Preparation method for metal-free perovskite quantum dots DABCO-NH4X3 (X=Cl, Br, I)

A perovskite and quantum dot technology, applied in chemical instruments and methods, luminescent materials, etc., to achieve the effects of low cost, simple operation and short reaction time

Active Publication Date: 2019-07-19
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] As far as the applicant knows, the current metal-free perovskite quantum dot DABCO-NH 4 x 3 The preparation method of (X=Cl, Br, I) has not been reported yet, is a kind of brand-new synthetic method

Method used

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  • Preparation method for metal-free perovskite quantum dots DABCO-NH4X3 (X=Cl, Br, I)
  • Preparation method for metal-free perovskite quantum dots DABCO-NH4X3 (X=Cl, Br, I)
  • Preparation method for metal-free perovskite quantum dots DABCO-NH4X3 (X=Cl, Br, I)

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Embodiment 1

[0019] Add 20mL N-N dimethylformamide and 5mL hydrochloric acid to a 100mL single-necked flask, weigh 10mmol ammonium chloride solid, stir to dissolve it completely, then add 2mL oleic acid and 1mL n-octylamine to it, stir for 30 minutes, and finally Weigh 10mmol of DABCO solid and dissolve it in N-N dimethylformamide, then add it dropwise to the precursor solution, continue to stir for 30 minutes, add 40mL of ethyl acetate to it, a white precipitate will be produced rapidly, and the solution will be centrifuged at 12000r / min at high speed Wash and centrifuge in the machine for 3 times, and dry the solid after washing and centrifuging in vacuum at 40°C for 6 hours to obtain DABCO-NH 4 Cl 3 finished product. figure 1 It can be seen from the XRD pattern that all its diffraction peaks correspond to the standard card, further confirming that DABCO-NH was successfully prepared 4 Cl 3 finished product. and figure 2 DABCO-NH 4 Cl 3 TEM image of perovskite, DABCO-NH can be cle...

Embodiment 2

[0021] Add 20mL N-N dimethylformamide and 5mL hydrobromic acid to a 100mL single-necked flask, weigh 10mmol ammonium bromide solid, stir to dissolve it completely, then add 2mL oleic acid and 1mL n-octylamine to it, and stir for 30 minutes , and finally weighed 10mmol of DABCO solid and dissolved it in N-N dimethylformamide and added it dropwise to the precursor solution. Stirring was continued for 30 minutes, and 40mL of ethyl acetate was added to it to rapidly produce white precipitate. Wash and centrifuge 3 times in a high-speed centrifuge, and dry the solid after washing and centrifuging in vacuum at 40°C for 6 hours to obtain DABCO-NH 4 Br 3 finished product. figure 1 It can be seen from the XRD pattern that all the diffraction peaks correspond to the standard card.

Embodiment 3

[0023] Add 20 mL of N-N dimethylformamide and 5 mL of hydroiodic acid to a 100 mL single-necked flask, and then add 2 mL of phosphoric acid to prevent I - Oxidation, weigh 10mmol ammonium chloride solid, stir to dissolve it completely, then add 2mL oleic acid and 1 mL n-octylamine to it, stir for 30 minutes, finally weigh 10mmol DABCO solid and dissolve it in N-N dimethylformamide Then add it dropwise to the precursor solution, continue to stir for 30 minutes, add 40mL ethyl acetate to it, quickly produce white precipitate, wash and centrifuge the solution 3 times in a 12000r / min high-speed centrifuge, and centrifuge the solid at 40 After vacuum drying at ℃ for 6 hours, DABCO-NH 4 I 3 finished product. figure 1 It can be seen from the XRD pattern that all the diffraction peaks correspond to the standard card.

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Abstract

The invention relates to a preparation method for metal-free perovskite quantum dots DABCO-NH4X3 (X=Cl, Br, I). The preparation method comprises the following steps: (1) dissolving NH4X (X=Cl, Br, I)solids in a mixed solution of N-N dimethylformamide and HX acid, then adding a certain amount of oleic acid and n-octylamine in the mixed solution; (2) adding DABCO (diazabicyclooctane) solids to theprecursor solution, fully reacting, adding ethyl acetate and rapidly producing white solids; and (3) washing and performing centrifugation with cyclohexane, and carrying out vacuum drying to obtain afinished product. According to the invention, long-chain oleic acid and n-octylamine are utilized to control the reaction process of NH4X and DABCO at room temperature effectively, finally the metal-free perovskite quantum dots DABCO-NH4X3 are prepared. The method has the advantages of short reaction time, simple operation, low cost and the like, and is a novel preparation method for the DABCO-NH4X3 quantum dots.

Description

technical field [0001] The invention relates to the field of optoelectronic materials, in particular to metal-free perovskite quantum dots DABCO-NH 4 x 3 (X=Cl, Br, I) preparation method. Background technique [0002] Human production and life require energy, but the energy depletion and environmental problems caused by burning coal, natural gas and other fossil energy are becoming more and more serious. The development and utilization of new green energy has become a major issue of sustainable development strategy. Among the various existing new energy technologies, photoelectric conversion is undoubtedly one of the most promising directions. [0003] Metal-free perovskite, since there is no need to introduce metal elements, metal-free perovskite can effectively avoid the toxicity and high cost of some heavy metals, so as to meet the requirements for energy saving, economical and environmental protection of materials. More importantly, the all-organic composition can bri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/61
CPCC09K11/06C09K11/615
Inventor 刘文超冯贤斌宋挺辉方庭森居红梅朱凡凡
Owner NANJING UNIV OF TECH
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