Method for efficiently synthesizing CuInSe2 quantum dots with chalcopyrite structures

A chalcopyrite and quantum dot technology is applied in the field of efficient synthesis of CuInSe2 quantum dots with chalcopyrite structure, which can solve the problems of large particle size, small output and high price of quantum dots, and achieves controllable particle size and particle size. small effect

Active Publication Date: 2017-06-13
WUHAN UNIV OF TECH
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  • Claims
  • Application Information

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Problems solved by technology

However, the raw materials (anhydrous indium trichloride, indium acetate, etc.) and solvent (oleylamine) used in the current hot injection method are expensive, and the dissolving of selenium powder needs expensive phosphorus-containing solvents (tri-n-octylphosphine, tri-n-octylphosphine, tri-n-octylphosphine, etc.) Butylphosphine, etc.) or higher dissolution temperature (soluble in oleylamine at about 250°C), is not conducive to the large-scale synthesis of CuInSe by hot injection method 2 quantum dot
According to the literature Zhong H, Li Y, Ye M, et al.A facile route to synthesize chalcopyrite CuInSe 2 nanocrystals in non-coordinating solvent[J].Nanotechnology,2007,18(2):025602. The reported method uses a mixture of dodecylmercaptan and octadecene as a metal precursor solvent, and tri-n-octyl Phosphine is used as a solvent for selenium powder, injected at 180°C and reacted for 1 hour, CuInSe with uniform particle size can be obtained 2 Quantum dots, but the mixture of dodecyl mercaptan and octadecene has a high viscosity at low temperature, it is difficult to remove the water and air dissolved in it, and the expensive and environmentally harmful tri-n-octyl phosphine is used in this paper. In addition, , the actual output of this method is relatively small, and the particle size of the synthesized quantum dots is relatively large

Method used

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  • Method for efficiently synthesizing CuInSe2 quantum dots with chalcopyrite structures
  • Method for efficiently synthesizing CuInSe2 quantum dots with chalcopyrite structures
  • Method for efficiently synthesizing CuInSe2 quantum dots with chalcopyrite structures

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Embodiment 1

[0052] An Efficient Synthesis of CuInSe with Chalcopyrite Structure 2 A method for quantum dots comprising the steps of:

[0053] 1) Weigh 1mmol of CuCl and 1mmol of InCl 3 4H 2 O was placed in a 50mL three-necked flask with a stirrer, 6mL oleylamine (OLA) and 10mL octadecene (ODE) were added, stirred and heated to 110°C, and the three-necked flask was evacuated for 30min (one-time vacuuming), and then introduced Argon, repeat the steps of vacuuming and argon a total of three times, continue to stir and heat to 155 ° C, stir for 10 min until the solid particles are completely dissolved, and obtain a dark red metal precursor solution (containing Cu + 、In 3+ cationic precursor solution), then lower the temperature of the precursor solution to 110°C, vacuumize for 15 minutes (secondary vacuum pumping), then pass argon, repeat the steps of vacuum pumping and argon for a total of three times;

[0054] 2) Weigh 2 mmol of Se powder into a 15 mL sample bottle, add 4 mL of oleylami...

Embodiment 2

[0060] An Efficient Synthesis of CuInSe with Chalcopyrite Structure 2 The method for quantum dots, its preparation method is roughly the same as Example 1, the difference is: the add-on of oleylamine (OLA) in step 1) is 5mL, the add-on of octadecene (ODE) is 10mL; Step 2) in oil The amounts of amine and cetyl mercaptan added were 3.8mL and 1.2ml respectively; in step 3), the temperature of the obtained reaction solution was raised twice, and the temperature was raised to 230° C., and then kept for 1 h.

[0061] CuInSe obtained in this embodiment 2 The quantum dot powder was analyzed by X-ray diffraction, the results are shown in Figure 5 , the obtained product has a chalcopyrite structure, and the TEM spectrum shows that the obtained CuInSe 2 Quantum dots are triangular, square and spherical in shape, with few defects and good monodispersity, with an average size of 7nm (see Figure 6 ), EDS results show that the resulting CuInSe 2 The stoichiometric ratio of quantum dots...

Embodiment 3

[0064] An Efficient Synthesis of CuInSe with Chalcopyrite Structure 2 The method for quantum dots, its preparation method is roughly the same as Example 1, the difference is: the add-on of oleylamine (OLA) in step 1) is 4mL, and the add-on of octadecene (ODE) is 10mL; Step 2) in oil The amounts of amine and cetyl mercaptan added were 3.5mL and 1.5ml respectively; in step 3), the temperature of the obtained reaction solution was raised twice, and the temperature was raised to 210°C, and then kept for reaction for 1h.

[0065] CuInSe obtained in this embodiment 2 The quantum dot powder was analyzed by X-ray diffraction, the results are shown in Figure 9 , the figure shows that the resulting CuInSe 2 Quantum dots have a chalcopyrite structure. The TEM spectrum shows that the obtained CuInSe 2 The quantum dots are triangular in shape, have few defects and have good monodispersity, and the average grain size is 4.2nm (see Figure 10 ).

[0066] CuInSe obtained in this embodi...

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Abstract

The invention discloses a method for efficiently synthesizing CuInSe2 quantum dot with a chalcopyrite structure. By using a method for dissolving selenium powder by using a mixed solvent of oleylamine and hexadecyl mercaptan instead of oleylamine single solvent, a difficulty problem that high temperature is needed during dissolving the selenium powder by using oleylamine is solved. By using cheap indium trichloride tetrahydrate as an indium source instead of expensive anhydrous indium trichloride or indium acetate and using octadecene as metallic precursor instead of partial oleylamine, the CuInSe2 quantum dot with the chalcopyrite structure is successfully synthesized. Compared with the traditional hot injection method, the method for efficiently synthesizing the CuInSe2 quantum dots with the chalcopyrite structures, disclosed by the invention, has the advantages of low raw material cost, simple operation, easy control, high repeatability and no pollution to environment. The synthesized CuInSe2 quantum dot has the advantages of less defects, high yield, uniform particle size distribution, good dispersion and important industrial application values and can be used for preparing CuInSe2 quantum dot solar cells.

Description

technical field [0001] The invention belongs to the technical field of solar photovoltaic material preparation, in particular to the efficient synthesis of CuInSe with a chalcopyrite structure 2 method of quantum dots. Background technique [0002] Semiconductor quantum dots are quasi-zero-dimensional nanomaterials, generally composed of a small number of atoms, also known as "artificial atoms". Because the size of the three dimensions of quantum dots is generally between 1 and 100 nm, the movement of electrons in them is limited in all directions, and thus exhibits many unique properties, such as quantum confinement effects, surface effects, and quantum size effects. And the multi-exciton effect, etc., so that it has broad application prospects in the fields of new luminescent materials, photocatalytic materials and photovoltaic power generation materials. [0003] CuInSe 2 The excitonic Bohr radius of the material is 10.6nm, and nanocrystals smaller than this size are c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88B82Y40/00
CPCB82Y40/00C09K11/88
Inventor 夏冬林杲皓冉李云峰赵修建
Owner WUHAN UNIV OF TECH
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