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Preparation method of rare earth halide

A rare earth oxide and halide technology, applied in the direction of rare earth metal halide, rare earth metal chloride, etc., can solve the problems of increased oxygen content and pollution of LnX3, and achieve the effect of avoiding the increase of oxygen content and pollution

Active Publication Date: 2020-05-22
北京梦晖科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1) At the stage where the temperature is higher than 400°C, as the temperature reaches 400°C, NH 4 X gradually transforms into gaseous NH 3 And HX, where HX is a strongly acidic and corrosive gas, will react with the quartz crucible, and the degree of reaction will become more serious with the increase of temperature, thus introducing the Si element in the crucible into LnX 3 , causing LnX 3 pollution
[0008] 2) The most commonly used quartz (SiO 2 ) when the crucible reaches a temperature above 500°C, some of the hydroxyl groups are released and combine with LnX 3 react to generate LnOX, thus causing LnX 3 elevated oxygen levels

Method used

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preparation example Construction

[0026] Aiming at the problems in the prior art that rare earth halides are easily polluted and the oxygen content increases during the preparation process of rare earth halides, the embodiment of the present invention discloses a preparation method of rare earth halides. Deamination is carried out in a homogeneous rare earth oxide crucible, thereby obtaining an oxygen-free, anhydrous high-purity rare earth halide. Specifically, the preparation method of the rare earth halide described in the present application specifically includes the following steps:

[0027] Will LnX 3 · nNH 4 X powder is heated in a rare earth oxide crucible to obtain the rare earth halide LnX 3 ; the LnX 3 · nNH 4 The rare earth elements in the X powder are the same as those in the rare earth oxide crucible;

[0028] Wherein Ln is selected from rare earth elements, and the rare earth elements are selected from any one of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc and Y, X is halogen...

Embodiment 1La2

[0040] Example 1La 2 o 3 Preparation of LaBr by crucible method 3

[0041] (1) La with a purity ≥ 99.99% 2 o 3 React with HBr to give LaBr 3 solution, then press LaBr 3 with NH 4 The molar ratio of Br is 1:6 and NH is added 4 Br is mixed, the mixed solution is concentrated and dehydrated to obtain LaBr 3 6NH 4 Br powder solid;

[0042] (2) LaBr obtained in step (1) 3 6NH 4 Br powder solids were transferred into the pre-prepared La 2 o 3 Crucible, and pass through argon or nitrogen for gas protection;

[0043] (3) Raise the temperature of the material treated in step (2) to 350°C at a heating rate of 10°C / min, keep it warm for 2 hours, then raise the temperature to 900°C at a heating rate of 5°C / min, then stop heating after holding for 2 hours , cooled naturally to room temperature to obtain high-purity, oxygen-free, anhydrous LaBr 3 .

Embodiment 2La2

[0044] Example 2La 2 o 3 Preparation of LaBr by crucible method 3

[0045] (1) La with a purity ≥ 99.99% 2 o 3 with NH 4 Br is mixed in a molar ratio of 1:12, and LaBr is obtained after heating 3 12NH 4 Br powder; LaBr 3 12NH 4 Br powder loaded into La 2 o 3 Crucible, and pass through argon or nitrogen for gas protection;

[0046] (2) Raise the temperature of the material treated in step (1) to 400°C at a heating rate of 2°C / min, keep it warm for 4 hours, then raise the temperature to 900°C at a heating rate of 4°C / min, then stop heating after holding for 4 hours , cooled naturally to room temperature to obtain high-purity, oxygen-free, anhydrous LaBr 3 .

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PUM

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Abstract

The invention provides a preparation method of rare earth halide. The method comprises the following steps: heating LnX3.nNH4X powder in a rare earth oxide crucible to obtain rare earth halide LnX3, wherein the rare earth element in the LnX3.nNH4X powder is the same as the rare earth element in the rare earth oxide crucible, Ln is selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc and Y, X is halogen, and n is more than 0 and less than or equal to 12. According to the preparation method provided by the invention, the high-purity, anhydrous and oxygen-free rare earth halide can be obtained; and the anhydrous high-purity rare earth halide obtained by the method can be used for growing high-purity blocky single crystals or fibrous single crystals with excellent scintillation performance.

Description

technical field [0001] The invention relates to the technical field of new inorganic materials, in particular to a preparation method of rare earth halides. Background technique [0002] Metal halides are very important chemical raw materials and are widely used in the fields of catalysis, luminescence, and functional materials. In particular, the anhydrous and oxygen-free high-purity rare earth halides in metal halides are important raw materials for the preparation of scintillation crystals, but due to their strong hygroscopicity and easy oxidation at high Water halides are both important and difficult. [0003] At present, the commonly used high-purity anhydrous halide preparation methods mainly include two routes: [0004] 1) Get LnX in solution 3 with NH 4 A mixture or complex of X, and then the solution is concentrated and dehydrated under certain conditions to obtain LnX 3 · nNH 4 X powder solid, then heated in a quartz crucible to remove excess NH 4 X to obtai...

Claims

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Application Information

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IPC IPC(8): C01F17/253C01F17/271
CPCC01P2006/80C01P2006/82
Inventor 李文宝
Owner 北京梦晖科技有限公司
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