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A preparation method of inorganic halogen perovskite fluorescent quantum dots through one-step synthesis and a product thereof

A technology of fluorescent quantum dots and perovskite, applied in chemical instruments and methods, nano optics, luminescent materials, etc., can solve the problems of increased cost of preparation requirements, reduced product quality and monodispersity, and reduced material synthesis efficiency, etc., to achieve The preparation method is simple and feasible, the reaction conditions are not harsh, and the effect of simple and convenient operation

Inactive Publication Date: 2018-11-09
广东两山科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because of its harsh preparation requirements, it increases the cost and reduces the efficiency of material synthesis; in addition, there are also problems in the large-scale preparation of the hot injection method, which will reduce the quality and monodispersity of the product

Method used

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  • A preparation method of inorganic halogen perovskite fluorescent quantum dots through one-step synthesis and a product thereof
  • A preparation method of inorganic halogen perovskite fluorescent quantum dots through one-step synthesis and a product thereof
  • A preparation method of inorganic halogen perovskite fluorescent quantum dots through one-step synthesis and a product thereof

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Experimental program
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Effect test

Embodiment 1

[0026] Weigh 0.0605g of PbCl 2 , 0.030g CsCO 3 (molar ratio 2:1), added to 5mL of ODE, and added 2mL oleic acid and 1mL oleylamine (volume ratio 5:2:1), heated and stirred at 170°C for 20min, cooled in an ice-water bath after the reaction After reaching room temperature, the solution obtained by the reaction was centrifuged, the supernatant was removed, centrifuged three times with n-hexane, and dried to obtain a solid powder. Such as figure 1 As shown, the inorganic halogen perovskite fluorescent quantum dots prepared in this embodiment have a maximum emission wavelength of 455 nm, a crystal structure of perovskite structure, and a fluorescence quantum yield of 40%.

Embodiment 2

[0028] Weigh 0.68g PbBr 2 , 0.30g CsCO 3 (molar ratio 2:1), add to 50mL ODE, and add 20mL oleic acid and 10mL oleylamine (volume ratio 5:2:1), heat and stir at 120°C for 20min, cool in an ice-water bath after the reaction to room temperature; then the solution obtained by the reaction was centrifuged, the supernatant was removed, centrifuged 3 times with n-hexane, and dried to obtain a solid powder, about 11g, such as figure 2 As shown, wherein a is weighing under natural light, b is weighing under ultraviolet irradiation, and it can be seen that the products all emit fluorescence. All operations are carried out under normal pressure without protective gas. Such as image 3 As shown in (a), under the excitation of a blue LED, the inorganic halogen perovskite fluorescent quantum dots prepared in this example can emit bright green light (b) without blue light leakage. Figure 4 Spectrum of the inorganic halogen perovskite fluorescent quantum dots prepared for this example u...

Embodiment 3

[0030] Weigh 0.085g PbI 2 , 0.030g CsCO 3 (molar ratio 2:1), added to 5mL of ODE, and added 2mL oleic acid and 1mL oleylamine (volume ratio 5:2:1), heated and stirred under vacuum at 120°C for 20min, after the reaction was completed, placed in an ice-water bath Cool to room temperature; centrifuge the solution obtained from the reaction, remove the supernatant, centrifuge 3 times with n-hexane, and dry to obtain a solid powder. Such as Image 6 It is shown that the inorganic halogen perovskite fluorescent quantum dots prepared in this example have a maximum emission wavelength of 595nm, as shown in Figure 7 Its fluorescence lifetime is shown as 5.7 ns and its size is about 20 nm.

[0031] Verified by experiments, PbX 2 with CsCO 3 The molar ratio of 2-4:1 all can realize reaction, and wherein X is selected from Cl, Br, I, PbX 2 The volume ratio of the amount of substance to octadecene is calculated as 1mol:25-27L; the volume ratio of octadecene, oleic acid and oleylamin...

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Abstract

The invention relates to a preparation method of inorganic halogen perovskite fluorescent quantum dots through one-step synthesis. CsCO3, PbX2, octadecene, oleic acid and oleylamine are mixed, and directly heated and reacted under stirring to obtain the inorganic halogen perovskite fluorescent quantum dots CsPbX3, wherein the X is one of Cl, Br and I. The method is simple and convenient to operate, reaction conditions are not rigorous, and one-step synthesis of the three types of perovskite quantum dots can be achieved in air, nitrogen and vacuum conditions. Through comparison with fluorescence and absorption strength of standard fluorescence substances, the perovskite fluorescent quantum dots have the fluorescence quantum efficiency as high as 90%, and good stability. A container having avolume of 500 mL is utilized for reaction, and 10 grams or above of the quantum dots can be prepared in one time. The method is simple, feasible, and simple in reaction condition, and can be furtherscaled up, and the quantum dots can be prepared in a large scale in one time.

Description

technical field [0001] The invention belongs to the field of semiconductor quantum dot luminescent materials, and relates to a preparation method and products thereof for one-step synthesis of inorganic halogen perovskite fluorescent quantum dots. Background technique [0002] Perovskite semiconductors, especially perovskite organic lead halides (CH 3 NH 3 wxya 3 , X=F, Cl, Br, I) has potential application value in solar cells, lasers, photodetectors, light-emitting diodes and other fields because of its low cost, high efficiency and adjustable band gap. In the field of solar cells, the photoelectric conversion efficiency of solar cells based on this material has exceeded 20% in only three years. However, the extreme sensitivity of perovskite organolead halides to air and moisture limits their applications in optoelectronics. CH 3 NH 3 + Extremely unstable in the air state, organolead perovskites degrade rapidly. Protesescu et al. used the hot injection method to dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/66B82Y20/00B82Y30/00B82Y40/00
CPCB82Y20/00B82Y30/00B82Y40/00C09K11/06C09K11/664
Inventor 王富
Owner 广东两山科技有限公司
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