Tunable multicolor luminescence materials can flexibly meet the needs of smart lighting, enabling efficient light energy use and minimizing waste. Lead-free hybrid double perovskites AMM(NO) hold great potential in luminescence, benefiting from their tunable composition, high light absorption, low synthesis cost, and environmental friendliness. However, achieving tunable multicolor emission within a single matrix of these materials has yet to be realized. In this study, a series of [(CH)N]KEuTb(NO) single crystals have been synthesized using an environmentally friendly and mild aqueous solution evaporation method. The two emitter centers, Tb and Eu, display energy transfer from Tb to Eu. The emission color of the as-synthesized crystals gradually changes from red to orange, then to yellow, and finally to green with an increase of Tb concentration, achieving yellow and green light emission in the three-dimensional rare-earth hybrid double perovskites for the first time. Green emission from [(CH)N]KTb(NO) displays the highest quantum yield at 87%. The millisecond-level emission decay time and high decomposition temperatures (365 °C) of [(CH)N]KEuTb(NO) single crystals highlight their potential for use in luminescent devices and phosphors, among other fields.
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