Preparation method of rare-earth doped nanometer spherical CePo4 material

A rare earth doping and nano-technology, which is applied in the field of preparation of hexagonal nano-spherical CePO4 particle materials, can solve problems such as low friction coefficient, and achieve the effects of simple preparation method, energy saving and simple equipment

Inactive Publication Date: 2012-12-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Among materials with different morphologies, spherical particle materials have important application value in various fields due to their low frictio

Method used

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  • Preparation method of rare-earth doped nanometer spherical CePo4 material
  • Preparation method of rare-earth doped nanometer spherical CePo4 material

Examples

Experimental program
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Embodiment 1

[0026] Weigh commercially available spectrally pure cerium sulfate tetrahydrate (Ce(SO 4 ) 2 4H 2 O) Reagent 101.075g (0.25mol), is mixed with 0.25 mol / liter of Ce(SO 4 ) 2 solution. Take by weighing the concentrated phosphoric acid 230.6g (containing 2mol H 3 PO 4 ), prepared as 2 mol / L H 3 PO 4 solution. Measure 10mL of Ce(SO 4 ) 2 Solution, according to absolute ethanol / Ce(SO 4 ) 2 The solution volume ratio is 7:1, Ce 4+ / polyoxyethylene ether-polyoxypropylene ether-polyoxyethylene ether triblock copolymer (P123, 5800) proportioning is 0.0005mol:1g, takes by weighing 55g dehydrated alcohol and 5g P123 respectively, joins Ce(SO 4 ) 2 solution and mix well. Press PO 4 3- / C 4+ =1:1 (molar ratio), measure 1.25mL of H with a concentration of 2 mol / L 3 PO 4 Solution, added to the above mixed solution at a rate of 0.1mL / min under stirring conditions to generate a cerium phosphate mesophase precursor, continue to stir for 2h after the dropwise addition, and the...

Embodiment 2

[0028] Using the same steps as in Example 1, the prepared concentration is 0.25 mol / liter of Ce(SO 4 ) 2 solution and 2 mol / L H 3 PO 4 solution. Measure 13mL of Ce(SO 4 ) 2 Solution, according to absolute ethanol / Ce(SO 4 ) 2 The solution volume ratio is 5:1, Ce 4+ / polyoxyethylene ether-polyoxypropylene ether-polyoxyethylene ether triblock copolymer (P123, 5800) proportioning is 0.0005mol:1g, takes by weighing 51g dehydrated alcohol and 6.5g P123 respectively, joins Ce(SO 4 ) 2 solution and mix well. Press PO 4 3- / C 4+ =1:1 (molar ratio), measure 1.625mL of H with a concentration of 2 mol / L 3 PO 4 Solution, under stirring condition, join in the above-mentioned mixed solution with the drop speed of 0.1mL / min, generate cerium phosphate mesophase precursor, all the other steps are identical with embodiment 1, obtain white hexagonal crystal phase nano-spherical CePO 4 particles. The product was characterized by XRD as hexagonal CePO 4 Pure phase, the product obta...

Embodiment 3

[0030] Using the same steps as in Example 1, the prepared concentration is 0.25 mol / liter of Ce(SO 4 ) 2 solution and 2 mol / L H 3 PO 4 solution. Measure 16mL of Ce(SO 4 ) 2 Solution, according to absolute ethanol / Ce(SO 4 ) 2 The solution volume ratio is 4:1, Ce 4+ / polyoxyethylene ether-polyoxypropylene ether-polyoxyethylene ether triblock copolymer (P123, 5800) proportioning is 0.0005mol:1g, takes by weighing 50g dehydrated alcohol and 8g P123 respectively and joins Ce(SO 4 ) 2 solution and mix well. Press PO 4 3- / C 4+ =1:1 (molar ratio), measure 2.0 mL of H with a concentration of 2 mol / L 3 PO 4 Solution, under stirring condition, join in the above-mentioned mixed solution with the drop speed of 0.1mL / min, generate cerium phosphate mesophase precursor, all the other steps are identical with embodiment 1, obtain white hexagonal crystal phase nano-spherical CePO 4 particles. The product was characterized by XRD as hexagonal CePO 4 Pure phase, the product obta...

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Abstract

The invention aims to provide a hexagonal crystal phase nanometer spherical CePO4 granular material with regular morphology, high crystal phase purity and obvious light-emitting performances and a preparation method of a rare-earth doped hexagonal crystal phase nanometer spherical CePO4 granular material serving as an activating agent. The hexagonal crystal phase nanometer spherical CePO4 granular material is characterized by being synthesized by regarding quadrivalent cerium salts as a cerium source and adopting a solvent thermal crystallization method. The preparation method comprises the steps of precipitation, crystallization, washing and drying, to be specific: mixing quadrivalent cerium salts with rare-earth ion solution serving as an activating agent; adding a water-soluble organic alcohol and/or water-soluble polymer and mixing uniformly; adding a phosphoric acid or phosphate precipitator solution to generate cerous phosphate and the activating agent rare-earth doped cerous phosphate intermediate phase precursor; and then sealing the cerous phosphate and the activating agent rare-earth doped cerous phosphate intermediate phase precursor into a kettle for a solvent thermal crystallization reaction so as to prepare the hexagonal crystal phase nanometer spherical CePO4 and rare-earth doped CePO4 particles. According to the invention, addition amounts of the water-soluble organic alcohol and the water-soluble polymer in a solvent heat system are changed, and the particle size of the product can be controlled.

Description

technical field [0001] The invention belongs to the field of nano-rare earth phosphate materials, and provides a nano-spherical CePO with a hexagonal crystal structure 4 Hexagonal Nanospherical CePO Doped with Particle Material and Activator Rare Earth 4 Process for the preparation of granular materials. The characteristic is to use tetravalent cerium salt as the cerium source, phosphoric acid or phosphate as the precipitating agent, and use water-water-soluble organic alcohol and / or water-water-soluble polymer system for solvothermal crystallization reaction to prepare hexagonal nano-spherical CePO 4 particles. The particle size of the product can be controlled by changing the addition amount of water-soluble organic alcohol and water-soluble polymer in the solvothermal system. Background technique [0002] As human science continues to explore the two directions of the macrocosm and the microcosm, the nanoworld between the microcosm and the macrocosm has gradually beco...

Claims

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Application Information

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IPC IPC(8): C09K11/81B82Y30/00B82Y40/00
Inventor 杨儒秦杰李敏
Owner BEIJING UNIV OF CHEM TECH
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