A kind of preparation method of low-cost cadmium phosphide quantum dot material

A quantum dot material, cadmium phosphide technology, which is applied in the field of preparation of low-cost cadmium phosphide quantum dot materials, can solve the problems of transportation and storage conditions, no industrialization prospects, difficulty in scaling up synthesis experiments, etc., and achieve easy separation , production cost reduction, and the effect of easy experimental dosage

CN102268253AInactive Publication Date: 2011-12-07HEFEI UNIV OF TECH
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2011-12-07
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a preparation method of a low-cost cadmium phosphide quantum dot material. The preparation method comprises the following steps: based on a cheap cadmium compound such as cadmium oxide, cadmium acetate or cadmium cetylacetonate and the like as a raw material, dissolving the cadmium compound and long-chain fatty acid in octadecylene at a high temperature so as to prepare a long-chain fatty acid salt of cadmium; or dissolving cadmium cetylacetonate in organic amine, and then carrying out a gas-liquid reaction based on hydrogen phosphide as a phosphorus source so as to prepare the high-quality cadmium phosphide quantum dot luminescent material. According to the invention, a cheap and continuously operable synthesis method is provided for the cadmium phosphide quantum dot material, and a solid foundation is provided for industrialized production of the cadmium phosphide quantum dot material; and through controlling factors such as reaction temperature, time and the like, the luminescence of the cadmium phosphide quantum dot material can be achieved in a wide region ranging from visible light (460nm) to infrared light (1500nm).
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Description

1. Technical field

[0001] The invention relates to a preparation method of a nanometer material, in particular to a preparation method of a low-cost cadmium phosphide quantum dot material. 2. Background technology

[0002] Cadmium phosphide is an important II-V semiconductor material, because cadmium phosphide has a narrow bandwidth (0.55eV), a high dielectric constant (5.8), a large Bohr radius (18nm) and excitation Molecules have the advantages of very light effective mass [1-4], and are expected to be applied in the fields of biomarkers, fluorescent probes, photoelectric conversion, solar cells, etc. [5-8]. When the size of the semiconductor is smaller than the Bohr radius, the quantum size effect is obvious, the size decreases, and the absorption spectrum peak shows a blue shift. Because cadmium phosphide has a relatively small forbidden band width [3], with the reduction of its physical size, it can achieve a wide range of mediation from the infrared to the visible reg...

Examples

Embodiment 1

[0050] The preparation method of low-cost cadmium phosphide quantum dot material in the present embodiment is to operate according to the following steps:

[0051] a, Preparation of cadmium precursor

[0052] Put 0.258g of cadmium oxide and 1.3mL of oleic acid in a 25mL three-necked flask, add 15mL of octadecene, vacuumize (0.5-0.05mbar) at room temperature for 30 minutes, then heat to 270°C in a nitrogen atmosphere, and keep warm for 20 minutes to obtain Cadmium oleate solution;

[0053] b. Preparation of cadmium phosphide quantum dots

[0054] The temperature of the obtained cadmium oleate solution is controlled at 60°C, and with the assistance of nitrogen gas flow, the pH 3 gas, pH 3 Flow rate is 2mL / min, carrier gas N 2 The flow rate is 30mL / min, N 2 with PH 3 The flow rate ratio is 15:1, and the insulation reaction is 180min to obtain an octadecene solution of cadmium phosphide quantum dots, with a yield of 97.5%;

[0055] c. Separation and purification

[0056] A...

Embodiment 2

[0058] The preparation method of low-cost cadmium phosphide quantum dot material in the present embodiment is to operate according to the following steps:

[0059] a, Preparation of cadmium precursor

[0060] Put 0.258g of cadmium oxide and 0.8g of lauric acid in a 25mL three-necked flask, add 15mL of octadecene, vacuumize (0.5-0.05mbar) at room temperature for 30 minutes, then heat to 250°C in a nitrogen atmosphere, and keep the temperature for 20 minutes to obtain Cadmium laurate solution;

[0061] b. Preparation of cadmium phosphide quantum dots

[0062] The temperature of the obtained cadmium laurate solution is controlled at 120°C, and with the assistance of nitrogen gas flow, the pH 3 gas, pH 3 Flow rate is 2mL / min, carrier gas N 2 The flow rate is 2mL / min, N 2 with PH 3 The flow rate ratio is 1:1, and the insulation reaction is 120min to obtain an octadecene solution of cadmium phosphide quantum dots, with a yield of 97.0%;

[0063] c, the method for separation a...

Embodiment 3

[0065] The preparation method of low-cost cadmium phosphide quantum dot material in the present embodiment is to operate according to the following steps:

[0066] a, Preparation of cadmium precursor

[0067] Put 0.258g of cadmium oxide and 1.05g of palmitic acid in a 25mL three-necked flask, add 15mL of octadecene, vacuumize (0.5-0.05mbar) at room temperature for 30 minutes, then heat to 260°C in a nitrogen atmosphere, and keep the temperature for 20 minutes to obtain Cadmium palmitate solution;

[0068] b. Preparation of cadmium phosphide quantum dots

[0069] The temperature of the resulting cadmium palmitate solution is controlled at 180°C, and with the assistance of nitrogen gas flow, the pH 3 gas, pH 3 Flow rate is 2mL / min, carrier gas N 2 The flow rate is 20mL / min, N 2 with PH 3 The flow rate ratio is 10:1, and the heat preservation reaction is 30min to obtain an octadecene solution of cadmium phosphide quantum dots, with a yield of 97.3%;

[0070] c, the method ...