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Superfine and spheroidizing rare-earth polish and preparing process thereof

A rare earth polishing powder and preparation process technology, applied in other chemical processes, chemical instruments and methods, etc., can solve the problems of polishing powder with good reusability, poor polishing effect, poor reusability, etc., and achieve good polishing effect, The effect of fine powder particle size and easy operation

Active Publication Date: 2008-10-15
GRIREM ADVANCED MATERIALS CO LTD
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Problems solved by technology

U.S. Patent 5543216 discloses a preparation method for synthesizing cerium oxide particles. The method adjusts the pH value of the reactant to 8-9, and raises the temperature to 100-200°C under pressure. The particle size obtained is between 0.03-5um. This method is more complicated, the equipment is expensive, the particle size distribution is wide, and the polishing effect is not good
[0005] Chinese patent CN1821314 discloses a preparation method of ultrafine cerium oxide, which uses a salt solution containing cerium ions, and after adding a surfactant, the solution is first contacted with an alkaline substance to control the pH value of the reaction suspension to form a precipitate Then the suspension is converted with oxalic acid to control the pH value at the end of the reaction. Finally, the precipitate is filtered, washed, dried, and burned at 600-1000°C. The obtained ultra-fine cerium oxide can be used for polishing, but this method The preparation steps are also relatively complicated, and the particle size distribution of the prepared product is also relatively wide between 10nm and 30um, and the specific surface area reaches 50m 2 / g, it has poor reusability as a polishing powder
[0006] The preparation steps in the method disclosed in Chinese patent 200510132522.8 are also relatively complicated, and the particle size distribution of the prepared product is also relatively wide, between 10nm and 30um, and the specific surface area reaches 50m 2 / g, when it is used as polishing powder, the reusability is poor
[0007] At present, the average particle size of polishing powder is between 0.02-2.0um, 02 / g, 0<dispersion degree σ<1.5, good spheroidization, high cutting force, and good reusability The preparation method of polishing powder has not been reported

Method used

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Examples

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example 1

[0038] Example 1: Dissolve cerium chloride in water to make a 0.05 mol / L solution into a reactor, and heat it to 30°C. Add the prepared precipitant ammonium bicarbonate solution with a concentration of 0.1mol / L to the bottom solution at a rate of 2L / min; after the addition is completed, stir for 10 minutes, and add the ammonium ion at a concentration of 0.01 The weight percentage of mol / L ammonium chloride and F / TREO is 0.1% ammonium fluoride in the mixed solution; Mixed mother liquor is heated up to 90 ℃ and continues stirring reaction for 5 hours, makes reaction fully carry out, and obtains precipitation; Will obtain The precipitate was aged at 30°C for 0.5 hours; the precipitate was separated, collected, washed, and dried to obtain a white precursor powder, which was calcined at 600°C to obtain CeO 2 The powder is passed through a 200-mesh sieve after wet ball milling, and then centrifugally dried to obtain a high-performance ultrafine, spheroidized rare earth polishing pow...

example 2

[0039]Example 2: Dissolve lanthanum and cerium nitrate in water to form a 3 mol / L solution, put it into a reactor, and heat it to 80°C. Add the prepared precipitant ammonium carbonate solution with a concentration of 2.0mol / L into the base solution at a rate of 2L / min; after the addition is completed, stir for 10min, and add ammonium ions at a concentration of 1.0mol when calculated according to the volume of the mother liquor The weight percentage of / L ammonium nitrate and F / TREO is 10.0% ammonium fluoride in the mixed solution; the mixed mother liquor is heated up to 90 ° C, and the stirring reaction is continued for 5 hours, so that the reaction is fully carried out, and precipitation is obtained; the obtained precipitation Aged at 100°C for 48 hours; the precipitate was separated, collected, washed, and dried to obtain a white precursor powder, which was calcined at 1100°C to obtain La 2 o 3 -CeO 2 The powder is passed through a 500-mesh sieve after wet ball milling, an...

example 3

[0040] Example 3: Dissolve lanthanum, cerium, praseodymium, and neodymium sulfate in water to form a 1.5 mol / L solution in a reactor, and heat it to 40°C. Add the mixed solution of precipitant ammonium bicarbonate and ammonia water with a concentration of 1.0mol / L to the bottom solution at a rate of 2L / min; after the addition is completed, stir for 15min, and add ammonium ions when calculated according to the volume of the mother solution The concentration of 0.5mol / L ammonium sulfate and the weight percent of F / TREO are 1.0% ammonium fluorosilicate in the mixed solution; the mixed mother liquor is heated to 80 ° C, and the reaction is continued for 5 hours with stirring, so that the reaction is fully carried out, and obtained Precipitate; age the obtained precipitate at 60°C for 24 hours; separate, collect, wash, and dry the precipitate to obtain a white precursor powder, which is calcined at 900°C to obtain a mixed powder, which is wet ball milled After passing through a 400...

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Abstract

The invention provides ultrafine spheroidized rare earth polishing powder and a process for making the same. The process comprises the following steps that: one of or the mixture of ammonia water, ammonium bicarbonate and ammonium carbonate is used as precipitant; ammonium salt and fluoride ions are added into precipitated slurry to adjust the ionic strength in mother liquid, so as to increase the surface electrical property of solid particles in the slurry; after high temperature aging, the ultrafine rare earth polishing powder with good dispersity and high spheroidization degree can be obtained by filtering the slurry, drying, burning, ball-milling and sieving filter cakes. The average particle size of the obtained polishing powder is between 0.02 mu m and 2.0 mu m, wherein the specific surface area BET is more than 0 and less than 10 m<2> / g, and the powder is in a well-dispersed spherical shape. The powder is used for polishing optical glass, crystal, display screens, etc., strong in cutting force, few in scratch and long in service time.

Description

technical field [0001] The invention relates to an ultrafine, spheroidized rare earth polishing powder and a preparation process thereof, and belongs to the technical field of chemical preparation of rare earth powder materials. Background technique [0002] Rare earth polishing powder is mainly used for polishing glass, crystal and other products. Rare earth polishing powder is mainly cerium-based oxide powder. According to the content of cerium oxide, it can be divided into high cerium polishing powder, medium cerium polishing powder and low cerium polishing powder. At present, there are many low-grade polishing powders produced in China, and there is still some gap in the production of higher-grade rare earth polishing powders compared with foreign countries, and it is still necessary to rely on imported polishing powders for the polishing of devices with high requirements. Many countries produce high-performance polishing powder, but it still cannot meet the growing dome...

Claims

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Application Information

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IPC IPC(8): C09K3/14
Inventor 朱兆武韩业斌龙志奇黄小卫崔大立张顺利崔梅生
Owner GRIREM ADVANCED MATERIALS CO LTD
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