| CPC C09K 11/883 (2013.01) [C09K 11/02 (2013.01); H10K 50/115 (2023.02); B82Y 20/00 (2013.01); B82Y 30/00 (2013.01); B82Y 40/00 (2013.01)] | 1 Claim |
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1. A preparation method of a core-shell structure quantum dot, comprising the following steps:
1) completely dissolving zinc acetate in a first oleic acid solution with a molar ratio of 1:2 by mixing at 200° C., conducting suction filtration to extract a solid phase product and drying to obtain a powder, and dissolving the powder in a first 1-octadecene solution to obtain a zinc precursor with a molar concentration of 0.3 mol/L;
mixing cadmium oxide, a second 1-octadecene solution, and a second oleic acid solution with a molar ratio of 1:10:4 at 200° C. until a resulting mixture is clarified to obtain a cadmium precursor;
dissolving a selenium powder in a third 1-octadecene solution and tri-n-octylphosphine with a molar ratio of 1:10:4 to allow ultrasonic vibration dissolution in a protective atmosphere to obtain a selenium precursor; and
dissolving a sulfur powder in a fourth 1-octadecene solution and the tri-n-octylphosphine with a molar ratio of 1:10:4 in a glove box to allow ultrasonic vibration dissolution in a protective atmosphere to obtain a sulfur precursor;
2) injecting a first amount of the zinc precursor, the cadmium precursor, a third oleic acid solution as an organic ligand, and a fifth 1-octadecene solution as an organic solvent into a first amount of the selenium precursor in a nitrogen atmosphere at 300° C. to induce a nucleation reaction and obtain a sixth 1-octadecene solution with a cadmium selenide core, wherein the first amount of the zinc precursor measured by the zinc acetate, the cadmium precursor measured by the cadmium oxide, and the first amount of the selenium precursor measured by the selenium powder are at a molar ratio of 16:2.5:1, and the oleic acid and cadmium ions in the cadmium oxide are at a molar ratio of 6:1;
3) coating an inner shell: injecting a second amount of the selenium precursor into a reactor containing the sixth 1-octadecene solution with the cadmium selenide core through a syringe pump at 3 mL/h, and then conducting heat preservation for 30 min; coating an outer shell layer: injecting 3 mmol of a second amount of the zinc precursor into the reactor, wherein the second amount of the zinc precursor measured by the zinc acetate and the second amount of the selenium precursor in the inner shell measured by the selenium powder are at a molar ratio of 1:1, conducting heat preservation for 10 min, adding 1 mmol of the sulfur precursor dropwise at 3 mL/h, wherein the sulfur precursor measured by the sulfur powder and a remaining zinc source after coating the inner shell measured by the zinc acetate are at a molar ratio of 3:1, and then conducting heat preservation for 30 min; wherein a selenium element and a zinc element in the inner shell are at a molar ratio of 1:1; a selenium element and a sulfur element in the outer shell are at a molar ratio of 1:1; and the cadmium precursor in step 2) measured by the cadmium oxide and the second amount of the selenium precursor in step 3) measured by the selenium powder are at a molar ratio of 2:3; and
4) cooling a quantum dot solution obtained in step 3) to 50° C., adding n-hexane and methanol with a volume ratio of 1:2 into a reaction system of the quantum dot solution in step 3), conducting a process of stirring vigorously for 5 min, layering by allowing to stand for 5 min, and removing a methanol phase, repeating five times, introducing argon to blow away residual n-hexane and methanol, and adding acetone and performing centrifugation to obtain a precipitate, namely the core-shell structure quantum dot; wherein
the core-shell structure quantum dot emits red light with a high color purity, and has a low emission half-peak width of 15 nm and an average size of 17 nm.
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