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Fluorine doping method of cerium-based rare earth polishing powder

A rare earth polishing powder, cerium-based technology, applied in the fluorine-doped field of cerium-based rare earth polishing powder, can solve the problems affecting the polishing rate and precision of rare earth polishing powder, affecting the crystal structure of the final product, and difficult to control the particle size and particle size distribution. The particle size and particle size distribution are easy to control, the polishing accuracy is easy, and the polishing accuracy is controlled

Inactive Publication Date: 2015-03-18
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both of these methods are likely to cause uneven fluorination and affect the crystal structure of the final product
At the same time, whether it is pre-fluorination or post-fluorination, two precipitation processes are involved, and the particle size and particle size distribution are difficult to control
The defects of the two fluorine doping methods have seriously affected the polishing rate and precision of rare earth polishing powder, limiting its application in liquid crystal screens, semiconductor silicon wafers and other fields

Method used

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  • Fluorine doping method of cerium-based rare earth polishing powder
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  • Fluorine doping method of cerium-based rare earth polishing powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Prepare 2.0mol / L lanthanum cerium chloride solution, 2.5mol / L ammonium carbonate solution and 1.0mol / L fluosilicic acid solution respectively. In the state of continuous stirring, the above-mentioned raw material solution is continuously added into the reaction kettle in parallel. Adjust the flow rate of the fluosilicic acid solution, control the F / TREO to 5%, adjust the flow rate of the ammonium carbonate solution, control the pH of the reaction system to 8.50±0.05, and control the temperature of the reactor to 40°C. After the reaction was completed, it was aged for 1 h. The aged slurry is filtered, washed, and dried at 90° C. to obtain a polishing powder precursor.

[0025] The prepared polishing powder precursor was calcined at 900° C. for 3 h to obtain the finished polishing powder. Particle size analysis, scanning electron microscope analysis and XRD analysis were carried out on the sample, and the analysis results were as follows: Figure 1~3 As shown, the part...

Embodiment 2

[0027] Prepare 1.5 mol / L lanthanum cerium neodymium chloride solution, 2.0 mol / L ammonium bicarbonate solution and 0.5 mol / L ammonium fluoride solution respectively. Under the condition of continuous stirring, the above-mentioned raw material solution is continuously added into the reactor in parallel flow. Adjust the flow rate of ammonium fluoride solution, control the F / TREO to 6%, adjust the flow rate of ammonium carbonate, control the pH of the reaction system to 8.00±0.05, and control the temperature of the reaction kettle to 50°C. After the reaction was completed, it was aged for 1 h. The aged slurry is filtered, washed, and dried at 90° C. to obtain a polishing powder precursor.

[0028] The prepared polishing powder precursor was calcined at 950° C. for 2 h to obtain the finished polishing powder. The particle size of the sample D50 = 0.857 μm.

Embodiment 3

[0030] Prepare 2.5mol / L lanthanum cerium nitrate solution, 4.0mol / L sodium hydroxide solution and 1.5mol / L hydrofluoric acid solution respectively. Under the condition of continuous stirring, the above-mentioned raw material solution is continuously added into the reactor in parallel flow. Adjust the flow rate of ammonium fluoride solution, control the F / TREO to 6.5%, adjust the flow rate of sodium hydroxide, control the pH of the reaction system to 9.00±0.05, and control the temperature of the reaction kettle to 55°C. After the reaction was completed, it was aged for 1.5h. The aged slurry is filtered, washed, and dried at 90° C. to obtain a polishing powder precursor.

[0031] The prepared polishing powder precursor was calcined at 1000° C. for 2 h to obtain the finished polishing powder. The particle size of the sample D50 = 1.235 μm.

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Abstract

The invention discloses a fluorine doping method of cerium-based rare earth polishing powder. The fluorine doping method comprises the following steps: (1) respectively preparing a cerium-based rare earth salt solution, a precipitator and a fluorinating agent; (2) adding the rare earth salt solution, the precipitator and the fluorinating agent into a reaction kettle through parallel flow at a certain flow velocity, controlling the pH of the reaction system through controlling the flow velocity of the precipitator, controlling the fluorine doping proportion through controlling the flow velocity of the fluorinating agent, keeping a certain temperature in the reaction process, stirring violently, carrying out ageing after the reaction, and carrying out filtration, cleaning and drying on the sizing agent to obtain a cerium-based rare earth polishing powder precursor; and (3) calcining the prepared cerium-based rare earth polishing powder precursor, and carrying out natural cooling in the furnace to obtain the cerium-based rare earth polishing powder material. The fluorine doping method is simple in process, convenient to operate and suitable for industrial production. The cerium-based rare earth polishing powder prepared through the method is spherical in particle shape and controllable in particle size of product; and products with different particle sizes and different particle size distributions can be prepared according to the requirements of rare earth polishing powder with different applications.

Description

technical field [0001] The invention relates to a method for doping cerium-based rare earth polishing powder with fluorine. Background technique [0002] Cerium-based rare earth polishing powder is an excellent polishing material, which is widely used in optical glass, liquid crystal screen, semiconductor silicon wafer and other fields because of its unique polishing performance. [0003] Fluorine is added to the existing cerium-based rare earth polishing powder to improve the crystal structure, participate in chemical adsorption during the polishing process, and improve the polishing ability. There are two main ways of doping fluorine: one is to first synthesize rare earth carbonate, and then perform fluorination treatment to prepare fluorine-doped rare earth polishing powder, as mentioned in the patent document CN101899281A; the other is to first generate rare earth fluoride, and then Precipitate with bicarbonate to prepare fluorine-doped rare earth polishing powder, such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K3/14C09G1/02
Inventor 郭荣贵蒋文全于丽敏李涛张婧黄小卫胡运生
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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