High-purity strontium-calcium-europium nitride solid solution powder and preparation method thereof

A technology of pure strontium calcium europium and nitride, which is applied in the field of high-purity strontium calcium europium nitride solid solution powder and its preparation, can solve the problems of low purity and waste of nitrogen, and achieve the effect of high purity of raw materials

Pending Publication Date: 2021-03-05
兰州冉华实德新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purity of the product obtained by the above method is not high, and it also costs nitrogen

Method used

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  • High-purity strontium-calcium-europium nitride solid solution powder and preparation method thereof
  • High-purity strontium-calcium-europium nitride solid solution powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: (Sr 0.992 Eu 0.008 )2N

[0033] Weigh 819.7g of calcium metal and 1.25g of europium metal, wash the furnace with argon three times in a vacuum melting furnace, flush with argon to 80KPa, heat to 800°C to melt into a slurry state, pour and cool to obtain an alloy ingot. After cleaning the surface of the alloy ingot, put it into a hydrogen breaker furnace, heat it to 220°C for three times to activate and feed in hydrogen, then heat it to 400°C for 4 hours, then heat it to 600°C to remove the hydrogen, and the vacuum degree is less than 40pa ( instrument display), cool to below 150°C, start feeding nitrogen gas to 0.4MPa, then gradually raise the temperature to 580°C and maintain the gas pressure at 0.5MPa for 4 hours, if the pressure gauge shows no lower within 5 minutes, the reaction is over. Then cool to room temperature, put the material in a stainless steel tank, move it into a glove box with water and oxygen content less than 1ppm, grind it in a pulve...

Embodiment 2

[0034] Embodiment 2: (Sr 0.8 Ca 0.185 Eu 0.015 ) 2 N

[0035]Weigh 83.2g of calcium metal, 786.5g of strontium metal, and 25.57g of europium metal, wash the furnace with argon three times in a vacuum melting furnace, flush with argon to 80KPa, heat to 830°C to melt into a slurry state, pour and cool to obtain an alloy ingot. Clean the surface of the alloy ingot and put it into a hydrogen breaker furnace, heat it to 220°C for three times to activate and feed in hydrogen gas, then heat it to 400°C for 4 hours, then heat it to 600°C to remove the hydrogen gas, and the vacuum degree is less than 40pa (the instrument shows ), cool down to below 150°C, start feeding nitrogen gas to 0.4MPa, then gradually raise the temperature to 580°C and maintain the gas pressure at 0.5MPa for 4 hours, the pressure gauge will not show within 5min, and the reaction is over. Then cool to room temperature, fill the material with a stainless steel tank, move it into a glove box with water and oxyge...

Embodiment 3

[0036] Embodiment 3: (Sr 0.75 Ca 0.235 Eu 0.015 ) 2 N

[0037] Weigh 295.7g of calcium metal, 543.9g of strontium metal, and 31.44g of europium metal, wash the furnace with argon three times in a vacuum melting furnace, flush with argon to 80KPa, heat to 850°C to melt into a slurry state, pour and cool to obtain an alloy ingot. Clean the surface of the alloy ingot and put it into a hydrogen breaker furnace, heat it to 220°C for three times to activate and feed in hydrogen gas, then heat it to 400°C for 4 hours, then heat it to 600°C to remove the hydrogen gas, and the vacuum degree is less than 40pa (the instrument shows ), cool down to below 150°C, start feeding nitrogen gas to 0.4MPa, then gradually raise the temperature to 580°C and maintain the gas pressure at 0.5MPa for 4 hours, the pressure gauge will not show within 5min, and the reaction is over. Then cool to room temperature, fill the material with a stainless steel tank, move it into a glove box with water and ox...

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Abstract

The invention discloses high-purity strontium-calcium-europium nitride solid solution powder and a preparation method thereof. The general formula of the high-purity strontium-calcium-europium nitridesolid solution powder is (Sr1-x-yCaxEuy)2N (x is more than or equal to 0 and less than or equal to 0.45, and y is more than or equal to 0.008 and less than or equal to 0.025). The preparation methodcomprises the steps that S1, Ca, Sr and Eu with the purity larger than or equal to 99.99% are weighed and placed in a vacuum smelting furnace, argon is introduced, melting and pouring are conducted atthe temperature of 700-880 DEG C, and an alloy cast ingot is obtained; S2, after the surface of the cast ingot is cleaned, the cast ingot is placed in a hydrogen decrepitation furnace, hydrogen withthe purity larger than or equal to 99.99% is introduced, the cast ingot is heated to 200-400 DEG C, and the cast ingot is broken and dehydrogenated to obtain alloy coarse powder; S3, the temperature is reduced, liquid nitrogen with the purity larger than or equal to 99.99% is introduced, the temperature is increased to 580 DEG C, the pressure ranges from 0.5 Mpa to 0.8 Mpa, heat preservation is conducted for 5 hours, and high-purity strontium-calcium-europium nitride solid solution coarse powder is obtained; and S4, the coarse powder is transferred into a glove box, and the coarse powder is crushed in a crusher coated with a tungsten carbide coating to obtain a powder finished product.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a high-purity strontium calcium europium nitride solid solution powder and a preparation method thereof. Background technique [0002] At present, with the development of new material technology, controllable high-purity strontium calcium europium nitride solid solution powder is gradually flourishing in the industry, showing a good market prospect, strontium calcium europium nitride solid solution can be used in LED Raw materials for phosphors, ceramic pigments and other fields. [0003] The preparation methods of calcium nitride and strontium nitride are generally obtained by the direct action of alkaline earth metals and nitrogen or ammonia at high temperature. The earliest typical method to develop this technology is to place alkaline earth metal nitrides in a nickel crucible and heat them in a pure nitrogen stream. This work was studied by Henri de moissan (Com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/30C01F17/10C01B21/00
CPCC01B21/0602C01F17/10C01F17/30
Inventor 周宏亮申晋陇张尚虎张轩荣
Owner 兰州冉华实德新材料有限公司
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