A method for preparing ultra-high α-phase silicon nitride by using silicon nanotubes

A technology of phase silicon nitride and silicon nanotubes, which is applied in the field of preparing ultra-high alpha phase silicon nitride by using silicon nanotubes, can solve the problems of difficulty in controlling the degree of nitridation, unsuitable for industrial production, complicated operation process, etc. The effect of increasing the reaction rate, suppressing self-sintering, and increasing the contact area

Active Publication Date: 2018-10-30
浙江锂宸新材料科技有限公司
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Problems solved by technology

Although this scheme can also increase the content of α-phase to a certain extent, it requires high equipment, and the operation process is complicated. The degree of nitriding in the first step is difficult to control, the repeatability is poor, and it is not suitable for industrial production.

Method used

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  • A method for preparing ultra-high α-phase silicon nitride by using silicon nanotubes
  • A method for preparing ultra-high α-phase silicon nitride by using silicon nanotubes
  • A method for preparing ultra-high α-phase silicon nitride by using silicon nanotubes

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Embodiment 1

[0023] Silicon nanotubes are used as raw materials, the outer diameter is 400nm, the inner diameter is 250nm, and the specific surface area is 24m2 / g. Under a nitrogen atmosphere, keep warm at 1350°C for 25 hours to obtain loose high-α-phase silicon nitride; then use a planetary ball mill to perform planetary high-energy ball milling on the obtained silicon nitride. The ball milling speed is 1000r / min, and the milling time is 30h, and ultra-high α-phase silicon nitride with uniform particle size distribution can be obtained.

[0024] The product prepared in this embodiment is carried out X-ray energy spectrum analysis (XRD), the result is as follows figure 1 As shown, the α-phase content is 94.8%.

Embodiment 2

[0026] Silicon nanotubes are used as raw materials, the outer diameter is 150nm, the inner diameter is 85nm, and the specific surface area is 75m2 / g. Under a nitrogen atmosphere, keep warm at 1300°C for 22 hours to obtain loose high-α-phase silicon nitride; then use a planetary ball mill to perform planetary high-energy ball milling on the obtained silicon nitride. The ball milling speed is 1000r / min, and the time is 26h, and ultra-high α-phase silicon nitride with uniform particle size distribution can be obtained.

[0027] The product prepared in this embodiment is carried out X-ray energy spectrum analysis (XRD), the result is as follows figure 2 As shown, the α-phase content is 97.9%.

Embodiment 3

[0029] Silicon nanotubes are used as raw materials, with an outer diameter of 75nm, an inner diameter of 30nm, and a specific surface area of ​​90m2 / g. In a nitrogen atmosphere, keep warm at 1250°C for 20 hours to obtain loose high-α-phase silicon nitride; then use a planetary ball mill to perform planetary high-energy ball milling on the obtained silicon nitride. The ball milling speed is 1000r / min, and the time is 22h, and ultra-high α-phase silicon nitride with uniform particle size distribution can be obtained.

[0030] The product prepared in this embodiment is carried out X-ray energy spectrum analysis (XRD), the result is as follows image 3 As shown, the α-phase content is 99.1%.

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Abstract

The invention discloses a method for preparing ultrahigh alpha-phase silicon nitride by means of silicon nanotubes. The method comprises the following steps that 1, silicon nanotubes of which the outer diameters range from 50 nm to 500 nm, the inner diameter ranges from 20 nm to 300 nm, and the specific surface area ranges from 20 m<2> / g to 100 m<2> / g are subjected to high-temperature nitridation in nitrogen at the temperature of 1,220 DEG C to 1,370 DEG C, and a first product is obtained, wherein the heat preservation temperature ranges from 12 h to 28 h; 2, the first product obtained in the first step is subjected to planetary high-energy ball milling, wherein the rotating speed of planetary high-energy ball milling is 1,000 r / min, and the time ranges from 20 h to 30 h. According to the method for preparing ultrahigh alpha-phase silicon nitride by means of the silicon nanotubes, the process is simple, the performance is controllable, the production cycle is short, the production energy consumption is greatly reduced, and the method is specially suitable for preparing ultrahigh alpha-phase silicon nitride.

Description

technical field [0001] The invention relates to the field of silicon nitride preparation, in particular to a method for preparing ultra-high α-phase silicon nitride by using silicon nanotubes. Background technique [0002] Silicon nitride is a widely used special ceramic material. It has the advantages of high temperature resistance, small specific gravity, high strength, high hardness, and wear resistance, and is widely used in automobile, military, metallurgy, medical and other industries. [0003] In order to obtain high-strength and high-hardness silicon nitride ceramics, silicon nitride powder with a high α phase is often used as a raw material. This is because during the high-temperature sintering process of silicon nitride, the α phase can be transformed into a rod-like or needle-like β phase, and this β phase with a certain aspect ratio will act like a toughening fiber, which will help silicon nitride ceramics Increased strength and hardness. Therefore, the prepar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/584C04B35/65
CPCC04B35/591C04B35/65C04B2235/5284C04B2235/658C04B2235/96
Inventor 赵立旸戎华李钦稿杜英
Owner 浙江锂宸新材料科技有限公司
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