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Silicon nitride nanowire preparation method, silicon nitride nanowire, silicon nitride powder and silicon nitride submicron powder

A technology of silicon nitride nanometer and silicon nitride powder, which is applied in chemical instruments and methods, nitrogen compounds, nanotechnology, etc., can solve the problems of difficult purification of silicon nitride, harsh process conditions, and difficulty in large-scale production equipment, and achieves High nitriding rate, high purity, and the effect of mass production

Active Publication Date: 2018-11-02
常州硅源新能材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In some existing methods, the raw materials used are expensive, such as nano-silicon powder, carbon nanotube template, etc.; while in other methods, the preparation of raw materials used is difficult or difficult to obtain on a large scale, such as metal sodium, polysilazane , sodium azide, etc.
2) The process conditions are harsh or the method is complicated
For example, in the combustion reaction method, the reaction temperature needs to reach 1400-1600 ° C, and the reaction pressure also needs to reach 1-30 MPa, which makes it difficult to enlarge the production equipment (such as patent CN02100195 - Synthesis of high α phase by combustion)
3) Separation or purification is difficult, that is, silicon nitride nanowires are often mixed with unreacted raw materials and silicon nitride powder, which is difficult to separate and purify; and if a metal catalyst is used in the raw materials, it will also make it difficult to purify silicon nitride in the later stage

Method used

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  • Silicon nitride nanowire preparation method, silicon nitride nanowire, silicon nitride powder and silicon nitride submicron powder
  • Silicon nitride nanowire preparation method, silicon nitride nanowire, silicon nitride powder and silicon nitride submicron powder
  • Silicon nitride nanowire preparation method, silicon nitride nanowire, silicon nitride powder and silicon nitride submicron powder

Examples

Experimental program
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Effect test

Embodiment 1

[0045] (1) Granulation: at room temperature, add 1 wt% amylopectin into water, stir and slowly heat up to 80°C, and obtain transparent starch colloid after constant temperature for 1 hour;

[0046] Add silicon powder with irregular shape and particle size of 0.1-10 μm into the starch colloid, so that the solid content in the colloid after adding the silicon powder is 50wt% (starch / silicon particle=0.01, mass ratio), and then at 80°C Stirring under constant temperature conditions for 3 hours to obtain a suspension slurry;

[0047] Use a centrifugal spray dryer to granulate the above slurry, the feed rate is 0.5L / h, the nozzle temperature is 320°C, and the rotation speed is 20r / min. The obtained product is porous spherical particles with a size of 50-300μm , which is granulated silicon powder, and the microscopic appearance of the obtained granulated silicon powder is as follows figure 2 shown;

[0048] (2) Nitriding: Place granulated silicon powder in an inert atmosphere pro...

Embodiment 2

[0057] (1) Granulation: at room temperature, add 0.5 wt% amylopectin into water, stir and slowly heat up to 75°C, and obtain transparent starch colloid after constant temperature for 1.5 hours;

[0058] Add silicon powder with irregular shape and particle size of 0.1-10 μm into the starch colloid, so that the solid content in the colloid after adding the silicon powder is 50wt% (starch / silicon particles=0.005, mass ratio), and then at 75°C Stirring under constant temperature conditions for 2.5 hours to obtain a suspension slurry;

[0059] Use a centrifugal spray dryer to granulate the above slurry, the feed rate is 0.75L / h, the temperature of the nozzle is 320°C, and the rotation speed is 20r / min to obtain porous spherical particles with a size of 50-200μm, which is the production process. silicon powder;

[0060] (2) Nitriding: Place granulated silicon powder in an inert atmosphere protection furnace, feed a mixed gas of nitrogen and hydrogen (the volume fraction of hydrogen...

Embodiment 3

[0069] (1) Granulation: at room temperature, add 0.5 wt% amylose into water, stir and slowly heat up to 90°C, and obtain transparent starch colloid after constant temperature for 3 hours;

[0070] Add silicon powder with irregular shape and particle size of 0.1-10 μm into the starch colloid, so that the solid content in the colloid after adding the silicon powder is 50wt% (starch / silicon particle=0.005, mass ratio), and then at 90°C Stirring under constant temperature conditions for 3 hours to obtain a suspension slurry;

[0071] Use the centrifugal spray dryer to granulate the above slurry, the feed rate is 1L / h, the nozzle temperature is 350°C, and the rotation speed is 10r / min to obtain porous spherical particles with a size of 50-300μm, which is granulation Silica fume;

[0072] (2) Nitriding: Place granulated silicon powder in an inert atmosphere protection furnace, feed a mixed gas of nitrogen and hydrogen (the volume fraction of hydrogen is 15%) into the furnace as a r...

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Abstract

The invention provides a preparation method for a silicon nitride nanowire. The method provided by the invention comprises the following steps: with cheap and easily-available silicon powder as a raw material, and without the need of using a catalyst, subjecting the silicon powder to granulating, then carrying out a nitridation reaction so as to prepare silicon nitride particles, and carrying out simple operations like grinding, crushing, washing, settling separation and drying so as to be able to simultaneously obtain a high-purity silicon nitride nanowire and a silicon nitride powder product. Thus, the preparation method is a simple and economical method applicable to industrial large-scale preparation of the silicon nitride nanowire.

Description

technical field [0001] The invention relates to the field of nanowire preparation, in particular to a method for preparing silicon nitride nanowires, silicon nitride nanowires, silicon nitride powder and silicon nitride submicron powder. Background technique [0002] Silicon nitride (Si 3 N 4 ) has a series of excellent thermal properties such as good thermal shock resistance, oxidation resistance, high temperature resistance, corrosion resistance, high chemical stability, high strength, and high hardness, and is an excellent high-temperature structural material. [0003] Silicon nitride (Si 3 N 4 ) nanowire is a one-dimensional nanostructure form of silicon nitride material, which not only has various excellent properties possessed by bulk materials, but also has many new characteristics as a one-dimensional nanomaterial. For example: the flexural strength (up to 3.6GPa) and elastic model (up to 570GPa) of silicon nitride nanowires are much higher than those of bulk mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/068B82Y40/00
CPCC01B21/0682C01B21/0687C01P2004/16C01P2004/60C01P2004/61C01P2006/80
Inventor 雷超魏飞张晨曦
Owner 常州硅源新能材料有限公司
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