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Those materials are widely used as catalyst supports, thermal insulators, sound insulators, shock adsorbents, and separation media. The aim of this research is to synthesize monolithic porous materials and observe from the aspects of both 3D bulk structure and 2D surface. Samples with high porosity are synthesized via a sol-gel process by utilizing phase separation and aggregation of particles. Structural and bulk properties are observed to develop practical applications such as thermal insulators, optical devices, and soft robotics. Also, I try to find processes to form macroporous structures by using interface phenomenon between particles/fibers and polymers. 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