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Preparation method of hyperpure nitride powder

A nitride and powder technology, which is applied in the field of preparation of ultrapure nitride powder, can solve the problems that the quality consistency and stability of the reaction product cannot be guaranteed, and the temperature control of the reaction system is inconvenient, so as to achieve good adhesion and stability. The effect of sintering activity, less impurities and high powder content

Active Publication Date: 2013-06-19
烟台同立高科新材料股份有限公司
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Problems solved by technology

However, this method is not convenient for temperature control of the reaction system, and the quality consistency and stability of the reaction product cannot be guaranteed

Method used

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  • Preparation method of hyperpure nitride powder

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preparation example Construction

[0030] Such as figure 1 Shown, a kind of preparation method of ultrapure nitride powder comprises the following steps:

[0031] (1) Combine metal powder, diluent and NH 4 Cl is fully mixed in the tank mill to obtain the original mixture;

[0032] (2) After the original mixture is screened, a reaction material is obtained, and the reaction material is evenly packed in a graphite boat;

[0033] (3) Close the reactor where the graphite boat is located, vacuumize it, and then fill it with high-purity nitrogen;

[0034] (4) In the reactor, the primer is ignited by energizing the nickel-chromium wire, and the heat generated by the primer ignites the reaction material to obtain the ultra-pure nitride powder.

[0035] Typically, the primer is ignited by passing a 10 A DC current through the nichrome wire. After the reaction, the reactor is cooled to room temperature, the gas in the reactor is removed, and the product is unloaded from the graphite boat for processing. Among them, ...

Embodiment 1

[0038] Metal silicon powder, silicon nitride powder, NH 4 Cl is weighed at a mass ratio of 43:47:10, and fully mixed with silicon nitride balls in the pot mill for 4 hours. The purpose of using silicon nitride balls is to prevent other impurities from being brought in during the grinding process and reduce the synthesis of powder The impurity content of the mixed material is evenly packed in a porous semicircular graphite boat with a diameter of 150mm and a length of 800mm after passing through a 30-mesh sieve.

[0039] Vacuum after closing the reactor, and the vacuum degree reaches 10 -4 MPa, and then filled with high-purity nitrogen to a pressure of 4MPa. The mixture of Ti and C with a molar ratio of 1:1 is ignited by a direct current of 10A through a nickel-chromium wire, and the heat generated by the mixture ignites the reaction material until the reaction is complete.

[0040] Among them, the silicon nitride powder is synthesized by combustion synthesis method, the puri...

Embodiment 2

[0048] Metal aluminum powder, aluminum nitride powder, NH 4 Cl is weighed at a mass ratio of 40:50:10, and is fully mixed with alumina balls in the pot mill for 4 hours. The purpose of using aluminum nitride balls is to prevent other impurities from being brought into the grinding process and reduce the synthetic powder. Impurity content, the mixed material is evenly packed in a porous semicircular graphite boat with a diameter of 150mm and a length of 800mm after passing through a 30-mesh sieve.

[0049] Vacuum after closing the reactor, and the vacuum degree reaches 10 -4 MPa, and then filled with high-purity nitrogen to a pressure of 4MPa. The mixture of Ti and C with a molar ratio of 1:1 is ignited by a direct current of 10A through a nickel-chromium wire, and the heat generated by the mixture ignites the reaction material until the reaction is complete.

[0050] Among them, the aluminum nitride powder is synthesized by the aluminum powder nitriding method, the purity is...

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Abstract

The invention relates to a preparation method of hyperpure nitride powder. The preparation method comprises the following steps of fully mixing metal powder, a diluent and an additive in a pot mill to obtain an original mixture, screening the original mixture to obtain a reaction material, uniformly putting the reaction material into a graphite boat, closing a reactor with the graphite boat, carrying out vacuum-pumping, filling high-purity nitrogen into the reactor, and supplying power to nichrome wires to ignite a primer in the reactor, wherein the reaction material is ignited by heat produced by the primer and then produces the hyperpure nitride powder. In the reactor having high nitrogen pressure, through radiation ignition, a part of the reaction material is ignited, and through heat produced by a self-maintenance exothermic reaction of the powder and nitrogen, the reaction material fully reacts. The preparation method does not need an external heat source and has short reaction time. The hyperpure nitride powder obtained by the preparation method has high content and stable quality.

Description

technical field [0001] The invention relates to a preparation method of ultrapure nitride powder, which belongs to the field of chemical synthesis of inorganic materials. Background technique [0002] The new material industry is an emerging industry in the 21st century, covering more than 10 key areas and included in the national "Twelfth Five-Year" strategic plan. Ultra-pure nitride powder materials belong to the field of new inorganic non-metallic materials in planning, and are widely used in functional ceramics, new energy materials, semiconductor lighting materials, nanomaterials and other fields. [0003] In the prior art, the gas-phase enhanced temperature-controlled activated combustion synthesis technology is usually used for the development of ultra-pure nitride powder technology. The Combustion Synthesis (CS) method is an emerging material preparation method, which was first proposed by Merzhanov and Borovinskya of the Institute of Chemical Physics of the former ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06
Inventor 郭大为陈晓光孙洪亮
Owner 烟台同立高科新材料股份有限公司
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