CN101391788A - Method for preparing alumina powder for polishing solution - Google Patents
Method for preparing alumina powder for polishing solution Download PDFInfo
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- CN101391788A CN101391788A CNA2008102264403A CN200810226440A CN101391788A CN 101391788 A CN101391788 A CN 101391788A CN A2008102264403 A CNA2008102264403 A CN A2008102264403A CN 200810226440 A CN200810226440 A CN 200810226440A CN 101391788 A CN101391788 A CN 101391788A
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- preparation
- alumina powder
- alumina
- polishing
- urea
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000005498 polishing Methods 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 31
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- 238000001556 precipitation Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 8
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 claims description 10
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 3
- 238000012216 screening Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 3
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 239000012530 fluid Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- NPSSWQJHYLDCNV-UHFFFAOYSA-N prop-2-enoic acid;hydrochloride Chemical compound Cl.OC(=O)C=C NPSSWQJHYLDCNV-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method for polishing liquid used alumina powder, relates to a preparation method for alumina, in particular to a preparation method for polishing liquid and polishing powder used for spherical alumina powder by liquid phase precipitation method. The preparation method is characterized by the preparation process thereof, comprising: adding urea and catalyst in 0.2-0.4M ammonium aluminum sulfate solution for carrying out reaction under the temperature of 60 to 80 DEG C till the precipitation appears; carrying out aging, and then filtering, washing, and drying so as to obtain the precursor of the alumina powder which is calcined for 2 to 6 hours at 1200 to 1600 DEG C; later calcined alumina is obtained; finally, by screening, spherical alumina which has integral crystallization, high purity (the alumina content reaches 99.5 percent), good mobility, and uniform particle diameter, and is suitable to be used for the polishing liquid is obtained.
Description
Technical field
A kind of preparation method of alumina powder for polishing solution relates to a kind of preparation method of aluminum oxide, particularly adopts liquid-phase precipitation method to prepare the preparation method of the ball-aluminium oxide powder that polishing fluid uses with polishing powder.
Background technology
Along with the fast development of electronic technology towards high precision, high-performance, high integration and high reliability direction, to machinery manufacturing industry high requirement has been proposed, especially the requirement to working accuracy and surface quality also becomes more and more higher.Like this, to being widely used in computer hard disc and CD, advanced glass such as optical elements such as ultraprecise optical lens and optical window and light communication element, flat-panel screens, it is shaggy to be the key factor that influences the performance of these high-tech products, and polishing is the important means that reduces the glass surface roughness.In glossing, the preparation of polishing fluid is a key wherein, and aluminum oxide is one of main component in the polishing fluid, and the performance of aluminum oxide directly influences the performance of product.
Aluminum oxide, because of its fusing point height, hardness is big, and chemical property is stable, is widely used in association areas such as wear-resisting, anti-corrosion, high temperature resistant, insulation.At present,, in the process of preparation slurry, exist shortcomings such as dispersion stabilization is bad, easy reunion, often will occur precipitation in the several minutes, the particle chap as alumina abrasive in the polishing fluid.Like this, matrix surface tear in polishing is serious, damages layer depth, has finally influenced the performance of product.
The performance of aluminum oxide for a change, Lu Haican etc. have carried out surface modification with acrylate chloride to aluminum oxide, have improved the suspended dispersed performance of aluminum oxide to a certain extent, have also increased production cost simultaneously, the pattern of aluminum oxide does not change, and can not improve the polishing usefulness of alumina polishing solution well.Though Zhengzhou research institute of Chinese Aluminium Co., Ltd exploitation high pure spherical aluminum oxide can be as abrasive material in the polishing fluid, cost is too high.
Summary of the invention
Deficiency and shortcoming that purpose of the present invention just exists at prior art provide preparation method a kind of purity height, even particle size distribution, good fluidity, perfect crystalline, formed the spheric alumina powder for polishing solution by the nano particle agglomeration.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of alumina powder for polishing solution, it is characterized in that its preparation process comprises adds urea and catalyzer after reaction under the 60-80 ℃ of temperature to precipitation occurs with aluminum ammonium sulfate solution, carry out ageing, filter then, wash, drying obtains the aluminum oxide powder presoma, the aluminum oxide powder presoma was got 2-6 hour 1200-1600 ℃ of roasting, obtain alumina powder for polishing solution.
The preparation method of a kind of alumina powder for polishing solution of the present invention, when it is characterized in that described aluminum ammonium sulfate solution adds urea and catalyst reaction, the exsiccated ammonium alum of reaction and the mass ratio of urea are to be 0.069-0.34: 1; The catalyzer that adds is a urase, and the adding quality of catalyzer is the 0.2%-1% of urea quality.
