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CN103965790B - Zr-Al-Ce polishing solution and preparation method thereof - Google Patents

Zr-Al-Ce polishing solution and preparation method thereof Download PDF

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Publication number
CN103965790B
CN103965790B CN201410169996.9A CN201410169996A CN103965790B CN 103965790 B CN103965790 B CN 103965790B CN 201410169996 A CN201410169996 A CN 201410169996A CN 103965790 B CN103965790 B CN 103965790B
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polishing
powder
cerium
polishing fluid
glass
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CN103965790A (en
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于长江
王兆敏
王猛
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Shandong Maifeng New Material Science And Technology Co ltd
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Tai'an Mai Feng Novel Material Science And Technology Ltd
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Abstract

The invention belongs to the technical field of polishing solutions, aims to overcome the defects in the prior art, and provides a polishing solution for soft thin glass materials. Especially, the polishing solution is prepared by compounding zirconia powder, ceria polishing powder, alumina polishing powder, ferric oxide powder, composite additives and water. The polishing solution is mild in polishing process, the surface of the glass after polishing is smooth, and the glass surface finish is high. The polishing solution improves the suspension stability of a slurry system, reduces the viscosity of zirconia grinding materials, improves the fluidity and the cutting speed, shortens the corrosion time, prevents the scratch and water stain phenomena, reduces the surface tension, improves the compatibility, and solves the industrial technical problems of corrosion and water stain.

