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Preparation methods of nano-material and nano-material modified glassy carbon electrode

A nanomaterial and glassy carbon electrode technology, which is applied in the field of nanomaterials, can solve the problem that the electrochemiluminescence properties of inorganic perovskite quantum dot materials are rarely studied.

Inactive Publication Date: 2019-12-03
CHINA UNIV OF GEOSCIENCES (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The electrochemiluminescence of Si, CdTe, CdSe nanocrystals and nanoclusters has been reported many times, but the electrochemiluminescence properties of inorganic perovskite quantum dot materials are rarely studied

Method used

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  • Preparation methods of nano-material and nano-material modified glassy carbon electrode
  • Preparation methods of nano-material and nano-material modified glassy carbon electrode
  • Preparation methods of nano-material and nano-material modified glassy carbon electrode

Examples

Experimental program
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Embodiment 1

[0040]Example 1. Microwave Synthesis of Inorganic Perovskite Quantum Dots

[0041] Weigh 0.3mmol PbX 2 (X is one or more in Cl, Br or I) and 0.1mmol CsCO 3 Mix well with 1.5mL oleic acid, 1.5mL oleylamine and 10mL 1-octadecene in a beaker. Put the mixture into a microwave oven and heat it with a certain power for a certain period of time (such as figure 1 ). The obtained product was cooled to room temperature (eg, 15°C-40°C), centrifuged at 9000rpm for 10min to remove the supernatant, and washed several times with cyclohexane and ethanol. The final product was dissolved in 4 mL of cyclohexane for later use.

[0042] The growth rate of inorganic perovskite quantum dots depends on the process of raw material dissolution to form precursors, which means that the power and time of microwave heating determine the size and shape of inorganic perovskite quantum dots, thereby affecting their optical properties. Therefore, the present invention optimizes the power and time of micro...

Embodiment 2

[0043] Embodiment 2. Characterization of basic properties of inorganic perovskite quantum dots

[0044] Under optimized conditions, 12 kinds of inorganic perovskite quantum dots (CsPbCl 3 ,CsPbCl 2 Br,CsPbCl 1.5 Br 1.5 ,CsPbClBr 2 ,CsPbCl 0.5 Br 2.5 ,CsPbBr 3 ,CsPbBr 2 I,CsPbBr 1.8 I 1.2 ,CsPbBr 1.5 I 1.5 ,CsPbBr 1.2 I 1.8 ,CsPbBrI 2 and CsPbI 3 ), enabling high-throughput synthesis. The basic properties of these 12 inorganic perovskite quantum dots with different compositions were characterized. Specifically, such as Figure 6 The TEM photos in the above show that the 12 kinds of quantum dots obtained by microwave synthesis are all monodisperse square or rectangular, and the size is relatively uniform. Select one of the CsPbBr 3 Quantum dots were structurally characterized, and the XRD patterns showed that they belonged to the monoclinic crystal system (PDF#18-0364), which was different from the tetragonal phase products synthesized by thermal injection (su...

Embodiment 3

[0045] Example 3. Characterization of Electrochemiluminescence Properties of Inorganic Perovskite Quantum Dots

[0046] A glassy carbon electrode modified with inorganic perovskite quantum dots was prepared first. With 0.3μm α-Al 2 o 3 The powdered glassy carbon electrode (GCE) was polished to a mirror surface, and then the electrode surface was rinsed with deionized water and dried with nitrogen gas. Take 10 μL of microwave-synthesized CsPbBr 3 The quantum dot solution was dropped on the surface of the glassy carbon electrode and dried naturally to obtain CsPbBr 3 Quantum dot modified glassy carbon electrode (CsPbBr 3 QDs|GCE).

[0047] Using the prepared CsPbBr 3 The QDs|GCE electrodes were used to characterize the electrochemical properties of the inorganic perovskite quantum dots obtained by the above microwave synthesis. Such as Figure 12 , in the cathodic cyclic voltammetry curve, CsPbBr 3 The QDs|GCE electrode has an obvious current signal at -1.34V, indicatin...

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Abstract

The embodiment of the specification provides a preparation method of a nano-material. The nano-material is a CsPbX3-type inorganic perovskite quantum dot material, wherein X is one or more of Cl, Br or I. The preparation method comprises the following steps that firstly, 0.3 mmol of PbX2, 0.1 mmol of CsCO3, 1.5 mL of oleic acid, 1.5 mL of oleylamine and 10 mL of 1-octadecene are weighed and put into a container to be evenly mixed as reaction raw materials; then, the container is put into a microwave oven, and heating is conducted for the preset heating duration at the preset heating power so as to enable the reaction raw materials to react to obtain a reaction product, wherein the nano-material is included; then the reaction product is cooled to the preset temperature, centrifuging is conducted for the preset heating duration at the preset centrifuging rotating speed so as to separate the nano-material; and then supernatant is removed, and the separated nano-material is cleaned throughcyclohexane and ethyl alcohol. In this way, various different inorganic perovskite quantum dots can be synthesized easily and rapidly in a high-flux mode. The obtained inorganic perovskite quantum dots can be applied to an electrochemical luminescence sensor.

Description

technical field [0001] One or more embodiments of this specification relate to the field of nanomaterials, in particular to a method for preparing an inorganic perovskite quantum dot material and a method for applying it to an electrochemiluminescent sensor. Background technique [0002] Semiconductor nanocrystals, also known as quantum dots, have been widely studied as a potential optoelectronic material. This kind of quantum dot materials has excellent properties such as size effect, easy surface modification and free colloidal state, so that they show better optical properties than macroscopic substances with the same composition. They can be dispersed in a variety of solvents and different matrices, so they can be used to make a variety of optoelectronic devices. [0003] At present, the most mature optoelectronic nanocrystalline materials are bivalent and multivalent metal oxide nanocrystals, while metal halide nanomaterials are relatively less studied. Inorganic pero...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B9/00C09K11/66G01N21/64G01N21/76G01N27/30G01N27/327G01N27/48
CPCC01B9/00C01P2002/72C01P2004/04C09K11/665G01N21/6428G01N21/643G01N21/76G01N27/308G01N27/3277G01N27/3278G01N27/48
Inventor 吴静王宇飞
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)