High-surface-area mesoporous materials expose abundant functional sites for improved performance in applications such as gas storage/separation, catalysis, and sensing. Recently, soft templates composed of amphiphilic surfactants and block copolymers have been used to introduce mesoporosity in various materials, including metals, metal oxides and carbonaceous compounds. In particular, mesoporous metals are attractive in electrocatalysis because their porous networks expose numerous unsaturated atoms on high-index facets that are highly active in catalysis. In this protocol, we describe how to create mesoporous metal films composed of gold, palladium, or platinum using block copolymer micelle templates. The amphiphilic block copolymer micelles are the sacrificial templates and generate uniform structures with tunable pore sizes in electrodeposited metal films. The procedure describes the electrodeposition in detail, including parameters such as micelle diameters, deposition potentials, and deposition times to ensure reproducibility. The micelle diameters can be controlled by swelling the micelles with different solvent mixtures or by using block copolymer micelles with different molecular weights. The deposition potentials and deposition times allow further control of the mesoporous structure and its thickness, respectively. Procedures for example applications are included: glucose oxidation, ethanol oxidation and methanol oxidation reactions. The synthetic methods for preparation of mesoporous metal films will take ~4 h; the subsequent electrochemical tests will take ~5 h for glucose sensing and ~3 h for alcohol oxidation reaction.

高表面积介孔材料暴露出丰富的功能位点，可提高气体储存/分离、催化和传感等应用的性能。最近，由两亲性表面活性剂和嵌段共聚物组成的软模板已被用于在各种材料中引入介孔性，包括金属、金属氧化物和碳质化合物。特别是，介孔金属在电催化方面很有吸引力，因为它们的多孔网络在高折射率面上暴露出许多不饱和原子，这些原子在催化方面具有很高的活性。在此协议中，我们描述了如何使用嵌段共聚物胶束模板创建由金、钯或铂组成的介孔金属膜。两亲性嵌段共聚物胶束是牺牲模板，可在电沉积金属薄膜中生成具有可调孔径的均匀结构。该过程详细描述了电沉积，包括胶束直径、沉积电位和沉积时间等参数，以确保重现性。可以通过用不同的溶剂混合物溶胀胶束或通过使用具有不同分子量的嵌段共聚物胶束来控制胶束直径。沉积电位和沉积时间分别允许进一步控制中孔结构及其厚度。示例应用程序包括：葡萄糖氧化、乙醇氧化和甲醇氧化反应。制备介孔金属膜的合成方法将耗时约 4 小时；