A thermally activated delayed fluorescence crystalline frame material and its preparation method and application
A technology for thermally activated delayed and frame materials, which is applied in the field of thermally activated delayed fluorescent crystalline frame materials and its preparation, and can solve problems such as sensitive, difficult to achieve TADF emission, and quenching of luminescence
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Embodiment 1
[0093] Preparation of Thermally Activated Delayed Fluorescence Crystalline Framework Materials
[0094] (1) Synthesis of organic ligands
[0095] In a 250ml two-necked flask, add spirobiacridine (1.04g, 3mmol), methyl 4-bromobenzoate (1.29g, 6mmol), palladium acetate (34mg, 0.15mmol), tri-tert-butylphosphine tetrafluoroboric acid (131mg, 0.45mmol) and cesium carbonate (9.8g, 30mmol), then add 30ml redistilled toluene in an Ar atmosphere, heat to 120°C for 24h under anhydrous and oxygen-free conditions, then dichloromethane and petroleum ether The intermediate 1 (methyl 4,4'-(spirobiacridine)dibenzoate) was obtained after developing solvent column chromatography and drying by rotary evaporation. The yield was 82%. HRMS: theoretical value m / z[M+H + ]=615.2278, actual value m / z[M+H + ] = 615.2254.
[0096] In a 250ml one-necked flask, Intermediate 1 (1.5g, 2.44mmol) was dissolved in a mixed solution of 100mL tetrahydrofuran and water, wherein the volume ratio of tetrahydrofur...
Embodiment 2
[0105] (1) Preparation of Nanoscale Thermally Activated Delayed Fluorescence Crystalline Framework Materials
[0106] The organic ligand and synthesis method in this example are the same as those in Example 1.
[0107] In a 5ml glass bottle, add organic ligand (15mg, 0.025mmol), zirconium oxychloride (8mg, 0.025mmol) and N,N-dimethylformamide (1mL), after ultrasonication for 30min, add formic acid (10μL) , placed in an oven at 120°C for 24h. Then perform solvent exchange, wash with N,N-dimethylformamide and dichloromethane, and vacuum-dry at room temperature, and then vacuum-dry at 120°C to obtain a nanoscale heat-activated delayed fluorescence crystalline framework material, record For: Nano-Spiro-MOF-1.
[0108] The powder crystal diffraction pattern of Nano-Spiro-MOF-1 is as follows Figure 6 shown by Figure 6 It can be seen that the structure of Nano-Spiro-MOF-1 conforms to the crystal structure of Spiro-MOF-1.
[0109] The scanning electron microscope image of Nano-...
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