The microphase separation method is recognized as one of the most promising approaches to fabricate superhydrophobic surfaces (SHS), but it is still subjected to confined polymer materials, expensive instruments, and complicated techniques. Here we innovatively proposed a solvent evaporation-induced self-assembly method to produce SHS with facile prepared, environmentally friendly, ultrafast ambient temperature curable properties. In this study, a new category of silicone-urea copolymers was synthesized via step-growth polymerization of polydimethylsiloxane (PDMS) and different diisocyanates. The SHS induced by the microphase separation and solvent evaporation was then fabricated by spraying these copolymer solutions onto various substrates. It was discovered that the surface superhydrophobicity and morphology can be readily tuned by varying the spraying concentrations, diisocyantes, solvents, spraying heights, and molecular weight of PDMS. And those synthesized copolymers were assembled into micrometer-size fibers or spheres consisting of hierarchical microstructure using tetrahydrofuran as spraying solvent and 10–15 cm spraying height, and the contact angles of surfaces reached 119° and 153°, respectively. To further explore the possible formation mechanism of the SHS, small-angle scattering, and X-ray photoelectron spectroscopy were carried out to investigate the effects of the microphase separation and solvent evaporation. With the induced microscopic roughness caused by the copolymers, these prepared super-anti-wetting surfaces have been demonstrated for potential utilization in the field of waterproofing, self-cleaning, and antifouling aspects. This work provides an effective way for the potential large-scale preparation of superhydrophobic surfaces with environmentally friendly materials and straightforward techniques.

微相分离方法被认为是制造超疏水表面（SHS）最有前途的方法之一，但它仍然受到受限聚合物材料、昂贵仪器和复杂技术的影响。在这里，我们创新地提出了一种溶剂蒸发诱导的自组装方法，以生产具有易于制备、环保、超快环境温度可固化特性的 SHS。在这项研究中，通过聚二甲基硅氧烷 (PDMS) 和不同二异氰酸酯的逐步聚合反应，合成了一类新型有机硅-脲共聚物。然后通过将这些共聚物溶液喷涂到各种基材上来制造由微相分离和溶剂蒸发引起的 SHS。人们发现，通过改变喷涂浓度、二异氰酸酯、溶剂、喷涂高度和 PDMS 的分子量，可以很容易地调整表面超疏水性和形态。并且这些合成的共聚物被组装成由四氢呋喃作为喷涂溶剂和10-15cm喷涂高度的分级微结构组成的微米级纤维或球体，表面接触角分别达到119°和153°。为了进一步探索 SHS 的可能形成机制，进行了小角散射和 X 射线光电子能谱，以研究微相分离和溶剂蒸发的影响。由于共聚物引起的微观粗糙度，这些制备的超级抗湿表面已被证明在防水、自清洁和防污方面具有潜在用途。这项工作为使用环境友好的材料和简单的技术大规模制备超疏水表面提供了一种有效的方法。