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Method of preparing light-emitting porous silicon from LiAlH4

A technology of porous silicon and mixtures, applied in luminescent materials, chemical instruments and methods, preparation of alkali metal aluminate/alumina/aluminum hydroxide, etc., can solve the problems of slow electrochemical corrosion, difficult disposal of waste liquid, and preparation of High cost and other issues, to achieve the effect of easy large-scale use, no need for corrosion resistance of equipment, and low raw material prices

Active Publication Date: 2017-08-18
凤阳振兴电子材料有限公司
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  • Application Information

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Problems solved by technology

[0002] Most of the existing methods for preparing luminescent porous silicon adopt electrochemical corrosion method, that is, in a polytetrafluoroethylene corrosion tank, insert a silicon wafer and a platinum wafer as the anode and cathode respectively, and use hydrofluoric acid or hydrofluoric acid plus ethanol As an electrolyte, the preparation of luminescent porous silicon is limited by many factors such as the concentration and composition of the solution, current density, resistivity, environmental protection and temperature, and the preparation of luminescent porous silicon is more sensitive to light.
The chemical reaction process of preparing luminescent porous silicon by this method is complicated, and it is not completely clear so far. In the hydrofluoric acid solution, the electrochemical corrosion rate of silicon wafers is extremely slow, and the waste liquid produced is also difficult to handle.
[0003] This method has the following deficiencies: 1. Waste liquid, etc. are generated during the preparation process, which pollutes the environment; 2. A large amount of electric energy is consumed during the preparation process, resulting in high energy consumption; 3. It is difficult to purify the prepared luminescent porous silicon; 4. The production cost is high (the price of raw materials is high), the equipment used must be corrosion-resistant (hydrofluoric acid is extremely corrosive), and the structure is relatively complicated
The above-mentioned lack of stuffing makes it difficult for the existing methods for preparing luminescent porous silicon to be used on a large scale in industry

Method used

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  • Method of preparing light-emitting porous silicon from LiAlH4
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  • Method of preparing light-emitting porous silicon from LiAlH4

Examples

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Effect test

Embodiment 1

[0029] A LiAlH 4 The method for preparing luminous porous silicon comprises the following steps in sequence:

[0030] (1) White carbon black, LiAlH 4 Mix evenly according to the ratio of 0.8:0.53 parts by weight to obtain a mixture, and place the mixture in a heating furnace with a cavity volume of 10 liters;

[0031] (2) Evenly spread 100-mesh carbon powder on the surface of the mixture, and the ratio of carbon powder to the mixture is 0.07:1.33 by weight;

[0032] (3) The temperature of the furnace cavity of the heating furnace is raised to 400° C. over 1 hour, and the heat preservation reaction is carried out for 5 hours to obtain a reaction product;

[0033] (4) The reaction product is gradually cooled to room temperature, and the cooling condition is to reduce the temperature by 55°C per hour, then, use hydrochloric acid, normal temperature distilled water, and ethanol to repeatedly wash the reaction product three times in a repeated manner, and each time the reaction p...

Embodiment 2

[0037] A LiAlH 4 The method for preparing luminous porous silicon comprises the following steps in sequence:

[0038] (1) White carbon black, LiAlH 4 Mix evenly according to the ratio of 1.6:1.13 parts by weight to obtain a mixture, and place the mixture in a heating furnace with a chamber volume of 30 liters;

[0039] (2) Evenly spread 325-mesh carbon powder on the surface of the mixture, and the ratio of carbon powder to the weight part of the mixture is 0.17:2.73;

[0040] (3) The temperature of the furnace cavity of the heating furnace is raised to 550° C. over 2 hours, and the temperature is kept for 3 hours to obtain the reaction product;

[0041] (4) The reaction product is gradually cooled to room temperature, and the cooling condition is to reduce the temperature by 65°C per hour. Then, use hydrochloric acid, normal temperature distilled water, and ethanol to repeatedly wash the reaction product three times in a repeated manner, and each time the reaction product is...

Embodiment 3

[0045] A LiAlH 4 The method for preparing luminous porous silicon comprises the following steps in sequence:

[0046] (1) White carbon black, LiAlH 4 Mix evenly according to the ratio of 1.2:0.83 parts by weight to obtain a mixture, and place the mixture in a heating furnace with a chamber volume of 20 liters;

[0047] (2) Evenly spread 230-mesh carbon powder on the surface of the mixture, the ratio of carbon powder to the mixture is 0.12:2.03 by weight;

[0048] (3) The temperature of the furnace chamber of the heating furnace is raised to 500° C. over 1.5 hours, and the temperature is kept for 4 hours to obtain the reaction product;

[0049] (4) The reaction product is gradually cooled to room temperature, and the cooling condition is to reduce the temperature by 60°C per hour. Then, use hydrochloric acid, normal temperature distilled water, and ethanol to repeatedly wash the reaction product three times in a repeated manner, and each time the reaction product is washed, ...

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Abstract

A method of preparing light-emitting porous silicon from LiAlH4 comprises the steps of uniformly mixing white carbon black and LiAlH4 at a weight part ratio of (0.8-1.6):(0.53-1.13) to form a mixture, and putting the mixture in a heating furnace with the furnace chamber volume of 10-30L; uniformly spreading 100-325-mesh carbon powder on the surface of the mixture at a weight part ratio of the powdered carbon to the mixture of (0.07-0.17):(1.33-2.73); raising the temperature of a furnace chamber of the heating furnace to 400-550 DEG C within 1-5h, and keeping the temperature for reaction for 3-5h to form a reaction product; gradually cooling the reaction product to the room temperature at a rate of 55-65 DEG C per hour, washing the reaction product with hydrochloric acid, room temperature distilled water and alcohol sequentially for at least once to obtain a washing product, and drying the washing product for 2-3h at 90-110 DEG C to form the light-emitting porous silicon with a better photoelectric effect.

Description

technical field [0001] The present invention relates to a kind of using LiAlH 4 A method for preparing luminescent porous silicon. Background technique [0002] Most of the existing methods for preparing luminescent porous silicon adopt electrochemical corrosion method, that is, in a polytetrafluoroethylene corrosion tank, insert a silicon wafer and a platinum wafer as the anode and cathode respectively, and use hydrofluoric acid or hydrofluoric acid plus ethanol As an electrolyte, the preparation of luminescent porous silicon is limited by many factors such as the concentration and composition of the solution, current density, resistivity, environmental protection and temperature, and the preparation of luminescent porous silicon is more sensitive to light. The chemical reaction process of preparing luminescent porous silicon by this method is complicated and not completely clear up to now. In hydrofluoric acid solution, the electrochemical corrosion rate of silicon wafer ...

Claims

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Application Information

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IPC IPC(8): C09K11/59C01B33/023C01F7/04
Inventor 汪徐春张文张雪梅叶祥桔陈俊明过家好张婷刘涛严家玉徐鑫强
Owner 凤阳振兴电子材料有限公司
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