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Method for preparing ultra-high-purity volatile rare earth cerium chelate

A chelate, high-purity technology, applied in the field of CVD, can solve the problems of difficult separation and purification, low yield, and difficulty in preparing β-diketone rare earth cerium, so as to improve purity, high yield, control the introduction of impurities and side effects The effect of the reaction

Active Publication Date: 2020-06-16
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Rare earth cerium (Ce) has III, IV valence states, and compounds of IV valence cerium (CeO 2 、Ce(OH) 4 ) has insoluble characteristics, which brings certain difficulties to the preparation of β-diketone rare earth cerium (IV) chelate, resulting in many by-products and lower yield
A variety of reagents and raw materials are used in the preparation process of chelates, and the metal impurity elements contained in them will generate various metal chelates during the preparation process. These chelates have similar properties and many types, and subsequent separation and purification are difficult, making There are many impurities in the target chelate, and it is difficult to obtain higher purity (≥5N); materials with low-level purity (<5N) do not meet the requirements of chemical vapor deposition (CVD) for high-purity materials

Method used

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  • Method for preparing ultra-high-purity volatile rare earth cerium chelate
  • Method for preparing ultra-high-purity volatile rare earth cerium chelate
  • Method for preparing ultra-high-purity volatile rare earth cerium chelate

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Embodiment

[0047] Rare earth cerium raw material processing:

[0048] The purity of Ce(NO 3 ) 3 Raw materials are processed by ion exchange method to obtain high purity CeO 2 Raw material (relative purity> 5N), the ICP-MS analysis results of the treated cerium raw materials are as follows:

[0049]

[0050]

[0051] Dione ligand treatment:

[0052] Take the commercially available analytically pure 2,2,6,6-tetramethyl-3,5-heptanedione for distillation, collect the middle distillate, the color of the obtained ligand is colorless, GC-MS analysis, after processing 2, 2,6,6-Tetramethyl-3,5-heptanedione content> 99%, ICP-MS analysis showed that the content of Fe in the ligand was reduced from 154.9ppb to 60ppb, and the content of Mg was reduced from 137ppb to <10ppb.

[0053] Preparation of high purity cerium chelate (tetramethyl-2,2,6,6-tetramethyl-3,5-heptanedione cerium chelate) 1:

[0054] ①Take 7.45g of CeO obtained after treatment 2 In the beaker, then add 1M treated HNO 3 10ml, stir overnight an...

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Abstract

The invention discloses a method for preparing ultrahigh-purity volatile rare earth cerium chelate. The method includes the steps of conducting high-purity treatment with one or more of rare earth cerate, rare earth cerium oxide and metal cerium as the raw materials to obtain high-purity rare earth cerium oxide or metal cerium, making the high-purity rare earth cerium oxide or / and metal cerium react with a reaction reagent to generate III-valence-state rare earth cerate, and making the generated III-valence-state rare earth cerate subjected to a chelating reaction with a chelating ligand to prepare the rare earth cerium chelate. The rare earth cerium (IV) chelate with the relative purity larger than or equal to 5N(99.999%) can be prepared through the method.

Description

Technical field [0001] The present invention relates to the field of CVD technology, in particular to a method for preparing ultra-high-purity volatile rare earth cerium chelate that can be used in the field of high-purity rare earth materials for doping in the preparation of laser optical fibers. Background technique [0002] Chemical vapor deposition (CVD) is an important material and coating preparation technology. It is widely used in the fields of semiconductors, solar cells, optical materials and devices. The raw material required for this technology application is volatile organic metals ( MO); β-diketone rare earth chelate has good stability and relatively easy volatilization, and can be used as an important MO source for chemical vapor deposition technology to achieve rare earth element doping or to prepare rare earth element-containing functional coatings Layers, materials and devices; among these rare earth chelates, 2,2,6,6-tetramethyl-3,5-heptanedione rare earth chel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00C07C45/77C07C49/12
CPCC07C45/77C07F5/003C07C49/12
Inventor 焦鹏冲居佳蔡华强向恒
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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