Method for preparing rare earth oxides

A rare earth oxysulfide, rare earth technology, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problem that rare earth oxysulfide cannot be directly prepared

Inactive Publication Date: 2010-08-25
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, according to the above methods, it is impossible to di

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preparation example Construction

[0023] The embodiment of the present invention discloses a preparation method of spherical sulfur oxide, comprising:

[0024] a, after mixing the rare earth salt solution and PVP, dissolve it with an organic solvent to obtain the first reaction solution;

[0025] b. Obtaining the second reaction solution after dissolving thiourea with an organic solvent;

[0026] c. After mixing the first reaction solution and the second reaction solution, heating, and constant temperature reaction to obtain the precursor;

[0027] d. Spherical rare earth sulfur oxides obtained by calcining the precursor in a sulfur-containing atmosphere.

[0028] According to the present invention, the rare earth salt solution is a rare earth nitrate solution and / or a rare earth chloride solution, and the rare earth in the rare earth salt solution is lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium ( Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), er...

Embodiment 1

[0033] 1. Take 40mL of 0.5mol / L Gd(NO 3 ) 3 solution and mix it with 20g of PVP, add the mixed solution into the mixed solution of 150mL ethanol and 100mL ethylene glycol, and stir until the PVP is completely dissolved to obtain the first reaction solution.

[0034] 2. Dissolve 1.1 g of thiourea in a mixed solution of 50 mL of ethanol and 50 mL of ethylene glycol to obtain a second reaction solution.

[0035] 3. Add the second reaction solution dropwise to the first reaction solution, stir evenly, transfer to an autoclave, and react at a constant temperature at 210°C for 24 hours to obtain a reaction product, mix the reaction product with ethanol and transfer to a centrifuge for centrifugation Separated to obtain the precursor.

[0036] 4. Put the precursor at 700℃ in N 2 After calcination in / S atmosphere for 2 hours, the calcined product was cooled to room temperature to obtain spherical Gd 2 o 2 S.

[0037] see figure 1 Gd prepared for this example 2 o 2 SX-ray dif...

Embodiment 2

[0039] 1. Take 39mL of 0.5mol / L Gd(NO 3 ) 3 solution, 10mL 0.05mol / L Eu(NO 3 ) 3 solution, the weighed Gd(NO 3 ) 3 solution and Eu(NO 3 ) 3 After the solution was mixed with 20g of PVP, 250mL of ethylene glycol was added, and stirred until all the PVP was dissolved to obtain the first reaction solution.

[0040] 2. Dissolve 1.1 g of thiourea in 100 mL of ethylene glycol to obtain a second reaction solution.

[0041] 3. Add the second reaction solution dropwise to the first reaction solution, stir evenly, transfer to an autoclave, and react at a constant temperature at 200°C for 24 hours to obtain a reaction product, mix the reaction product with ethanol and transfer to a centrifuge for centrifugation Separated to obtain the precursor.

[0042] 4. Put the precursor at 700℃ in ℃S 2 After calcination in the atmosphere for 2 hours, the calcined product was cooled to room temperature to obtain spherical Gd 1.95 Eu 0.05 o 2 S.

[0043] see image 3 Gd prepared for this...

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Abstract

The invention provides a method for preparing rare earth oxides, which comprises: mixing solution of rare earth salts and polyvinylpyrrolidone, and dissolving the mixture in an organic solvent to obtain first reaction solution, wherein the solution of the rare earth salts is solution of rare earth nitrates and/or rare earth chlorides and the solution of the rare earth salts may contain one or two of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium and yttrium; dissolving thiourea in an organic solvent to obtain second reaction solution; mixing the first reaction solution and the second reaction solution, heating the mixed reaction solution, and allowing the mixed solution to react at a constant temperature to obtain a precursor; and calcining the precursor in sulfur-containing atmosphere to obtain spherical rare earth oxides. The rare earth oxides prepared by the method have a spherical shape, and therefore, materials prepared by using the rare earth oxides have remarkable luminous effect.

Description

technical field [0001] The invention relates to the field of rare earth luminescent materials, in particular to a preparation method of rare earth sulfur oxides. Background technique [0002] Rare earth sulfide has high chemical stability and wide bandgap of 4.6eV-4.8eV. It has high luminous efficiency as a luminescent matrix and is an important class of optical functional materials. High-performance luminescent materials can be prepared by doping active ions in rare earth sulfur oxides, so they are widely used in technical fields such as radiation-enhanced display materials, fluorescent picture tube materials, X-ray tomography, and jet shock heat transfer measurement. [0003] The preparation method of existing rare earth sulfide is following several: (1) utilize H 2 Or CO reduction of rare earth sulfate (Pitha J.J., Smith A.L.and Ward R., J.Am.Chem.Soc., 1947, 69, 1870); (2) CO reduction of rare earth sulfite (Koskenlinna M., Leskela M , and Niinisto L, J.Electrochem.Soc...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82B3/00
Inventor 尤洪鹏宋艳华洪广言
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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