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Water heat systhesis method for preparing phosphide nanometre wire

A technology of hydrothermal synthesis and nanowires, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of uneven product particle size, high cost of raw materials and equipment, etc., and achieve the effect of uniform particle size

Inactive Publication Date: 2004-03-17
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to propose a method for the preparation of hydrothermal synthesis of phosphide nanowires at a lower temperature and lower pressure in a hydrothermal system, to overcome the existing method or the use of highly toxic metal organic compound precursors , or the cost of raw materials and equipment is expensive, or defects such as uneven product particle size

Method used

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  • Water heat systhesis method for preparing phosphide nanometre wire
  • Water heat systhesis method for preparing phosphide nanometre wire
  • Water heat systhesis method for preparing phosphide nanometre wire

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a Teflon-lined autoclave, add 12 mmol NaOH and 1.5 mmol Ga 2 o 3 or In 2 o 3 , then add 30mL of water; after the solid is completely dissolved, add 3mmol cetyltrimethylammonium bromide (C 16 h 33 (CH 3 ) 3 NBr), 3mL n-hexanol, 10mL heptane; after stirring for 20 minutes, add 1g white phosphorus, 0.75g elemental iodine (I 2 ), sealed the autoclave, and kept the temperature at 160°C for 24 hours; the resulting product was washed twice with benzene, alcohol, dilute hydrochloric acid (1mol / L), and water successively, placed in a vacuum drying oven, and dried at 60°C for 4 hours. That is the product powder.

[0020] Adopt target X-ray powder diffraction (XRD), field emission scanning electron microscope (FE-SEM), high resolution transmission electron microscope (HRTEM), electron diffraction (ED) and photoluminescence spectrum (PL) to obtain in the above-mentioned embodiment The product is characterized.

[0021] figure 1 The given product powder XRD patterns A a...

Embodiment 2

[0026] In a Teflon-lined autoclave, add 12 mmol NaOH and 1.5 mmol In 2 o 3 , then add 30mL of water; after the solid is completely dissolved, add 6mmol cetyltrimethylammonium bromide (C 16 h 33 (CH 3 ) 3 NBr), 3mL n-hexanol, 10mL heptane; after stirring for 20 minutes, add 0.5g white phosphorus, 0.37g elemental iodine (I 2), sealed the autoclave, and kept the temperature at 160°C for 24 hours; the resulting product was washed twice with benzene, ethanol, dilute hydrochloric acid (1mol / L), and water successively, placed in a vacuum drying oven, and dried at 60°C for 4 hours. That is the product powder.

[0027] The products obtained in the above examples were characterized by using target X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and photoluminescence spectroscopy (PL).

[0028] Product powder XRD patterns and figure 1 B is consistent, indicating that the product is InP of sphalerite phase;

[0029] TEM photo Figure 4 A shows that the InP ...

Embodiment 3

[0032] In a Teflon-lined autoclave, add 12 mmol NaOH and 1.5 mmol In 2 o 3 , then add 30mL of water; after the solid is completely dissolved, add 3mmol cetyltrimethylammonium bromide (C 16 h 33 (CH 3 ) 3 NBr), 3mL n-hexanol, 10mL heptane; after stirring for 20 minutes, add 1g white phosphorus, 0.75g elemental iodine (I 2 ), sealed the autoclave, and kept the temperature at 160°C for 48 hours; the resulting product was washed twice with benzene, alcohol, dilute hydrochloric acid (1mol / L), and water successively, placed in a vacuum drying oven, and dried at 60°C for 4 hours. That is the product powder.

[0033] The products obtained in the above examples were characterized by using target X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and photoluminescence spectroscopy (PL).

[0034] Product powder XRD pattern and figure 1 B is consistent, indicating that the product is InP of sphalerite phase;

[0035] FE-SEM photo Figure 4 B show...

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Abstract

The present invention relates to metal luminescent phosphide material. The hydrothermal process of preparing nano phosphide line includes: adding gallium phosphide or indium phosphide and sodium hydroxide in the molar ratio of 1 to 8 into high pressure reactor and adding water to reach sodium hydroxide concentration of 0.4 mol / L; adding cetyl trimethyl ammonium bride of 2-4 molar times the metalphosphide and n-hexanol and heptane in the amount of 0.1 time and 1 / 3 time the volume of water separately via stirring; adding white phosphorus in 5 molar times the phosphide and elementary iodine in2 molar times; reaction in closed condition at 160-200 deg.c for 24-48 hr; filtering to obtain coarse product; washing wo benzene, ethanol, dilute hydrochloric acid solution and water successively and drying to obtain the product.

Description

1. Technical field: [0001] The invention belongs to the technical field of hydrothermal synthesis preparation methods, in particular to a preparation method of metal phosphide luminescent materials. 2. Background technology: [0002] Nano-gallium phosphide and indium phosphide are widely used in light-emitting diodes, optical filters, superionic materials and semiconductor materials. Their nanowires have potential applications as the smallest unit of electron transport. "Chemical Physical Letters" (Chemistry Physical Letters, vol. 367, pp. 717-722, 2003) reported that gallium phosphide nanowires were synthesized by vapor phase deposition, and the obtained product was impure. The American Journal of Physical Chemistry B (Journal of Physical Chemistry B, 2001, Volume 105, pages 4062-4064) reported laser catalytic growth of indium phosphide nanowires, but this method requires complex synthesis equipment and is very expensive and difficult to achieve Mass production. British ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/70
Inventor 谢毅熊宇杰李正全
Owner UNIV OF SCI & TECH OF CHINA
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