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Method for producing zirconium nitride powder

A production method, zirconium nitride technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of long production process, easy melting, and high cost, so as to reduce production cost, increase production capacity, and improve nitrogen The effect of chemical efficiency

Active Publication Date: 2012-07-04
锦州市金属材料研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the problems of the existing metal zirconium nitriding method, such as long production process, high cost, and easy melting phenomenon in the synthesis process, and provide a short process flow, low production cost, and no melting in the synthesis process. Phenomenon of production method of zirconium nitride powder

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1.1. Grinding zirconium sponge with a purity greater than 99% into particles with a particle size of less than 3mm;

[0017] 1.2. Pre-nitridation: Put the pulverized zirconium sponge particles in a vacuum furnace, firstly evacuate, and the vacuum degree reaches 10Pa, then power on and heat up, continue to evacuate during the heating process, and keep the vacuum degree within the range of 10-100Pa, After reaching the pre-nitridation temperature, keep the temperature constant, stop the vacuuming, and fill the furnace with nitrogen to carry out the pre-nitridation reaction, wherein the nitrogen purity is greater than 99.9%, the pre-nitridation temperature is 750°C, the heating time is 7 hours, and the nitrogen pressure in the furnace 80-100kPa, and the pre-nitridation time is 4 hours; after the pre-nitridation is completed, the power is turned off to cool down, and nitrogen gas is continuously filled during the cooling process, and the nitrogen pressure in the furnace is ke...

Embodiment 2

[0021] 2.1. Grinding zirconium sponge with a purity greater than 99% into particles with a particle size of less than 3 mm;

[0022] 2.2. Pre-nitridation: Put the pulverized zirconium sponge particles in a vacuum furnace, firstly evacuate, and the vacuum degree reaches 10Pa, then power on and heat up. After reaching the pre-nitridation temperature, keep the temperature constant, stop vacuuming, and fill the furnace with nitrogen to carry out the pre-nitridation reaction, wherein the nitrogen purity is greater than 99.9%, the pre-nitridation temperature is 800°C, the heating time is 9 hours, and the nitrogen pressure in the furnace 80-100kPa, and the pre-nitridation time is 4 hours; after the pre-nitridation is completed, the power is turned off to cool down, and nitrogen gas is continuously filled during the cooling process, and the nitrogen pressure in the furnace is kept at 100-110kPa, and the temperature is lowered to 80°C to release the furnace;

[0023] 2.3 Nitriding: Gri...

Embodiment 3

[0026] 3.1. Grinding zirconium sponge with a purity greater than 99% into particles with a particle size of less than 3 mm;

[0027] 3.2. Pre-nitridation: Put the pulverized zirconium sponge particles in a vacuum furnace, firstly evacuate, and the vacuum degree reaches 5Pa, then power on and heat up. After reaching the pre-nitridation temperature, keep the temperature constant, stop vacuuming, and fill the furnace with nitrogen to carry out the pre-nitridation reaction, wherein the nitrogen purity is greater than 99.9%, the pre-nitridation temperature is 700°C, the heating time is 5 hours, and the nitrogen pressure in the furnace 80-100kPa, and the pre-nitridation time is 5 hours; after the pre-nitridation is completed, the power is turned off to cool down, and the nitrogen gas is continuously filled during the cooling process, and the nitrogen pressure in the furnace is kept at 100-110kPa, and the temperature drops to 80°C to release the furnace;

[0028] 3.3 Nitriding: crush...

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Abstract

The invention discloses a method for producing zirconium nitride powder, which comprises the following steps of: crushing sponge zirconium into granules with the granularity of less than 3mm, putting the crushed sponge zirconium granules into a vacuum furnace, supplying power for raising the temperature when the vacuum degree is 5 to 40Pa, keeping the temperature at the pre-nitrogenization temperature, stopping vacuumizing, and introducing nitrogen into the furnace for a pre-nitrogenization reaction; after the pre-nitrogenization, cutting off the power for reducing the temperature to 80 DEG C, and discharging; crushing the pre-nitrogenized materials into powder with the granularity of less than 0.075mm, putting the powder into the vacuum furnace, supplying power for raising the temperature to between 500 and 700 DEG C within 2 to 5 hours when the vacuum degree is 5 to 40Pa; stopping vacuumizing, introducing nitrogen into the furnace continuously raising the temperature to the nitrogenization temperature within 3 to 6 hours, and continuously introducing the nitrogen for nitrogenization; after the nitrogenization, cutting off the power for reducing the temperature, continuously introducing the nitrogen in the process of reducing the temperature, and discharging a zirconium nitride clinker when the temperature is reduced to 80 DEG C; and crushing the zirconium nitride clinker so as to prepare the zirconium nitride powder.

Description

technical field [0001] The invention belongs to the field of powder metallurgy production, in particular to a production method of zirconium nitride powder. Background technique [0002] Zirconium nitride ZrN is a kind of refractory compound with golden yellow color, high decomposition temperature, good chemical stability, good high temperature resistance, corrosion resistance and wear resistance. Surface protection material. At present, there are roughly three methods for synthesizing ZrN: first, direct nitriding of metal zirconium powder Zr; second, zirconia ZrO 2 Carbothermal reduction nitriding method; third, zirconium chloride ZrCl 4 vapor deposition method. The direct nitriding method of metal zirconium powder is to heat zirconium powder with a particle size of less than 0.045mm to 1200°C in nitrogen to form ZrN. This method has simple process, low energy consumption and high purity of product ZrN, which can reach 99-99.9%. The disadvantage is that the reaction can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/076
Inventor 王明秋黎明张桂华卜宪坤
Owner 锦州市金属材料研究所
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