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High pure anhydrous composite rare earth halide and preparation method thereof

A technology for compounding rare earth and halide, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problem of uneven distribution of impurity content activator, and achieve easy mass production, simple operation and high purity. Effect

Active Publication Date: 2017-05-31
GRIREM ADVANCED MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second object of the present invention is to provide the high-purity anhydrous composite rare earth halide obtained by the above preparation method, which effectively overcomes the phase segregation, high impurity content, and activator distribution in the prior art. Inhomogeneity and other defects can fully meet the preparation needs of scintillation crystals, ceramics or thin film materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: Accurately weigh 325.8g Cs 2 CO 3 (99.99%), 36.9g Li 2 CO 3 (99.99%), 112.9g Y 2 o 3 (99.99%), 107.0 g NH 4 Cl (99.9%) was co-dissolved in hydrochloric acid to obtain a mixed clear solution, which was concentrated at 120°C until the material contained no liquid water. After cooling, a blocky solid was obtained. Crush the blocky solid and put it in a quartz dehydration tube, then put it into a tube furnace for dehydration. The dehydration temperature was slowly raised from room temperature to 230°C and kept for 5 hours at a rate of 5°C / h. During this period, a water ring pump was used to evacuate, and the vacuum degree was about 2400Pa. After dehydration, the material was burned at 450°C for 8 hours under the condition of high-purity Ar gas, and the remaining product was Cs 2 LiYCl 6 . The water content was detected to be 12ppm, and the oxygen content was 56ppm.

Embodiment 2

[0022] Embodiment 2: Accurately weigh 325.8g Cs 2 CO 3 (99.99%), 36.9g Li 2 CO 3 (99.99%), 107.3g Y 2 o 3 (99.99%), 11.5g Ce 2 (CO 3 ) 3 (99.99%), 53.5g NH 4 Cl (99.9%) was co-dissolved in hydrochloric acid to obtain a mixed clear solution, which was concentrated at 120°C until the material contained no liquid water. After cooling, a blocky solid was obtained. Crush the blocky solid and put it in a quartz dehydration tube, then put it into a tube furnace for dehydration. The dehydration temperature was slowly raised from room temperature to 200°C and kept for 10 hours at a rate of 8°C / h. During this period, a water ring pump was used to draw a vacuum with a vacuum degree of about 2200Pa. After dehydration, the material is in high-purity N 2 Burning at 550°C for 4h under atmospheric conditions, the remaining product is Cs 2 Li Y 0.95 Ce 0.05 Cl 6 . The water content was detected to be 10ppm, and the oxygen content was 72ppm.

Embodiment 3

[0023] Embodiment 3: Accurately weigh 325.8g Cs 2 CO 3 (99.99%), 36.9g Li 2 CO 3 (99.99%), 112.9g Y 2 o 3 (99.99%), 293.9 g NH 4 Br (99.9%) was co-dissolved in hydrobromic acid to obtain a mixed clear solution, which was concentrated at 150°C until the material contained no liquid water. After cooling, a blocky solid was obtained. Crush the blocky solid and put it in a quartz dehydration tube, then put it into a tube furnace for dehydration. The dehydration temperature was slowly raised from room temperature to 220°C and kept for 48 hours at a rate of 30°C / h. During this period, a water ring pump was used to draw a vacuum with a vacuum degree of about 3000Pa. After dehydration, the material was burned at 500°C for 10 hours under the condition of high-purity Ar gas, and the remaining product was Cs 2 wxya 6 . Its water content was detected to be 11ppm, and the oxygen content was 32ppm.

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Abstract

The invention relates to a method for preparing a high pure anhydrous composite rare earth halide. The composite rare earth halide has a general formula of A2BMX6, wherein A represents Rb or Cs, B represents Li or Na, M represents one or two of rare earth elements of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc and Y, and X represents one of halogen elements of Cl, Br and I. The method comprises (1) preparing a mixed solution, (2) concentrating the mixed solution, (3) dehydrating the mixed solution and (4) removing ammonium, wherein in the step (1), ammonium halide NH4X is used as a dehydrating agent. In addition, the invention also provides the high pure anhydrous composite rare earth halide obtained by the method. The high pure anhydrous composite rare earth halide does not contain crystal water and oxide impurities, has high purity and good uniformity, and can meet the application requirements of scintillating crystals and scintillating ceramics.

Description

technical field [0001] The invention belongs to the field of luminescent materials, in particular to inorganic scintillation materials, and more specifically to a high-purity anhydrous composite rare earth halide and a preparation method thereof. Background technique [0002] Scintillation materials are a class of materials that emit ultraviolet or visible photons after absorbing the energy of high-energy rays or particles. It can be used for the detection of high-energy rays such as α-rays, γ-rays, and X-rays, and high-energy particles such as neutrons. It is widely used in nuclear medicine, high-energy physics, safety inspection, industrial non-destructive testing, space physics, and nuclear prospecting. They are usually used in the form of single crystals, but also in some cases glass, ceramic or other forms. [0003] Ce 3+ Activated complex rare earth halide scintillation materials (such as Cs 2 LiYCl 6 : Ce 3+ ) has attracted widespread attention, and has a good ap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 余金秋彭鹏刁成鹏吴浩刘荣辉何华强胡运生
Owner GRIREM ADVANCED MATERIALS CO LTD
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