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Preparation method of spherical nanometer CeO2 polishing powder

A polishing powder and nanotechnology, applied in the field of nanomaterials, can solve the problems of unsuitability for industrial production and promotion, excessive heating time for gels, severe reaction conditions, etc., and achieves good polishing performance, short gel drying time, and ingredients. The effect of process simplification

Active Publication Date: 2017-04-26
SICHUAN UNIV
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Problems solved by technology

Patent CN101244837 discloses a kind of Ce(NO 3 )·6H 2 O and N, N dimethylacetamide (DMA) were used as raw materials to prepare nano-CeO with relatively uniform particles and high purity by combining hydrothermal method and solid-state reaction method. 2 , the hydrothermal reaction needs to be carried out at 150~180°C for 24~72 hours, the preparation cycle is too long, the efficiency is low, and the energy consumption is high
Patent CN102557103A discloses a nano-CeO with no obvious particle agglomeration and uniform particle size distribution prepared by microemulsion method 2 Particles, but a large amount of organic solvents and strong alkali solutions are used in the preparation process, which causes serious environmental pollution
Patent CN201210473426.X discloses a shape-controllable nano-CeO 2 The preparation method, the raw materials used are cerium nitrate hexahydrate, citric acid and ammonia water, by controlling the experimental conditions of the sol-gel method and the roasting temperature, nano-CeO with different shapes are prepared. 2 particles, this method suffers from the disadvantages common to the sol-gel method: excessive heating time is required to prepare the gel from the reaction solution
In addition, there are many preparation nano-CeO 2 Powder method, but these methods have the following problems to varying degrees: complex preparation process, high operation requirements, harsh reaction conditions and other shortcomings, not suitable for industrial production and promotion
In the patent CN105733445A, it is disclosed that a uniform and dispersed nano CeO 2 The method of polishing powder, which uses a fluorinating agent to refine the particle size of cerium oxide, uses stearic acid or ethylene glycol to gel the reactants, and this method can effectively obtain nano CeO 2 Polishing powder; however, there are many types of raw materials, and the batching process is more complicated. When ethylene glycol, which is difficult to volatilize, is added to the system as a complexing agent, the drying time is too long, and a pre-calcination step is required

Method used

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  • Preparation method of spherical nanometer CeO2 polishing powder
  • Preparation method of spherical nanometer CeO2 polishing powder
  • Preparation method of spherical nanometer CeO2 polishing powder

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0024] Weigh cerium chloride heptahydrate and anhydrous citric acid according to the molar ratio of cerium salt and citric acid as 1:1.5, place in a ball mill jar, add absolute ethanol as lubricant, and ball mill at room temperature for 2.5 hours in a planetary ball mill, Add absolute ethanol during ball milling so that the mixed powder is fully lubricated; the gel obtained from ball milling is placed in a drying oven, and dried at 70°C for 6 hours to form a xerogel; then the xerogel is placed in a muffle furnace and heated at 400 Thermally decompose at ℃ for 2 hours; then grind the powder obtained by thermal decomposition, wash with deionized water and ethanol three times respectively, put it into a drying oven, and dry it at 60°C; then put it in a muffle furnace, at 800 Calcined at ℃ for 1 hour; the final spherical nano-CeO 2 Polishing powder. The resulting CeO 2 Polishing powder is pure CeO 2 Phase, high crystallinity, average particle size is 40nm, particle size is very...

Embodiment 2

[0026] Weigh cerium nitrate hexahydrate and citric acid monohydrate according to the molar ratio of cerium salt to citric acid as 1:2, place them in a ball mill jar, add absolute ethanol as a lubricant, and ball mill at room temperature for 3 hours in a planetary ball mill. When adding absolute ethanol to make the mixed powder fully lubricated; the gel obtained by ball milling was placed in a drying oven and dried at 60°C for 8 hours to form a xerogel; then the xerogel was placed in a muffle furnace and heated at 500°C Thermally decompose for 1.5 hours; then grind the powder obtained by thermal decomposition, wash three times with deionized water and ethanol respectively, put it in a drying oven, and dry it at 60°C; then place it in a muffle furnace at 800°C Calcined for 1 hour; finally spherical nano-CeO 2 Polishing powder; resulting CeO 2 The average particle size of the polishing powder is 60nm, the primary particle size is within 10-20nm, the particle size is very uniform...

Embodiment 3

[0028] Weigh cerium nitrate hexahydrate and citric acid monohydrate according to the molar ratio of cerium salt to citric acid as 1:2, place them in a ball mill jar, add absolute ethanol as a lubricant, and ball mill at room temperature for 3 hours in a planetary ball mill. When adding absolute ethanol so that the mixed powder is fully lubricated; the gel obtained by ball milling is placed in a drying oven, and dried at 50°C for 10 hours to form a xerogel; then the xerogel is placed in a muffle furnace and heated at 600°C Thermally decompose for 1 hour; grind the powder obtained by thermal decomposition, wash with deionized water and ethanol three times respectively; then put it in a drying oven to dry at 70°C, and place it in a muffle furnace for calcination at 800°C for 1 hour; The final spherical nano-CeO 2 Polishing powder. The resulting CeO 2 The average particle size of the polishing powder is 70nm, the particle size is relatively uniform, and the dispersion is good. ...

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Abstract

The invention discloses a preparation method of spherical nanometer CeO2 polishing powder and belongs to the field of nanometer material research. The preparation method utilizes a crystal water-containing cerium salt and citric acid as raw materials, a proper amount of ethanol as a lubricant and the ball milling mechanical force to refine the raw materials so that reaction efficiency is improved. Crystal water released by the raw materials and the lubricant ethanol form a liquid film and precursor gel is directly prepared so that a ball milling solid-phase chemical reaction method and a sol-gel method are combined. The gel can effectively inhibit the agglomeration and growth of cerium oxide particles in later calcination processes so that the pherical nanometer CeO2 polishing powder with uniform particle sizes, good dispersibility and good polishability are prepared. The pherical nanometer CeO2 polishing powder has uniform particle sizes, good dispersibility and good polishability. The preparation method has the advantages of simple processes, high efficiency, no pollution and good reproducibility, and is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the field of nano-material research, in particular to a spherical nano-CeO with uniform particle size and good dispersion 2 Preparation method of polishing powder. Background technique [0002] Since the 1940s, people began to use rare earth polishing powder to polish optical glass. Compared with the iron oxide polishing powder used earlier, the polishing efficiency of the rare earth polishing powder is doubled. Common glass polishing powders are mostly trivalent and tetravalent metal oxides, such as iron, aluminum, cerium, titanium, zirconium, thorium and chromium. Cerium-based rare earth polishing powder is known as the best polishing material. It is widely used in polishing the surface of materials to improve the surface smoothness of materials. It has the advantages of moderate hardness, high efficiency and long service life. With the continuous and rapid development of science and technology, some special polishing fiel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C09G1/02
CPCC01F17/206C01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/64C09G1/02
Inventor 朱达川周川
Owner SICHUAN UNIV
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