The preparation method of a kind of alumina powder for polishing solution of the present invention is characterized in that described aluminum ammonium sulfate solution is that to be configured to concentration with deionized water heated and stirred dissolving be 0.2-0.4M aluminum ammonium sulfate solution.
A kind of preparation polishing fluid method of alumina of the present invention is under the effect of catalyzer, and liquid-phase precipitation has been prepared the spheric aluminum oxide that the roasting at a certain temperature of ball-aluminium oxide presoma obtains.The alumina powder for polishing solution of the present invention's preparation is the ball-aluminium oxide of nanostructure, perfect crystalline, and good fluidity especially is suitable as the polishing fluid abrasive powder, and as thermospray.Adopt this prepared ball-aluminium oxide, have following advantage: 1) preparation technology is simple, cost is low, the cycle is short, is easy to engineering and amplifies; 2) improve speed of response, helped energy efficient, and do not produced the three wastes, environmentally friendly; 3) this ball-aluminium oxide even particle size distribution, good fluidity, perfect crystalline; 4) the ball-aluminium oxide powder of preparing, perfect crystalline, good fluidity can be used as fields such as thermospray and fine ceramics.
Description of drawings
Fig. 1 is for adopting the polishing fluid alumina precursor stereoscan photograph of method preparation of the present invention.
Fig. 2 is for adopting the polishing fluid ball-aluminium oxide stereoscan photograph of method preparation of the present invention.
Embodiment
A kind of preparation method of alumina powder for polishing solution, the step of its preparation process comprises:
(1) with the exsiccated ammonium alum be raw material, with the dissolving of deionized water heated and stirred, being configured to concentration is 0.2-0.4M aluminum ammonium sulfate solution;
(2) aluminum ammonium sulfate solution is added in the isothermal reactor, and to wherein adding urea and catalyzer, stir, solution reaction generates precipitation;
(3), after reacting completely, continue to stir half an hour after, ageing, the washing secondary, after the filtration, 80 ℃ of dryings are 12 hours in loft drier, obtain dry precursor;
(4) with the ball-aluminium oxide presoma in retort furnace 1200-1600 ℃ roasting 2-6 hour, with products therefrom screening, obtain the ball-aluminium oxide of the uniform nanostructure of particle diameter.
The preparation method of a kind of alumina powder for polishing solution of the present invention, described reaction process adds hydrolyst, and catalyzer is a urase, and the add-on of catalyzer is the 0.2%-1% of urea quality.
The preparation method of a kind of alumina powder for polishing solution of the present invention, the mass ratio of described reaction process exsiccated ammonium alum and urea is: (0.069-0.34): 1
The preparation method of a kind of alumina powder for polishing solution of the present invention, the temperature of described reaction are 60-80 ℃.
The preparation method of a kind of alumina powder for polishing solution of the present invention, its stirring velocity is r≤500rpm.
Embodiment 1
80 gram exsiccated ammonium alums are put in the 1000 clean ml beakers, added 800 milliliters of pure water, add 100 gram urea and 0.75 gram urase after the heating for dissolving, put into isothermal reactor, set 60-80 ℃ of bath temperature, the heating in water bath beaker, regulating stirring velocity simultaneously is the 200rpm stirred solution.After 3 hours, precipitation occurs, ageing is after 0.5 hour, filtration washing.In retort furnace 1200-1600 ℃ roasting 2-6 hour, obtain spherical αYang Hualv.
Embodiment 2
120 gram exsiccated ammonium alums are put in the 1000 clean ml beakers, add an amount of pure water to 800 milliliter, add 100 gram urea and 0.75 gram urase after the heating for dissolving, put into isothermal reactor, set 60-80 ℃ of bath temperature, the heating in water bath beaker, regulating stirring velocity simultaneously is the 200rpm stirred solution.After about 3.5 hours, precipitation occurs, ageing is after 0.5 hour, filtration washing.In retort furnace 1200-1600 ℃ roasting 2-6 hour, obtain spherical αYang Hualv.
Embodiment 3
80 gram exsiccated ammonium alums are put in the 1000 clean ml beakers, added an amount of pure water to 800 milliliter, add 100 gram urea after the heating for dissolving, put into isothermal reactor, set 60-80 ℃ of bath temperature, the heating in water bath beaker, regulating stirring velocity simultaneously is the 200rpm stirred solution.After about 4 hours, precipitation occurs, ageing is after 0.5 hour, filtration washing.In retort furnace 1200-1600 ℃ roasting 2-6 hour, obtain spherical αYang Hualv.
