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The microstructured surface of materials were fabricated by a two-step acid-base catalyzed sol-gel process. In fluorinated polymer with PTFE doping, the well-proportioned composite sols were prepared using sol-gel processing under the hydrochloric acid and deficiency of water conditions. After the substrate was coated by composite sols, and the gelation treatment on the surface of composite coating, the micrometer-scale and nanometer-scale hierarchical structures were formed in surface layer of material. XPS and TEM technologies were employed to identify that the gelation occurs just on the surface of composite coating. The morphology of coating surface was observed by SEM and AFM technologies. The microstructured surface of material can be fabricated using this inexpensive and easily controlled method on low surface energy resin materials, the super-hydrophobic coatings materials can be prepared.