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According to the principles of simultaneous equilibria and mass equilibria, CuInSe2 (CIS) were prepared by total aqueous process at normal pressure and room temperature. A series of thermodynamic equilibrium equations were deduced for the complex system of Cu+-In3+-Se2--NH3-L2--Cl--H2O (T=298 K), and the equilibrium curves of lgc-pH were drawn. It was found from these equilibrium diagrams that[NH3]T primarily affected the[Cu+]T concentration,[L2-]T influenced the[In3+]T concentration, and[Cl-]T had impact on both. The highest precipitation coefficient was obtained at pH 7.0-8.5. As a result, based on the principles of simultaneous equilibria and mass equilibria of the Cu+-In3+-Se2--NH3-L2--Cl--H2O system (T=298 K) and used total aqueous process at normal pressure and room temperature, CIS nanoparticles can be synthesized by adjusting the pH value to 7.0-8.5, and their size is about 20 to 50 nm.