Coordination template for ZnS or ZnSe nanometer crystal preparation and hydrothermal preparation method thereof

A nano-crystal and coordination technology, applied in nano-materials and nano-fields, can solve problems such as toxicity and achieve uniform distribution

Inactive Publication Date: 2009-02-18
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Coordination templates such as ethylenediamine and triethanolamine used in these background technologies have certain toxicity, so selecting new coordination templates is the focus of current research

Method used

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  • Coordination template for ZnS or ZnSe nanometer crystal preparation and hydrothermal preparation method thereof
  • Coordination template for ZnS or ZnSe nanometer crystal preparation and hydrothermal preparation method thereof
  • Coordination template for ZnS or ZnSe nanometer crystal preparation and hydrothermal preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Take 1.2g of zinc chloride, 6.0g of gelatin, and 20mL of water in a round bottom flask, heat to dissolve, stir evenly, heat at a constant temperature of 50°C for 8h, and filter after cooling.

[0024] (2) Add 5.0g Na to the filtrate 2 S 2 o 3 , 10ml of deionized water containing 0.04g NaOH and 6ml of hydrazine hydrate were loaded into a hydrothermal kettle (pH12), filled with water to 60%, sealed, and kept at a temperature of 180° C. for 16 hours. Filter after cooling. Spherical ZnS nanocrystals with a particle diameter of 24-36 nm are obtained. TEM photo see figure 1 .

Embodiment 2

[0026] (1) Take 1.5g of zinc acetate, 2.0g of gelatin, and 15mL of water in a round bottom flask, heat to dissolve, stir evenly, heat at a constant temperature of 80°C for 4h, and filter after cooling. .

[0027] (2) The filtrate is adjusted to a pH value of 11 with aqueous ammonia, and 3.0 g of Na 2 SeO 3 , and 5ml of hydrazine hydrate into a hydrothermal kettle, fill it with water to 80%, seal it, and keep it at a temperature of 160°C for 18 hours. Filter after cooling. Rod-shaped ZnSe nano-crystals with a diameter of 15-25 nm and a length of 40-60 nm are obtained. The average particle size of the rod-shaped ZnSe nano-crystal is 20×50 nm.

[0028] The obtained powder was rinsed with water and absolute ethanol and dried in vacuum, and the photoluminescence spectrum was shown in figure 2 Excited with 327nm ultraviolet light, the luminous peak wavelength is 450nm, which is blue-shifted compared with the bulk ZnSe band gap of 466nm; XRD spectrum see image 3 , found that t...

Embodiment 3

[0030] (1) Take 1.5g of zinc sulfate, 4.0g of glutamic acid chitosan, and 60mL of water, put them in a round bottom flask, heat to dissolve, stir evenly, and heat at a constant temperature of 70°C for 1h.

[0031] (2) After cooling, add 10ml of deionized water containing 0.10gNaOH, 4.0gNaOH 2 SeO 3 and 4.0g vitamin C are packed into a hydrothermal kettle, filled with water to 80%, sealed, and kept at a temperature of 200° C. for 12 hours. Filter after cooling. A mixture of spherical and rod-shaped ZnSe nanocrystals was obtained. TEM photo see Figure 8 .

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Abstract

The invention relates to a complexing template of nano ZnS or ZnSe crystal and a hydrothermal preparation method thereof. Glutin or chitosan salt is taken as the complexing template. The hydrothermal preparation method includes the following steps: heating zinc salt and complexing template agent at mass ratio of 1:1-10 for 1-8hours in water which is at mass ratio of 10-50 to zinc salt under constant temperature of 50-80 DEG C, then filtrating after cooling; adjusting the pH value to 9-12 through sodium hydroxide or ammonia, then adding sodium thiosulfate or sodium selenite at mass ratio of 0.5-5 to zinc salt; after dissolution, adding hydrazine hydrate or vitamin C at mass ratio of 0.5-10 to sodium thiosulfate or sodium selenite, after which clear and uniform solution can be obtained after dissolution; transferring the solution into a hydrothermal kettle and filling 60-90% of the hydrothermal kettle; rising the temperature to 120-240 DEG C and heating for 12-24h, then collecting the deposit and washing, after which nano crystals can be obtained. The invention takes glutin or chitosan salt which is cheap and low in toxicity as the soft template complexing agent for hydrothermal preparation of ZnS or ZnSe. In this way, nano crystals can be obtained, and adjusted to be rods or spheres in shape, with the diameter controllable within30-50nanometers and the length controllable within 20-70nanometers.

Description

technical field [0001] The invention belongs to the field of nanometer materials and nanotechnology, and specifically refers to a coordination template for preparing ZnS or ZnSe nanocrystals and a hydrothermal preparation method. Background technique [0002] II-VI elements can form semiconductors with excellent properties, and the most studied are cadmium chalcogenides such as CdS, CdSe, and CdTe. In recent years, the research on the properties of CdE (E=S, Se, Te) nanocrystals (also known as quantum dots) has shown its great application prospects, and has broad application prospects in immunofluorescence labeling, solar cells, quantum computers, etc. . However, Cd salt itself is highly toxic, and the synthesis process will introduce toxic reagents, so people are also studying its less toxic homologues. ZnSe is a wide bandgap direct transition semiconductor material (~2.67eV), with a wide light transmission range (0.15~22.0μm), high luminous efficiency, and low absorption...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/48C30B7/10
Inventor 陈巍谢闯冯文秀周丽娜王静康
Owner TIANJIN UNIV
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