Method for preparing magic number cluster nanocrystal in indirect mode of ion exchange

A technology of ion exchange and nanocrystals, which is applied in the preparation of cadmium compounds, lead compounds, nanotechnology, etc., can solve the problems of low yield and purity of semiconductor nanocrystal products, achieve improved atom utilization, simple operation, good stability effect

Active Publication Date: 2019-12-27
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existence of these intermediate species consumes a large amount of raw materials,

Method used

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  • Method for preparing magic number cluster nanocrystal in indirect mode of ion exchange
  • Method for preparing magic number cluster nanocrystal in indirect mode of ion exchange
  • Method for preparing magic number cluster nanocrystal in indirect mode of ion exchange

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1 Synthesis of cadmium selenide (CdSe) magic number cluster nanocrystals

[0050] Raw materials: cadmium oxide (CdO), oleic acid (OA), zinc oxide (ZnO), selenium powder (Se), trioctylphosphine (TOP), octadecene (ODE), octylamine (OTA) are all from Aldrich; Cyclohexane (CH) was from Tianjin Zhiyuan Reagent Co., Ltd.

[0051] Testing instrument: TECHCOMP UV 2310Ⅱ ultraviolet spectrophotometer is Shanghai Tianmei Technology Instrument.

[0052] (1) Referring to the aforementioned documents, according to the method and requirements for preparing ZnSe conventional nanocrystals (ZnSe RNCs):

[0053] (i) Weigh 0.4883g ZnO, 3.729g OA (oleic acid) and 5g ODE into a three-necked round-bottomed flask, switch between vacuum and nitrogen at 40°C for more than three times, wait until the bubbles disappear and slowly raise the temperature to 120°C, and keep vacuum heating 1h, change to N 2 The atmosphere was heated up to 290°C for 2 hours (the solution was clear and transpa...

Embodiment 2

[0059] Example 2 Synthesis of lead selenide (PbSe) magic number cluster nanocrystals

[0060] Raw materials: lead oxide (PbO), oleic acid (OA), zinc oxide (ZnO), selenium powder (Se), trioctylphosphine (TOP), octadecene (ODE) are all from Aldrich; cyclohexane (CH) From Tianjin Zhiyuan Reagent Co., Ltd.

[0061] Testing instrument: TECHCOMP UV 2310Ⅱ ultraviolet spectrophotometer is Shanghai Tianmei Technology Instrument.

[0062] Preparation:

[0063] (1) Synthesize ZnSe according to the same method as in Example 1;

[0064] (2) Test the dispersion of 15 μL of sample into 3 mL of dispersant (2 mL of cyclohexane-1 mL of octylamine mixed solvent) with a UV-visible spectrophotometer. It can be seen that in the octylamine-cyclohexane mixed solution, the sample immediately has the 299nm characteristic absorption peak of the ZnSe magic number nanocluster to appear, as figure 1 As shown, it can be judged that the ZnSe magic number cluster nanocrystal intermediate was obtained unde...

Embodiment 3

[0067] Example 3 Synthesis of cadmium sulfide (CdS) magic number cluster nanocrystals

[0068] Raw materials: cadmium oxide (CdO), oleic acid (OA), zinc oxide (ZnO), sulfur powder (S), octadecene (ODE) are all from Aldrich; cyclohexane (CH) is from Tianjin Zhiyuan Reagent Co., Ltd.

[0069] Testing instrument: TECHCOMP UV 2310Ⅱ ultraviolet spectrophotometer is Shanghai Tianmei Technology Instrument.

[0070] Preparation:

[0071] (1) According to the method and requirements of preparing ZnS conventional nanocrystals (RNCs), the Zn precursor (Zn(OA) 2 ), and the Cd precursor (Cd(OA) 2 ) stock solution raw material B.

[0072] Take 2.2mL of Zn(OA) of raw material A 2 and 3.158g of ODE were placed in a 50mL three-necked round bottom flask, and the vacuum-nitrogen gas was switched at 40°C for more than three times. After the bubbles disappeared, the temperature was raised to 80°C, and the vacuum was kept for 30min, and then switched to N 2 Warm up to 120°C under atmosphere, c...

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Abstract

The invention discloses a method for preparing a magic number cluster nanocrystal in an indirect mode of ion exchange. The method comprises the following steps: respectively employing a conventional induction period intermediate before conventional nanocrystalline nucleation, which is formed by a compound containing IIB group, IIIA group or IVA group metal elements in a periodic table of elementsand non-metal elements containing VIA group or VA group as raw materials, as a raw material A; employing a compound of another metal element different from the metal element contained in the raw material A in the IIB group, the IIIA group or the IVA group in the periodic table of elements is mixed with an organic ligand to react to obtain a product, which is used as a raw material B; carrying outcation exchange reaction at room temperature, and then growing the cluster nanocrystal in a dispersing agent, so as to obtain a magic number cluster nanocrystalline product in a new composition form after the metal elements in the raw material A are replaced by the metal elements in the raw material B. The method is simple to operate, the magic cluster nanocrystalline product with narrow size distribution can be obtained at room temperature, and the conversion yield and stability of the method are far superior to those of a traditional direct synthesis mode.

Description

technical field [0001] The invention relates to a method for preparing magic number cluster nanocrystals, specifically a method for preparing magic number cluster nanocrystals in an indirect manner of ion exchange. Background technique [0002] Conventional semiconductor nanocrystals (also known as quantum dots) are zero-dimensional nanomaterials composed of a finite number of atoms. It has excellent physical and chemical properties, such as size effect, quantum confinement effect, etc., and has shown good application prospects in the fields of photoelectrocatalysis, displays, and solar cells, so it has attracted extensive attention. In recent years, researchers have discovered semiconductor magic number cluster nanocrystals with a single size in the process of conventional quantum dot synthesis. The magic number cluster nanocrystal has a specific number of atoms and a stable internal structure, with a diameter of about 1-2nm and uniform size. They only show sharp absorpti...

Claims

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Application Information

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IPC IPC(8): C01B19/04C01G11/02C01G21/21B82Y40/00
CPCC01B19/007C01B19/001C01G11/02C01G21/21C01G21/003C01G11/003B82Y40/00C01P2002/84C01P2004/50
Inventor 梁斌陈檬刘尚谱张猛余睽
Owner SICHUAN UNIV
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