Abstract Synthesizing solids in molten fluxes enables the rapid diffusion of soluble species at temperatures lower than in solid‐state reactions, leading to crystal formation of kinetically stable compounds. In this study, we demonstrate the effectiveness of mixed hydroxide and halide fluxes in synthesizing complex Sr/Ag/Se in mixed LiOH/LiCl. We have accessed a series of two‐dimensional Sr(Ag1−xLix)2Se2 layered phases. With increased LiOH/LiCl ratio or reaction temperature, Li partially substituted Ag to form solid solutions of Sr(Ag1−xLix)2Se2 with x up to 0.45. In addition, a new type of intergrowth compound Sr3Se2(Ag1−xLix)2Se2 was synthesized upon further reaction of Sr(Ag1−xLix)2Se2 with SrSe. Both Sr(Ag1−xLix)2Se2 and Sr3Se2(Ag1−xLix)2Se2 exhibit a direct band gap, which increases with increasing Li substitution (x). Therefore, the band gap of Sr(Ag1−xLix)2Se2 can be precisely tuned via fine‐tuning x that is controlled by only the flux ratio and temperature.
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