Calcium europium nitride solid solution powder and preparation method thereof

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...

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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

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