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Preparation method of composite cerium-zirconium oxide polishing powder

A composite oxide and polishing powder technology, which is applied in the direction of chemical instruments and methods, and other chemical processes, to achieve the effects of small particle size, significant synergistic polishing, and high wear resistance

Active Publication Date: 2013-06-19
上海华明高纳稀土新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent 200910044264.6 reports a production process of zirconia grinding liquid, but zirconia (ZrO 2 ) The abrasive is soft, and the application of the polishing agent made from it is limited to the polishing of soft material spherical glass

Method used

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  • Preparation method of composite cerium-zirconium oxide polishing powder
  • Preparation method of composite cerium-zirconium oxide polishing powder
  • Preparation method of composite cerium-zirconium oxide polishing powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Ball mill pulverization: weigh 260 g of cerium carbonate (Ce 2 (CO 3 ) 3 ·8H 2 O) As a cerium source, add 2340 g of deionized water, stir and disperse, and prepare a slurry with a solid content of 10 wt% for high-energy ball milling and pulverization, until the average particle size of the particles in the corresponding slurry is D. 50 Equal to 0.66μm, D 90 equal to 1.16μm (eg figure 1 shown);

[0024] (2) Precipitation mixing: 373.2 g of zirconium nitrate (Zr(NO) was added to the product of step (1). 3 ) 4 ·5H 2 O), stir to prepare a mixed slurry of Ce:Zr=5:5 (molar ratio), slowly add ammonium bicarbonate solution (concentration of 10wt%) to the mixed slurry to precipitate zirconium ions, when the pH of the mixed solution reaches about 7.0 When the precipitation is over, continue to stir the mixed solution for 1 hour, then let it stand for 3 hours, and then dry at 80°C for 6 hours after dehydration;

[0025] (3) calcination: the product of step (2) is calc...

Embodiment 2

[0028] (1) Ball mill pulverization: Weigh 200 g of cerium hydroxide as a cerium source (corresponding to CeO 2 content is 80wt%), add 3800g deionized water, stir and disperse, prepare a slurry with a solid content of about 5wt%, and conduct high-energy ball milling and pulverize until the average particle size of the particles in the corresponding slurry is D. 50 is 0.7 μm, D 90 is 1.2μm;

[0029] (2) Precipitation mixing: 99.8 g of zirconium nitrate (Zr(NO) was added to the product of step (1). 3 ) 4 ·5H 2 O), stir to prepare a mixed slurry of Ce:Zr=8:2 (molar ratio), slowly add ammonia water (concentration: 30wt%) to the mixed slurry to precipitate zirconium ions, when the pH of the mixed solution reaches about 10.0, the precipitation After the end, continue to stir the mixed solution for 2 hours, then stand for 5 hours, and then dry at 80°C for 12 hours after dehydration;

[0030] (3) calcination: the product of step (2) is calcined at 1000° C. for 3 hours to obtain a ...

Embodiment 3

[0033] (1) Ball mill pulverization: Weigh 200 g of cerium oxalate as a cerium source (Ce (C 2 O 4 ) 3 ·9H 2 O), add 1800g deionized water, stir and disperse, prepare a slurry with a solid content of 10wt% and carry out high-energy ball milling pulverization, until the average particle size D of the corresponding slurry 50 is 0.72 μm, D 90 is 1.33 μm;

[0034] (2) Precipitation mixing: add 730 g of zirconium oxychloride (ZrOCl) to the product of step (1) 2 ·8H 2 O), stir to prepare a mixed slurry of Ce: Zr=2: 8 (molar ratio), and slowly add oxalic acid solution (concentration of 20wt%) to the mixed slurry while stirring to precipitate zirconium ions. Add oxalic acid dropwise to the supernatant, no more precipitation will be produced, the precipitation is over (the pH value is about 2.0), continue to stir the mixed solution for 2 hours, then let stand for 5 hours, and dry at 80 ° C for 10 hours after dehydration;

[0035] (3) calcination: the product of step (2) is calcin...

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Abstract

The invention provides a preparation method of a composite cerium-zirconium oxide polishing powder. The preparation method comprises the following steps: (1) preparing insoluble cerium salts into slurry, carrying out ball milling and smashing until the average particle size D50 of particles in the slurry is distributed within a range from 0.55mu m to 0.75mu m, and the average particle size D90 ofparticles in the slurry is distributed within a range from 1.1mu m to 1.4mu m; (2) adding soluble zirconium salts into a product obtained in the step (1), adding a precipitator, standing and ageing, dehydrating and drying, wherein the precipitator is ammonia water, ammonium bicarbonate or oxalic acid; and (3) roasting for 3-8 hours at the temperature of 850-1000 DEG C, and carrying out jet milling so as to obtain the composite cerium-zirconium oxide polishing powder. According to the invention, the obtained polishing powder has small particle size and narrow size distribution range, has the performance characteristics of rapid polishing rate, less scratches and high abrasive resistance on a glass substrate, and has obvious synergetic polishing effect.

Description

technical field [0001] The invention relates to a preparation method of cerium zirconium composite oxide polishing powder. Background technique [0002] With the continuous development of semiconductor technology and the continuous reduction of the structure of semiconductor elements, chemical mechanical polishing (Chemical Mechanical Polishing, CMP) plays an increasingly important role in providing global planarization in the semiconductor manufacturing process. The polishing liquid is one of the key elements of CMP, and the performance of the polishing liquid directly affects the polishing rate and the quality of the polished surface. The polishing liquid is generally composed of ultra-fine solid polishing powder particles (such as nano- or sub-micron Fe 2 O 3 , CeO 2 , SiO 2 , Al 2 O 3 Particles), surfactants, pH adjusters, etc., among which the polishing powder particles provide abrasive action and are the core material in the chemical mechanical polishing process....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K3/14
Inventor 尹先升赵月昌曹红霞杨筱琼赵秀娟蒙素玲
Owner 上海华明高纳稀土新材料有限公司
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