Embodiment 4
120 gram exsiccated ammonium alums are put in the 1000 clean ml beakers, added an amount of pure water to 800 milliliter, add 100 gram urea after the heating for dissolving, put into isothermal reactor, set 60-80 ℃ of bath temperature, the heating in water bath beaker, regulating stirring velocity simultaneously is the 200rpm stirred solution.After about 4.5 hours, precipitation occurs, ageing is after 0.5 hour, filtration washing.In retort furnace 1200-1600 ℃ roasting 2-6 hour, obtain spherical αYang Hualv.
Claims (3)
1. the preparation method of an alumina powder for polishing solution, it is characterized in that its preparation process is included in aluminum ammonium sulfate solution adding urea and catalyzer is reacting under the 60-80 ℃ of temperature to the precipitation appearance, carry out ageing, filter then, wash, drying obtained the aluminum oxide powder presoma, and the aluminum oxide powder presoma was obtained alumina powder for polishing solution at 1200-1600 ℃ of roasting 2-6 hour.
2. the preparation method of a kind of alumina powder for polishing solution according to claim 1, when it is characterized in that described aluminum ammonium sulfate solution adds urea and catalyst reaction, the exsiccated ammonium alum of reaction and the mass ratio of urea are to be 0.069-0.34:1; The catalyzer that adds is a urase, and the adding quality of catalyzer is the 0.2%-1% of urea quality.
3. the preparation method of a kind of alumina powder for polishing solution according to claim 1 is characterized in that described aluminum ammonium sulfate solution is the aluminum ammonium sulfate solution that is configured to 0.2-0.4M with the dissolving of deionized water heated and stirred.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102264403A CN101391788A (en) | 2008-11-11 | 2008-11-11 | Method for preparing alumina powder for polishing solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102264403A CN101391788A (en) | 2008-11-11 | 2008-11-11 | Method for preparing alumina powder for polishing solution |
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| Publication Number | Publication Date |
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| CN101391788A true CN101391788A (en) | 2009-03-25 |
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| CNA2008102264403A Pending CN101391788A (en) | 2008-11-11 | 2008-11-11 | Method for preparing alumina powder for polishing solution |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040236A (en) * | 2010-11-18 | 2011-05-04 | 中国海洋石油总公司 | Preparation method of super-purity aluminum oxide |
| CN102531015A (en) * | 2011-05-26 | 2012-07-04 | 中国科学院福建物质结构研究所 | Method for preparing porous aluminum oxide superfine powder |
| CN102643628A (en) * | 2012-03-13 | 2012-08-22 | 杭州智华杰科技有限公司 | Production method of polishing powder for crystal glass |
| CN102925060A (en) * | 2012-11-09 | 2013-02-13 | 济南大学 | Preparation method of marble composite polishing powder |
| CN103693664A (en) * | 2013-12-11 | 2014-04-02 | 北京世纪地和控股有限公司 | Method for preparing polished aluminium oxide by using precipitation method |
| CN113233486A (en) * | 2021-04-23 | 2021-08-10 | 中铝山东有限公司 | Sphere-like alumina and preparation method and application thereof |
-
2008
- 2008-11-11 CN CNA2008102264403A patent/CN101391788A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040236A (en) * | 2010-11-18 | 2011-05-04 | 中国海洋石油总公司 | Preparation method of super-purity aluminum oxide |
| CN102040236B (en) * | 2010-11-18 | 2012-09-26 | 中国海洋石油总公司 | Preparation method of super-purity aluminum oxide |
| CN102531015A (en) * | 2011-05-26 | 2012-07-04 | 中国科学院福建物质结构研究所 | Method for preparing porous aluminum oxide superfine powder |
| CN102643628A (en) * | 2012-03-13 | 2012-08-22 | 杭州智华杰科技有限公司 | Production method of polishing powder for crystal glass |
| CN102925060A (en) * | 2012-11-09 | 2013-02-13 | 济南大学 | Preparation method of marble composite polishing powder |
| CN102925060B (en) * | 2012-11-09 | 2014-03-26 | 济南大学 | Preparation method of marble composite polishing powder |
| CN103693664A (en) * | 2013-12-11 | 2014-04-02 | 北京世纪地和控股有限公司 | Method for preparing polished aluminium oxide by using precipitation method |
| CN103693664B (en) * | 2013-12-11 | 2015-12-30 | 北京世纪地和控股有限公司 | A kind of method utilizing the precipitator method to prepare polishing aluminum oxide |
| CN113233486A (en) * | 2021-04-23 | 2021-08-10 | 中铝山东有限公司 | Sphere-like alumina and preparation method and application thereof |
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Open date: 20090325 |