Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing rare earth halides

A halide and rare earth technology, applied in the field of preparation of high-purity rare earth halides, can solve problems such as unavoidable hydrolysis of LnX3, inability to ensure sufficient and thorough reaction, high environmental pollution and difficult operation

Active Publication Date: 2015-01-14
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method pollutes the environment and is difficult to operate
[0008] The above preparation methods cannot guarantee that the reaction is carried out fully and thoroughly, and it is difficult to avoid the hydrolysis of a small amount of LnX3

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: LaCl with a purity higher than 99.99% 3 preparation of

[0017] Weigh La with a purity of 99.999% 2 o 3 Sample 500g, NH with a purity higher than 99.9% 4 Cl sample 1250g, add 500ml of distilled ethanol, mix and stir with a high-speed homogenizer for 2h, then pour into the reaction vessel, put the reaction vessel into the atmosphere muffle furnace, open the high-purity nitrogen valve, maintain the flow rate at 2L / min, and heat up to After keeping at 200°C for 3 hours, raise the temperature to 300°C and keep for 6 hours, then raise the temperature to 400°C and keep for 12 hours, then lower the temperature in nitrogen atmosphere. A white powdery solid was obtained.

[0018] The white powder was placed in a long crucible, and the crucible was placed in a vacuum muffle furnace to evacuate, and then heated to 850°C for 2 hours. Obtain anhydrous lanthanum chloride crystal ingot.

[0019] Put the crystal ingot into the quartz ampoule bottle and vacuumize and se...

Embodiment 2

[0021] Embodiment 2: LaBr of purity 99.99% 3 preparation of

[0022] Weigh La with a purity of 99.999% 2 o 3 Sample 500g, NH with a purity higher than 99.9% 4 Br sample 2000g, add 500ml of distilled ethylene glycol, mix and stir with a planetary ball mill for 2h, then pour into the reaction vessel, put the reaction vessel into the atmosphere muffle furnace, open the high-purity nitrogen valve, maintain the flow rate at 2L / min, and heat up to After keeping at 200°C for 3 hours, raise the temperature to 300°C and keep for 6 hours, then raise the temperature to 500°C and keep for 12 hours, then lower the temperature in nitrogen atmosphere. A white powdery solid was obtained.

[0023] The white powder was placed in a long crucible, and the crucible was placed in a vacuum muffle furnace to evacuate, and then heated to 850°C for 2 hours. Obtain anhydrous lanthanum bromide crystal ingot.

[0024] Put the crystal ingot into the quartz ampoule bottle and vacuumize and seal it, th...

Embodiment 3

[0026] Embodiment 3: LuCl of purity 99.99% 3 preparation of

[0027] The operation is the same as that in Example 1, and the crystal forming ingot temperature is 950°C.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a method for preparing rare earth halides. The method comprises the following steps of: preparing rare earth halide powder, and performing zone-refining on the rare earth halide powder. The general formula of the rare earth halides is LnX3, wherein Ln is selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc or Y; and X is selected from Cl, Br or I. With the method, the content of oxyhalides and impurity metal ions can be reduced, the purity of the rare earth halides is increased, and the method is applicable to scale preparation.

Description

technical field [0001] The invention relates to a method for preparing high-purity rare earth halides, in particular to a preparation process for obtaining high-purity rare earth halides by using a zone smelting technique. Background technique [0002] High-purity anhydrous LnX 3 It is a very important chemical reagent, and has very important and broad application prospects in rare earth functional materials, such as LaCl 3 、LaBr 3 、LuCl 3 、LuBr 3 、LuI 3 , GdBr 3 etc. can be used to grow scintillation crystals, in which LaBr doped with cerium 3 and cerium-doped LaCl 3 Crystals have very excellent scintillation properties. It is the crystal with the best scintillation performance found so far. However, the disadvantage of this type of crystal is that the raw material LnX used for crystal growth 3 Strong hygroscopicity, hygroscopic raw materials will cause split tubes and crystal defects during crystal growth. High-purity anhydrous LnX 3 Preparation is the key tech...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 苏伟平洪茂椿阚剑吴少凡郑发鲲叶宁
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI