Antimony-based fluorescent material and preparation method thereof
A technology of alkyl and alkynyl, which is applied in the direction of luminescent materials, chemical instruments and methods, electrical components, etc., and can solve the problems of price increase, low quantum yield, high price, etc.
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Embodiment 1
[0068] The preparation of embodiment 1 sample 1#~sample 5#
[0069] Mix imidazole ionic liquid, chlorine source, antimony source and water according to the ratio shown in Table 1, add organic solvent, heat to a certain temperature and keep stirring until the system is completely dissolved and transparent, keep for a period of time to form a supersaturated solution, then cool Stir continuously until colorless crystals are precipitated. After the crystals are completely precipitated, wash with absolute ethanol two to three times at room temperature, and dry to remove the organic solvent to obtain the corresponding sample. Table 1 shows the sample number, reactant ratio, organic solvent type, temperature during the dissolution process and the time kept at this temperature, and the product.
[0070] Table 1 Relationship between sample numbers, raw material ratios, preparation conditions and products
[0071]
Embodiment 2
[0072] The structural characterization of embodiment 2 sample
[0073] Sample 1#~sample 5# were characterized by X-ray single crystal diffraction, and the sample structure was analyzed by Shelxtl97. The results show that sample 1# to sample 5# all have the general formula shown in formula (1), and the following will take sample 1# to sample 3# as typical representatives to describe in detail.
[0074] Wherein, the crystal structure of sample 1# is obtained by x-ray single crystal diffraction, such as figure 1 shown. Sample 1# crystal belongs to the Cc space group, and its unit cell parameters are: β=102.004(2)°, Z=12. figure 1 The large pure black ball in the middle pyramid shape represents the Sb atom, the gray-black ball connected to it represents the Cl atom, the small black ball on the five-membered ring represents the N atom, the gray-white ball represents the C atom, and the white ball represents the H atom. atom. The powder XRD diffraction pattern of sample ...
Embodiment 3
[0078] The excitation spectrum of sample 1# is as Figure 7 As shown, the emission spectrum as Figure 8 shown. It can be seen that sample 1# has two emission peaks at 480nm and 583nm under the excitation of ultraviolet light, and the intensity of the peaks changes with the excitation wavelength. Specifically, as the excitation wavelength ranges from 270 to 303 to 376 nm, the emitted visible light changes from yellow to white to yellow. Under the excitation of 376nm ultraviolet light, its solid-state quantum yield is 86.3%, and its fluorescence lifetime is 4.275μs.
[0079] Excitation and emission spectra of sample 2# such as Figure 9 As shown, it can be seen that sample 2# can emit yellow-green light at 533nm under the excitation of 350nm ultraviolet light, and its solid-state quantum yield is measured to be 73.19%, and its fluorescence lifetime is 3.185μs.
[0080] The excitation and emission spectra of sample 3# are as Figure 10 As shown, it can be seen that sample 3...
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