Abstract: Under hydrothermal synthetic conditions and from 1NiCl₂·6H₂O-mH₃PO₄-nNH₄F-pNH₃·H₂O-40H₂O(n=0, 3) system, we synthesized five kinds of materials
containing microporous VSB-1 and VSB-5 with 24 member rings, microporous sample A Ni₁₂(HPO₄)₆(PO₄)₂(OH)₆ with 12 member rings, layered
structural sample B NH₄NiPO₄·H₂O, and microporous sample C (C₂H₁₀N₂)[Ni(H₂O)₆](HPO₄)₂ with 8 member rings linked
by hydrogen bonds. They were characterized by XRD, FT-IR and TG. The effect factors of raw materials, pH, Ni/P ratio, template agents, and mineralization agent on synthetic products were investigated. The phase maps were also provided.
The effect factors of pH, Ni/P ratio, and mineralization agent play important roles in the synthetic processes. It is important that we synthesized VSB-1
without F ions.

Key words: hydrothermal syntheses, materials with open frameworks, nickel phosphates, effect factors