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Process for preparing magnesium nitride through airflow method

A technology of magnesium nitride and air flow method, which is applied in the direction of nitrogen-metal/silicon/boron binary compounds, etc., can solve the problems of complex operation of equipment, long reaction time, low yield of magnesium nitride, etc., and achieve uniform product particles, The effect of simple process operation and high synthesis efficiency

Inactive Publication Date: 2011-11-16
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods have disadvantages such as high cost, long process flow, complicated equipment operation, or relatively low yield of magnesium nitride, thus limiting its industrial production.
Although the direct reaction of magnesium powder with nitrogen has industrial value, the production of magnesium nitride powder requires a higher reaction temperature and a longer reaction time, and the shape of the particles is incomplete and easy to agglomerate, which cannot meet the requirements of industrial quality.

Method used

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  • Process for preparing magnesium nitride through airflow method
  • Process for preparing magnesium nitride through airflow method
  • Process for preparing magnesium nitride through airflow method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 (comparative example).

[0023] Put 1.5g of Mg powder in a ceramic boat, put the ceramic boat into the tube furnace, close the tube furnace, and then fill with ammonia gas for 10 minutes to replace the air in the tube furnace to avoid air affecting the test results. Then, when the furnace temperature of the tubular constant temperature furnace gradually reaches three specific temperatures of 750°C, 800°C and 850°C, the ammonia gas valve is opened for ammoniation, the ammonia gas flow rate is 500ml / min, and the nitriding time is 2h. Cool naturally in the furnace. A block-shaped sample of vegetable pine is obtained, and the sample is finely ground to obtain a product powder. After quantitative analysis of the phase, the result is: the main phase is Mg 3 N 2 phase, followed by the MgO phase. as attached figure 1 shown.

[0024] From the results obtained in Example 1, the generated Mg 3 N 2 The particles are less uniform, prone to caking, and the purity is...

Embodiment 2

[0026] Put 1.5g of Mg powder in a ceramic boat, put the ceramic boat into the tube furnace, close the tube furnace, and then fill with ammonia gas for 10min to replace the air in the tube furnace to avoid air affecting the test results, and then When the furnace temperature of the tubular thermostatic furnace reaches 600°C, keep it in an ammonia atmosphere for 60 minutes, and then gradually increase the tubular thermostatic furnace to three specific temperatures of 750°C, 800°C, and 850°C, and open the ammonia valve for ammoniation. , ammonia flow 500ml / min, nitriding time 60min, after nitriding, the ceramic boat is naturally cooled in the furnace. A block-shaped sample of vegetable pine is obtained, and the sample is finely ground to obtain a product powder. Quantitative analysis of the phase shows that the pure phase is Mg when the sample is kept at 600°C for 1h and then nitrided at 800°C for 1h. 3 N 2 Mutually. as attached figure 2 (b) shown.

Embodiment 3

[0028] Put 2g of Mg powder in a ceramic boat, put the ceramic boat into the tube furnace, close the tube furnace, and then fill with ammonia gas for 15min to replace the air in the tube furnace to avoid air affecting the test results, and then wait for When the furnace temperature of the tubular constant temperature furnace reaches 610°C, keep it in an ammonia atmosphere for 40 minutes, and then gradually increase the tubular constant temperature furnace to three specific temperatures of 750°C, 800°C, and 850°C, and open the ammonia valve for ammoniation. The flow rate of ammonia gas was 400ml / min, and the nitriding time was 70min. After nitriding, the ceramic boat was naturally cooled in the furnace. A block-shaped sample of vegetable pine is obtained, and the sample is finely ground to obtain a product powder.

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Abstract

The invention relates to a process for preparing magnesium nitride through an airflow method. The process comprises the following steps: placing Mg powder into a ceramic boat; sending the ceramic boat to a tube furnace; sealing the tube furnace; introducing ammonia gas for 10 to 15 min for displacing air in the tube furnace to avoid an influence of air on test results; keeping a temperature for 40 to 80 min in ammonia gas atmosphere when the temperature of a tube thermostatic furnace achieves 600 to 610 DEG C; ammonifying for 50 to 70 min through opening an ammonia gas valve with an ammonia gas flow of 400 to 600 ml / min when the temperature of the tube thermostatic furnace gradually achieves three specific values of 750 DEG C, 800 DEG C, and 850 DEG C; and carrying out natural cooling on the ceramic boat in the tube furnace after nitridation. The process of the present invention allows any additive not to be needed, operation to be simple, product purity to be guaranteed, synthesis efficiency to be high, a case that the process is more economical and has a higher production efficiency than processes adopting nitrogen to be realized, technology to be easily control, and low nitridation temperature, less energy consumption, short production period, and uniformity of product particles to be realized.

Description

technical field [0001] The invention belongs to the field of inorganic non-metallic materials, and relates to a preparation method of magnesium nitride powder. Background technique [0002] Magnesium nitride is widely used in the preparation of new ceramic materials with high hardness, high thermal conductivity, wear resistance, corrosion resistance and high temperature resistance. In the solid phase reaction of boron nitride and silicon nitride, magnesium nitride is an indispensable sintering aid. At the same time, magnesium nitride plays an important role in the recovery of nuclear fuel, purification of magnesium alloy melt, removal of aluminum alloy inclusions, and catalysis in the formation of hBN. In addition Mg 3 N 2 As an additive, it can effectively desulfurize and increase alum, thereby improving the density, strength, tensile force and bearing capacity of steel, so Mg 3 N 2 It is widely used in the smelting industry of construction steel. [0003] At present, ...

Claims

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Application Information

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IPC IPC(8): C01B21/06
Inventor 谭敦强陈发勤李建国陈强
Owner NANCHANG UNIV
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