Calcium europium nitride solid solution powder and preparation method thereof

A technology of nitride and solid solution, which is applied in the chemical industry, can solve problems such as failure to meet production requirements, long time consumption, and difficult reaction, and achieve high product uniformity and consistency, avoid uncontrollable impurities, and strict process control.

Pending Publication Date: 2021-02-26
兰州冉华实德新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The reaction between metallic calcium and nitrogen begins at a temperature of 360°C, but the increase in weight is small, and the reaction will stop at a later stage. This is because the reaction forms a layer of N-Ca film that makes the reaction difficult to proceed, even at If the temperature is kept at 650°C for more than 50 hours, the reaction is difficult to proceed, and a large amount of nitrogen gas flow is required.
At this time, if a small amount of impurity gases such as moisture, carbon dioxide, oxygen, etc. are entrained in nitrogen, they will be completely absorbed by the metal at high temperature, and the oxygen content of the final product will be high, and the reaction time needs to last for more than 100 hours to complete the reaction; Therefore, the purity of the product obtained by the preparation method in the prior art is not high, it takes a long time, and it needs to consume a large amount of nitrogen, which cannot meet the production requirements

Method used

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  • Calcium europium nitride solid solution powder and preparation method thereof
  • Calcium europium nitride solid solution powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: Preparation (Ca 0.995 Eu 0.005 ) 3 N 2 ;

[0037] Weigh 981.3g of calcium metal and 1.87g of europium metal, wash the furnace with argon three times in a vacuum melting furnace, flush with argon to 80KPa, heat to 780°C to melt into a slurry state, cast 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 activation after vacuuming three times, pass in hydrogen, and then heat it to 360°C for 4 hours, then heat it to 580°C and vacuumize to remove the hydrogen. After it is less than 40pa (displayed by the instrument), cool down to below 300°C, start to feed nitrogen to 0.5MPa, then gradually increase the temperature to 460°C, maintain the gas pressure at 0.5MPa, keep it for 3 hours, then raise the temperature to 610°C for 5 hours, Within 5 minutes, the pressure gauge shows that it is no longer declining, and the reaction is over. Then cool to room temperature, put t...

Embodiment 2

[0038] Embodiment 2: Preparation (Ca 0.985Eu 0.015 ) 3 N 2 ;

[0039] Weigh 945.3g of calcium metal and 54.7g 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 activation after vacuuming three times, pass in hydrogen, and then heat it to 360°C for 4 hours, then heat it to 580°C to remove the hydrogen, and the vacuum degree is less than After 40pa (instrument display), cool down to below 300°C, start feeding nitrogen gas to 0.55MPa, then gradually raise the temperature to 460°C, maintain the gas pressure at 0.5MPa, keep it for 4 hours, then raise the temperature to 610°C for 5 hours, 5min The internal pressure gauge shows that it is no longer declining, and the reaction ends. Then cool to room temperature, fill the materi...

Embodiment 3

[0040] Embodiment 3: preparation (Ca 0.98 Eu 0.02 ) 3 N 2 ;

[0041] Weigh 728g of calcium metal and 72g of europium metal, wash the furnace with argon three times in a vacuum melting furnace, flush with argon to 80KPa, heat to 810°C, 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 activation after vacuuming three times, pass in hydrogen, and then heat it to 360°C for 4 hours, then heat it to 580°C to remove the hydrogen, and the vacuum degree is less than After 40pa (instrument display), cool down to below 300°C, start feeding nitrogen gas to 0.6MPa, then gradually raise the temperature to 460°C, maintain the gas pressure at 0.6MPa, keep it for 4 hours, then raise the temperature to 610°C for 5 hours, 5min The internal pressure gauge shows that it is no longer declining, and the reaction ends. Then cool to room temperature, fill the material with ...

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Abstract

The invention discloses calcium europium nitride solid solution powder and a preparation method thereof. The calcium europium nitride solid solution powder is prepared by crushing a calcium europium nitride solid solution, and the chemical general formula of the calcium europium nitride solid solution is (Ca1-xEux)3N2; wherein x is larger than 0 and smaller than or equal to 0.025. The preparationmethod comprises the following steps: S1, weighing calcium Ca and europium Eu, putting calcium Ca and europium Eu into a vacuum smelting furnace, vacuumizing, washing the furnace, introducing argon asa protective gas, melting, and pouring into an ingot mold to obtain an alloy ingot; S2, after surface cleaning is conducted on the alloy ingot, placing the alloy ingot in a hydrogen breaking furnace,introducing hydrogen, heating, crushing the alloy ingot, heating, and removing hydrogen to obtain coarse alloy powder; and S3, reducing the temperature of the hydrogen breaking furnace to 300 DEG C or below, introducing nitrogen into the hydrogen breaking furnace, gradually reducing the temperature to 460 DEG C, keeping the temperature for 180 minutes, then raising the temperature to 610 DEG C, and keeping the temperature for 300 minutes to obtain the calcium europium nitride solid solution powder.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a calcium europium nitride solid solution powder and a preparation method thereof. Background technique [0002] At present, with the development of new material technology, calcium europium nitride solid solution powder with controllable composition and structure is gradually flourishing in the industry, showing a good market prospect. Calcium europium nitride solid solution can be used in LED phosphors , Ceramic pigments and other fields of raw materials. [0003] The reaction between metallic calcium and nitrogen begins at a temperature of 360°C, but the increase in weight is small, and the reaction will stop at a later stage. This is because the reaction forms a layer of N-Ca film that makes the reaction difficult to proceed, even at It is also difficult to carry out the reaction at 650°C for more than 50 hours, and a large amount of nitrogen gas flow must be intro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/30C01F17/10C01B21/06
CPCC01F17/30C01F17/10C01B21/0612C01P2002/72C01P2006/60
Inventor 申晋陇周宏亮张尚虎张轩荣
Owner 兰州冉华实德新材料有限公司
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