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New method for preparing indium nitride nano material

A technology of nano-indium nitride and a new method, which is applied in the direction of chemical instruments and methods, nanotechnology, nitrogen compounds, etc., can solve the problems of high reaction temperature, sensitivity, harsh synthesis conditions, etc., and achieve simple and easy control of the reaction process and the source of raw materials Broad, low reaction temperature effect

Inactive Publication Date: 2016-02-24
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Indium nitride prepared by these physical methods has the advantages of high purity and narrow particle size, but the preparation method requires large-scale equipment
The chemical method for preparing indium nitride is thermally decomposing metal organic compounds of indium (Dingman, Angew.Chem.Int.Ed., 2000, 39, 1470), but the organic precursors used in this preparation are used as raw materials, but the metals used The synthesis conditions of organic precursors are extremely harsh, and pyrolysis of amino indium In(NH 2 ) 3 (Purdy, Inorg.Chem., 1994,33,382), but the raw material is poisonous and extremely sensitive to air, metal indium and nitrogen react under microwave plasma conditions (J.S.Dyck, Solid State Commun., 2000,114,355; J.Mater.Res., 1999,14,2411) and high temperature ammoniation method (Zhao, Small,2005,1,1004)
This method is effective and can be scaled up, but the reaction temperature is higher (greater than 500°C), and toxic ammonia gas is used in the reaction process

Method used

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  • New method for preparing indium nitride nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 1 gram of indium trioxide, 1 gram of sublimed sulfur and 4 grams of sodium amide into a 20 ml stainless steel autoclave, seal it and put it into an electric furnace capable of temperature programming, and the furnace temperature rises from room temperature to 190°C, then maintained at 190°C for 30 hours and then naturally cooled to room temperature. The final product in the autoclave consisted of black deposits and residual gas. Collect the black sediment stuck on the inner surface of the kettle wall, wash it with distilled water and absolute ethanol several times, filter the sample obtained, and dry the sample in a vacuum drying oven at 50°C for 4 hours, and finally collect it for characterization .

[0033] The phase analysis of the powder was carried out by using the Japanese RigakuD / max-γA X-ray powder diffraction (XRD) instrument, CuKα Graphite monochromator, tube voltage and current are 40kV and 20mA, scanning speed 10.0° min -1 .

[0034] figure 1 It is...

Embodiment 2

[0040] The difference from Example 1 is that the reaction temperature is 350°C, and the reaction time is 10 hours. 1 gram of indium trioxide, 1 gram of sublimed sulfur and 4 grams of sodium amide are added to a 20 ml stainless steel high-pressure After sealing it, put it into an electric furnace capable of temperature-programming, then maintain it at 350°C for 10 hours, and then cool it down to room temperature naturally. The final product in the autoclave consisted of black deposits and residual gas. The black sediment stuck to the inner surface of the kettle wall was collected and washed several times, and the samples obtained after centrifugation were dried in a vacuum oven at 50°C for 4 hours, and finally collected for characterization.

[0041] To the X-ray diffraction figure ( Figure 5 ), obtain the same result as in Example 1.

Embodiment 3

[0043] The difference from Example 1 is that indium chloride is used as the indium-containing compound, the raw material diindium trioxide used in Example 1 can be replaced by indium chloride, and other conditions remain unchanged. Take 0.7 g of indium chloride, put it into a 20 mL stainless steel autoclave with 0.5 g of sublimed sulfur and 4.0 g of sodium amide, seal it and place it in a resistance furnace, react at 190 °C for 30 hours, and then naturally cool to room temperature. Open the autoclave, wash the obtained product, centrifuge to obtain a solid, and perform an X-ray diffraction pattern on the obtained indium nitride material ( Figure 6 ), SEM ( Figure 7 ), it can be seen from the scanning electron microscope of the product that the indium nitride is a particle of 50-200 nanometers.

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Abstract

The invention relates to a synthesis method of a semiconductor material and an application field of semiconductor material and particularly relates to a new method for preparing an indium nitride nano material. The new method comprises the following steps: adding an indium-containing compound, sulfur and sodium amide into a high-pressure kettle; heating the mixture to 190 DEG C to 400 DEG C, wherein the reaction time is 10 to 40 hours; washing a product, and centrifuging and drying to obtain the indium nitride nano material. In a closed system, the indium-containing compound is converted into the indium nitride nano material under the regulation and control of the sodium amide; compared with the prior art, the reaction temperature is relatively low; raw materials for the reaction are wide in source and cheap in price; a reaction process is simple and easy to control, the obtained product has a nanometer size and the yield is 90 percent or more.

Description

technical field [0001] The invention relates to a method for preparing indium nitride nanomaterials at low temperature, and belongs to the field of synthesis methods of semiconductor materials and their applications. Background technique [0002] Indium nitride is a very important light-emitting material, which is widely used in the preparation of optoelectronic devices such as photodiodes and solar cells. However, due to the relatively poor thermal stability of indium nitride, it will decompose to generate nitrogen and metal indium at a relatively low temperature (about 500 degrees Celsius), so the preparation of indium nitride materials is very difficult. Therefore, people are looking for a method for preparing indium nitride materials with cheap raw materials, simple process and clean environment. [0003] At present, the physical methods for preparing indium nitride are pulse discharge method and vapor phase deposition method. Indium nitride prepared by these physical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06B82Y40/00
CPCC01B21/0632C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2004/22C01P2004/61C01P2004/64
Inventor 王良彪刘维桥周全法
Owner JIANGSU UNIV OF TECH
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