Nanoparticles-based aerogels are 3-dimensional (3D) assemblies of macroscopic size that maintain the intrinsic properties of the initial nanoparticles. Accordingly, they bear immense potential to become an emerging platform for designing new and efficient photocatalysts. However, to take full advantage of this strategy, understanding of the multiscale processes occurring in such 3D-architectures is essential. Here, we prepared aerogels by co-assembling spherical Au, Pd, and PdAu with TiO₂ nanoparticles and investigated their photocatalytic properties for hydrogen generation. During gelation, the anatase nanoparticles undergo oriented attachment, homogeneously entrapping the metal nanoparticles in the growing network. The aerogels offer a high porosity with a mean pore size of ca. 34 nm and a large surface area of about 450 m² g^-1. The porous structure enhances the light-harvesting, reagent transport, and electron migration process, generating 3.5-fold more hydrogen in comparison to the corresponding powders.

基于纳米粒子的气凝胶是宏观尺寸的3维（3D）组件，可保持初始纳米粒子的固有特性。因此，它们具有巨大的潜力，可以成为设计新型高效光催化剂的新兴平台。但是，要充分利用此策略，必须了解这种3D架构中发生的多尺度过程。在这里，我们通过将球形Au，Pd和PdAu与TiO ₂共组装来制备气凝胶纳米颗粒，并研究了它们的光催化性能以产生氢气。在凝胶化过程中，锐钛矿型纳米粒子经过定向附着，使金属纳米粒子均匀地捕获在生长网络中。气凝胶具有高孔隙率，平均孔径约为。34nm和约450m ²  g ^-1的大表面积。多孔结构增强了光收集，试剂传输和电子迁移过程，与相应的粉末相比，生成的氢多出3.5倍。