedimentation and fluidisation: part 1", Chemical Engineering Research & Design, 75, S82, (1997)
Shaw, D. J. "Introduction to Colloid & Surface Chemistry" 4th ed, Butterworth-Heinemann, U.S.A. (1992)
Song X. L., N. Jiang, Y. K. Li, D. Y. Xu and G. Z. Qiu, "Synthesis of CeO2-coated SiO2 nanoparticle and dispersion stability of its suspension", Materials Chemistry and Physics, 110, 128, (2008)
Suzuki H., M. Murou, H. Kitano, K. Ohno and Y. Saruwatari, "Silica particles coated with zwitterionic polymer brush: Formation of colloidal crystals and anti-biofouling properties in aqueous medium", Colloids and Surfaces B-Biointerfaces, 84, 111, (2011)
Tseng T. Y. and J. J. Yu, "Various Atmosphere Effects on Sintering of Compacts of Sio2 Microspheres", Journal of Materials Science, 21, 3615, (1986)
Tomkins M. R., T. E. Baldock and P. Nielsen, "Hindered settling of sand grains", Sedimentology, 52, 1425, (2005)
Toki M., T. Y. Chow, T. Ohnaka, H. Samura and T. Saegusa, "Structure of Poly(Vinylpyrrolidone)-Silica Hybrid", Polymer Bulletin, 29, 653, (1992)
Xiao, H. "Introduction to Semiconductor Manufacturing Technology" Prentice Hall, U.S.A. (2000)
Zhang L., P. Li, D. Li, S. Guo and E. Wang, "Effect of freeze-thawing on lipid bilayer-protected gold nanoparticles", Langmuir, 24, 3407, (2008)
ITRS, Technology Working Group Reports：Front End Processes, ITRS, U.S.A. (2011)
林明智 "化學機械研磨的微觀機制探討" 中央大學論文，台灣 (2000)
高濂 "奈米粉體的分散與表面改性" 五南圖書出版，台灣 (2005)
高振裕 "軟性電子之印刷式奈米材料與元件研究" 清華大學論文，台灣 (2010)
李政麟 "化學機械研磨用奈米級二氧化鈰粉體之合成" 逢甲大學論文，台灣 (2002)
吳宗哲 "透明的中孔二氧化矽塊材" 國立中央大學化學工程與材料工程研究所碩士論文，台灣 (2007)
吳聖威 "奈米級二氧化矽SiO2粒子之燒結" 國立清華大學化學工程學系論文，台灣 (2001)
國研院儀器科技研究中心 "奈米檢測技術" 財團法人國家實驗研究院儀器科技研究中心，台灣 (2009)
王建榮，林必窕 "半導體平坦化CMP技術" 全華圖書，台灣 (2000)
林宗賢 "噴霧乾燥法製作六種水分散性粒劑劑型配方之研發" 朝陽科技大學應用化學系論文，台灣 (2004)