W-S-Cu cluster-based metal organic framework crystal material as well as preparation method and application thereof
A technology of metal-organic frameworks and crystal materials, applied in nonlinear optics, optics, instruments, etc., can solve problems such as high optical damage threshold, large nonlinear optical coefficient, complex synthesis, etc.
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Embodiment 1
[0035] (1) Add 0.1mmol ammonium tetrathiotungstate, 0.3mmol cuprous cyanide and 0.3mmol ammonium thiocyanate to 3mL N,N-dimethylformamide solvent and stir to obtain an orange solution;
[0036] (2) Add 0.05mmol 3,5-bis(4-pyridyl)-pyridine into the prepared orange solution and fully stir and dissolve to obtain a reaction solution;
[0037] (3) Filter the prepared reaction solution into a crystallization tube, slowly add 0.2mL N,N-dimethylformamide as a buffer to the upper layer of the filtrate, then add 6ml of acetonitrile as a diffusion layer to the upper layer of the buffer layer and seal it. After crystallization, filtration, washing and drying, the metal-organic framework crystalline material was obtained with a yield of 32%.
[0038] Such as figure 1 Shown is the three-dimensional structure diagram of the metal organic framework crystal material prepared in the present invention. It can be seen from the crystal structure analysis that the pentanuclear cluster [WS 4 Cu ...
Embodiment 2
[0046] (1) Add 0.1mmol ammonium tetrathiotungstate, 0.35mmol cuprous cyanide and 0.35mmol ammonium thiocyanate to 3mL N,N-dimethylformamide solvent and stir to obtain an orange solution;
[0047] (2) Add 0.05mmol 3,5-bis(4-pyridyl)-pyridine into the prepared orange solution and fully stir and dissolve to obtain a reaction solution;
[0048] (3) Filter the prepared reaction solution into a crystallization tube, slowly add 0.2mL N,N-dimethylformamide as a buffer to the upper layer of the filtrate, then add 6ml of acetonitrile as a diffusion layer to the upper layer of the buffer layer and seal it. Crystallization, filtration, washing, and drying give metal-organic framework crystalline materials with a yield of 30%.
Embodiment 3
[0050] (1) Add 0.1mmol ammonium tetrathiotungstate, 0.3mmol cuprous cyanide and 0.3mmol ammonium thiocyanate to 3mL N,N-dimethylformamide solvent and stir to obtain an orange solution;
[0051] (2) Add 0.05mmol 3,5-bis(4-pyridyl)-pyridine into the prepared orange solution and fully stir and dissolve to obtain a reaction solution;
[0052] (3) Filter the prepared reaction solution into a crystallization tube, slowly add 0.5mL N,N-dimethylformamide as a buffer to the upper layer of the filtrate, then add 8ml of acetonitrile as a diffusion layer to the upper layer of the buffer layer and seal it. After crystallization, filtration, washing and drying, the metal-organic framework crystalline material was obtained with a yield of 31%.
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