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Water heat synthesis preparation method of wurtzite phase nano-nitride and its solid solution

A technology for hydrothermal synthesis and nitride, which is applied in nitrogen compounds, chemical instruments and methods, nitrogen-metal/silicon/boron binary compounds, etc., can solve the problems of explosive dangerous azide, poor stability and high reaction temperature, Achieve the effect of reducing reaction temperature, low cost and uniform particle shape

Inactive Publication Date: 2004-07-21
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the invention is to propose a hydrothermal synthesis preparation method for preparing wurtzite phase nano-nitrides and their solid solutions in a hydrothermal system at a lower temperature and lower pressure, to overcome the existing methods or the relatively low reaction temperature. High, using highly toxic metal-organic compound precursors or organic solvents, or using azides with poor stability and explosion hazards

Method used

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  • Water heat synthesis preparation method of wurtzite phase nano-nitride and its solid solution
  • Water heat synthesis preparation method of wurtzite phase nano-nitride and its solid solution
  • Water heat synthesis preparation method of wurtzite phase nano-nitride and its solid solution

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Embodiment 1

[0030] Add 5 mmol of indium sulfide (In 2 S 3 ), 60mmol of ammonium chloride (NH 4 Cl), 15mmol of carbon disulfide (CS 2 ) and 7.5mmol of elemental iodine (I 2 ), then add 40mL of water and keep the temperature at 250°C for 24 hours; the obtained product is washed twice with dilute hydrochloric acid and then washed twice with water, and dried in a vacuum oven at 60°C for 3 hours to obtain the product InN powder.

Embodiment 2

[0032] Add 5 mmol of gallium sulfide (Ga 2 S 3 ), 60mmol of ammonium chloride (NH 4 Cl), 15mmol of carbon disulfide (CS 2 ) and 7.5mmol of elemental iodine (I 2 ), then add 40mL of water and keep the temperature at 250°C for 48 hours; the obtained product is washed twice with dilute hydrochloric acid and then washed twice with water, and placed in a vacuum drying oven to dry at 60°C for 3 hours, and the obtained crude product is calcined at 400°C under nitrogen protection for 8 Hours, the product GaN powder is obtained.

Embodiment 3

[0034] Add 5 mmol of aluminum sulfide (Al 2 S 3 ), 60mmol of ammonium chloride (NH 4 Cl), 15mmol of carbon disulfide (CS 2 ) and 7.5mmol of elemental iodine (I 2 ), then add 40mL of water and keep the temperature at 280°C for 48 hours; the obtained product is washed twice with dilute hydrochloric acid and then washed twice with water, and dried in a vacuum oven at 60°C for 3 hours to obtain the product AlN powder.

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Abstract

A process for hydrothermally preparing the wurtzite-phase nano-class InN, GaN, AIN and its sosoloid as luminescent semiconductor material includes such steps as proportionally adding M2S3, NH4CL, CS2, I2 and water into high-pressure reactor, reaction at 250-280 deg.C for 24-48 hr, filtering to obtain coarse product, washing with diluted hydrochloric acid and water, and drying. Its advantage is high safety.

Description

technical field [0001] The invention belongs to the technical field of hydrothermal synthesis preparation methods, and in particular relates to a preparation method of wurtzite phase nano-indium nitride InN, gallium nitride GaN, aluminum nitride AlN and solid solution semiconductor luminescent materials. Background technique [0002] Wurtzite phase nano-indium nitride InN, gallium nitride GaN, aluminum nitride AlN and their solid solutions have a wide range of applications in light-emitting diodes, optical filters, superionic materials and semiconductor materials. It is a problem faced by the semiconductor industry to realize the preparation method with simple process, clean environment, and the semiconductor bandwidth of the product can cover the blue light and ultraviolet regions. Taking gallium nitride GaN as an example, the American "Inorganic Chemistry" (Inorganic Chemistry, 1993, Vol. 32, pp. 2745-2752 and 1994, Vol. 33, pp. 5693-5700) reported...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/00C01B21/06C01B21/072
Inventor 谢毅熊宇杰
Owner UNIV OF SCI & TECH OF CHINA