Synthesis of Ordered Porous Graphitic‐C₃N₄ and Regularly Arranged Ta₃N₅ Nanoparticles by Using Self‐Assembled Silica Nanospheres as a Primary Template

Uniform-sized silica nanospheres (SNSs) assembled into close-packed structures were used as a primary template for ordered porous graphitic carbon nitride (g-C(3)N(4)), which was subsequently used as a hard template to generate regularly arranged Ta(3)N(5) nanoparticles of well-controlled size. Inverse opal g-C(3)N(4) structures with the uniform pore size of 20-80 nm were synthesized by polymerization of cyanamide and subsequent dissolution of the SNSs with an aqueous HF solution. Back-filling of the C(3)N(4) pores with tantalum precursors, followed by nitridation in an NH(3) flow gave regularly arranged, crystalline Ta(3)N(5) nanoparticles that are connected with each other. The surface areas of the Ta(3)N(5) samples were as high as 60 m(2) g(-1), and their particle size was tunable from 20 to 80 nm, which reflects the pore size of g-C(3)N(4). Polycrystalline hollow nanoparticles of Ta(3)N(5) were also obtained by infiltration of a reduced amount of the tantalum source into the g-C(3)N(4) template. An improved photocatalytic activity for H(2) evolution on the assembly of the Ta(3)N(5) nanoparticles under visible-light irradiation was attained as compared with that on a conventional Ta(3)N(5) bulk material with low surface area.