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Preparation method of cerium-doped rare earth silicate polycrystalline powder

A rare earth silicate, polycrystalline powder technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of complex operation process, affecting the performance of lutetium silicate crystal material such as light output, long reaction period, etc. Simple process flow, low cost and uniform distribution of elements

Active Publication Date: 2018-04-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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Problems solved by technology

Although the above methods have realized Lu 2 SiO 5 : The controllable morphology preparation of Ce precursor, but the use of organic solvents in the preparation process is easy to introduce impurity elements, the operation process is complicated, and the reaction cycle is long, which affects the light output and other properties of the subsequent lutetium silicate crystal material

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  • Preparation method of cerium-doped rare earth silicate polycrystalline powder
  • Preparation method of cerium-doped rare earth silicate polycrystalline powder

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preparation example Construction

[0024] The preparation method of the cerium-doped rare earth silicate polycrystalline powder provided by the present invention specifically comprises the following steps:

[0025] The chemical formula of the cerium-doped rare earth silicate polycrystalline powder is RE 2(1-x) SiO 5 : Ce 2x , where x=0.5‰-2%, RE is one or two of Y, Gd, Lu;

[0026] Step 1. Weigh one or both of cerium nitrate, yttrium nitrate, gadolinium nitrate and lutetium nitrate according to the molar ratio of the rare earth element in the above chemical formula, and mix and stir the weighed rare earth nitrate solution to obtain the first solution;

[0027] Step 2, weighing sodium metasilicate according to the molar ratio of rare earth element and silicon element in the above chemical formula, and mixing and stirring the weighed sodium metasilicate with ammonia water or ammonium carbonate solution to obtain a second solution;

[0028] Step 3. Under the condition of magnetic stirring, slowly add the first...

Embodiment 1

[0030] Example 1: Y 2 SiO 5 :1‰Ce polycrystalline powder preparation

[0031] According to the proportion of cerium in the total rare earth is 1‰, the total rare earth is 0.012mol yttrium nitrate solution and cerium nitrate solution are mixed uniformly; 0.006mol sodium metasilicate solution and 0.024mol ammonia solution are stirred uniformly; under magnetic stirring conditions, the The above mixed rare earth solution was slowly added dropwise to the mixed solution of sodium metasilicate and ammonia water, stirred for 2 hours, and aged overnight to obtain mixed precipitates of rare earth-containing colloidal silica and rare earth hydroxides, which were separated with deionized water and absolute ethanol Washing; first dry the mixed precipitate at 70°C for 24h, then in N 2 / H 2 Calcined at 1300°C for 2h in a mixed atmosphere (volume ratio 9:1) to obtain Y 2 SiO 5 :1‰Ce polycrystalline powder.

Embodiment 2

[0032] Example 2: Y 2 SiO 5 : Preparation of 1% Ce polycrystalline powder

[0033] According to cerium accounting for 1% of the total rare earth ratio, the total rare earth is 0.012mol yttrium nitrate solution and cerium nitrate solution are mixed uniformly; 0.006mol sodium metasilicate solution and 0.024mol ammonia solution are stirred uniformly; under magnetic stirring conditions, the The above mixed rare earth solution was slowly added dropwise to the mixed solution of sodium metasilicate and ammonia water, stirred for 2 hours, and aged overnight to obtain mixed precipitates of rare earth-containing colloidal silica and rare earth hydroxides, which were separated with deionized water and absolute ethanol Washing; first dry the mixed precipitate at 70°C for 24h, then in N2 / H 2 Calcined at 1300°C for 2h in a mixed atmosphere (volume ratio 9:1) to obtain Y 2 SiO 5 : 1% Ce polycrystalline powder.

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Abstract

The present invention provides a preparation method of a cerium-doped rare earth silicate polycrystalline powder, and belongs to the technical field of preparation technologies of a rare-earth compound luminescent powder. The preparation method solves the technical problems that in the preparation process of an existing cerium-doped rare earth silicate polycrystalline powder, organic solvents areused, impurity elements are easy to introduce, the operation process is complicated, the reaction period is long, and the performance, such as light output, of a subsequent lutetium silicate crystal material is affected. According to the preparation method for the cerium-doped rare earth silicate polycrystalline powder provided by the present invention, sodium metasilicate is employed as a siliconsource, ammonia water or ammonium carbonate is taken as a precipitating agent, homogeneous co-precipitation is carried out for obtaining a mixed rare earth silica gel and a precipitation precursor, and finally calcination is carried out, so that the cerium-doped rare earth silicate polycrystalline powder is obtained. The method adopts a liquid phase co-precipitation process to prepare the pure-phase polycrystalline powder, the elements are uniformly distributed, no aggregation phenomenon is caused, no other organic reagents are introduced, introduction of impurity elements is reduced, the process flow is simple, consumption of chemical raw materials is low, the cost is low, and the method is easy to control and amplify.

Description

technical field [0001] The invention relates to the technical field of rare earth compound luminescent powder preparation technology, in particular to a preparation method of cerium-doped rare earth silicate polycrystalline powder. Background technique [0002] Rare earth silicates (RE 2 SiO 5 :Ce(RE=Y,Gd,Lu)) scintillation crystals are widely used in the fields of high energy physics, nuclear physics, nuclear medicine and safety detection due to their excellent properties such as high light output and short decay time, especially Yttrium-lutetium silicate scintillation crystals have become an indispensable key component in positron emission tomography (PET-CT). The study of cerium-doped rare earth silicate scintillation crystals has become a hot field. In 1990, the U.S. Patent (Patent No.: 4958050) disclosed Lu 2 SiO 5 : Preparation method of Ce scintillation crystal, Chinese patent (patent number: 200480039681.7) and PCT patent (application number: WO 2005 / 042812 A1) d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/79
CPCC09K11/7774
Inventor 陈继邓岳锋李德谦杨桐常永青李海连刘郁
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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