Description

A kind of zirconium aluminium cerium polishing fluid and preparation method thereof
Technical field
The invention belongs to the production technical field of polishing fluid, relate to a kind of polishing fluid and preparation method thereof, particularly a kind of zirconium aluminium cerium polishing fluid and preparation method thereof.
Background technology
Along with optical field requires more and more higher to the unicity of light, require that the specific refractory power of glass is more and more higher, glass material or ultra-soft, ultra-thin, opticglass cold working belongs to labor-intensive enterprises, throws softwood matter glass and requires to produce cut, ensure stronger rate of cutting again, be convenient to cleaning after polishing, can not washmarking be remained.
CMP chemically machinery polished is the combination technique of mechanical mill and chemical corrosion, its grinding by ultramicron and the chemical corrosion effect of polishing slurries, in the alternation procedure of chemical membrane and mechanical striping, remove the layer of material of polished dielectric surface, realize the processing of ultraprecise planarized surface.Abrasive material in polishing fluid (slurry), mainly can form a class material of crystalline structure, mainly contain diamond, silicon carbide, ferric oxide, aluminum oxide, titanium oxide, zirconium white, cerium oxide etc.The polishing fluid sold in the market is cerium oxide, zirconium white, silicon oxide, diamond polishing liquid mainly.Wherein the most applicable opticglass polishing is cerium oxide polishing slurry, Mohs' hardness 7.0-7.5, and rate of cutting is strong, is suitable for large lens and harder material glass.Silicon dioxide polishing solution is nano level, and surface quality is high, but rate of cutting is too slow.Current high quality optical element all uses pitch polishing, but due to the seriously polluted cleaning difficulty of pitch complicated component; And adopt CeO2, Al2O3 abrasive material to grind, the problems such as this abrasive material generally adopts disintegrating process to make, and there is particle uneven, adopts this abrasive material also to there is seriously polluted not easy cleaning, and simultaneously operation is loaded down with trivial details.
Patent CN100497508C discloses a kind of production method of high-cerium rare-earth polishing powder, the fluorine cerium lanthanum oxide polishing powder of polymolecularity is obtained by introducing JZPD capsule in polishing powder building-up process, but described crystal seed needs previously prepared, and described polishing powder is formulated as the polishing slurries of specified chemical composition further.Patent CN101899281 discloses a kind of manufacture method of polishing powder, but described polishing powder particle size is comparatively large, and polishing precision is lower.
summary of the invention:
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of polishing fluid meeting soft thin glass material, its polishing process is gentle, and surface of polished is smooth, and glass surface finishes is high.
Particularly, the present invention is achieved through the following technical solutions:
A kind of zirconium aluminium cerium polishing fluid provided by the invention, is prepared from according to certain weight by water, zirconia powder, cerium rouge, aluminum oxide polishing powder, ferric oxide powder, comprehensive auxiliary agent etc.
Preferably, zirconium aluminium cerium polishing fluid of the present invention, it is characterized in that containing water 400-700 weight part, zirconia powder 240-260 part, cerium rouge 5-10 part, aluminum oxide polishing powder 0.1-2 part, account for the ferric oxide powder of zirconia powder weight part 0.25-0.5% and account for the comprehensive auxiliary agent of zirconia powder weight part 16-32%.
Preferably, the specific surface area of described zirconia powder is 2-6m 2/ g.
Preferably, the purity of described cerium rouge is between 99-99.9%.
Preferably, described zirconia powder and cerium rouge hardness be 5.5-6.0.
Preferably, described aluminum oxide polishing powder is purity is 99.9-99.99%, and outward appearance is the α-aluminum oxide of platy structure.
Preferably, described comprehensive auxiliary agent is a kind of functional agent for dispersion agent, alcohol mixture and deionized water composition.
Preferably, described dispersion agent: alcohol mixture: the weight ratio of water is 1:2:20.
Preferably, described dispersion agent is the water-soluble high-molecular compound of pH 5.0-8.0, and most preferably, described dispersion agent is the one in polyvidone, polyacrylic acid or poly amic acid.
Preferably, described alcohol mixture is arbitrary two kinds in ethanol, ethylene glycol, propylene glycol, glycerol, Virahol, and particularly preferably, described alcohol mixture is Virahol and ethylene glycol, and wherein the ratio of Virahol and ethylene glycol is 1:(1-2).
Present invention also offers a kind of preparation method of zirconium aluminium cerium polishing fluid, specifically comprise following steps:
Step 1) adds zirconia powder 240-260 part of autonomous roasting in 400-700 part water of high speed dispersion, is uniformly dispersed;
Step 2) add the aluminum oxide polishing powder of 5-10 part cerium rouge and 0.1-2 part, be equipped with the ferric oxide powder accounting for oxidation powder weight part 0.25-0.5%, be uniformly dispersed;
Step 3) enters Ball-stirring mill grinding, and rounding compounded abrasive being worn into certain granularity is spherical;
Step 4) adds the comprehensive auxiliary agent modulation accounting for zirconia powder weight 16-32% and evenly namely obtains zirconium aluminium cerium polishing fluid.
Preferably, the granularity described in above-mentioned steps 3 is D50:0.5-1.30um, D97≤3.60um.
The present invention's above-mentioned zirconium aluminium cerium polishing fluid can be applicable to space flight and aviation devitrified glass, accurate liquid crystal conductive glass, planar wave glass, optical spherical surface, optical lens glass, spectral filter, spectral window, and the aspect such as the precise finiss polishing of glass substrate.
The present invention compared with prior art has the following advantages:
1. select partially soft zirconium white as the main abrasive material of polishing fluid, well solve fine scratches phenomenon.Zirconic Mohs' hardness selected by the present invention is between 5.5-6.0, partially softer than cerium oxide, higher with the consistency of glass, is suitable for the polishing compared with softwood matter and ultra-thin glass material, can effectively solves fine scratches phenomenon.
2. the present invention's autonomous roasting of adopting specified weight part to form cerium oxide and introduce the alumina powder composition compounded abrasive of suitable stiffness.
3. the cerium oxide of creationary interpolation specified weight part composition and aluminum oxide are as auxiliary abrasive, improve rate of cutting, reduce polishing time, namely reduce the crevice corrosion time of polished glass and slurry, effectively alleviate washmarking and the orange peel phenomenon of glass surface, also reduce the cost of labor of cold working process.
4. the present invention add the effect that aqueous high molecular auxiliary agent and glycerol mixed aid play stable slurry system.
5. add the alcohol mixture of Virahol and ethylene glycol, reduce the surface tension of slurry, solve the viscosity of slurry and glass surface, efficiently solve the corrosion washmarking phenomenon of polished and cleaned process, solve a technical difficult problem for glass cold working industry.
6. add ferric oxide first as tinting material, play the effect of blast slurry, and zirconic viscosity can be reduced, easily clean, reduce washmarking phenomenon; Make the concentration of the slurries in polishing process keep stable, light stable circle is played a role.
The present invention achieves technique effect unexpected as follows:
1. this product uses a kind of superfine zirconia, cerium oxide, aluminum oxide mixing polishing powder as main abrasive material, and overcome existing zirconium cerium aluminium polishing fluid, polishing characteristic is partially soft, poor stability, deposit clumps, and viscosity is strong, the shortcomings such as rate of cutting is weak.The stability of mixed polishing solution of the present invention takes on a new look greatly, can long storage time, and keeps loose, can Eddy diffusion after fully stirring.
2. this product with the addition of a small amount of aluminum oxide and cerium oxide, improves cutting speed, shortens glass and polishing fluid duration of contact, decreases corrosion washmarking phenomenon to a certain extent; Reduce the cold worked cost of labor of opticglass.
3. this product with the addition of appropriate Virahol and ethylene glycol.Solve corrosion washmarking that glass polishing particularly easily occurs in softwood matter glass polishing process than phenomenon, effectively solve the industry difficult problem in domestic and international grinding and polishing.
4. this product adopts zirconium white to make main abrasive material, and ferric oxide carries out modification to whole polishing fluid system.The product that adds of ferric oxide improves the stability of polishing fluid suspension system and submissive color and luster.
Zirconium cerium aluminium polishing fluid of the present invention in a word, the suspension stability of slurry system strengthens greatly, reduces the viscosity of zirconia, improves mobility and rate of cutting, decreases etching time, solves cut and washmarking phenomenon; Reduce surface tension, improve consistency, solve an industry technology difficult problem for corrosion washmarking phenomenon.
Embodiment
The present invention is further described below by specific embodiment; but described embodiment is illustrative instead of determinate; several embodiments can be listed according to institute's limited range, therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.
embodiment 1
The specific surface area of autonomous roasting is added at 2-6m in 700 parts of water of high speed dispersion 2the zirconia powder of/g 240 parts, after being uniformly dispersed, adding the α-aluminum oxide polishing powder of the platy structure of 6 parts of cerium rouges and 0.2 part, is equipped with the ferric oxide powder accounting for zirconia powder weight part 0.25%, is uniformly dispersed; Enter Ball-stirring mill grinding, compounded abrasive being worn into granularity is that the rounding of D50:0.5-1.30um, D97≤3.60um is spherical; Then add the comprehensive auxiliary agent (wherein polyvidone: ethanol: propylene glycol: the weight ratio of water is 1:1:1:20) accounting for zirconia powder weight 16%, namely modulation evenly obtains zirconium aluminium cerium polishing fluid.
embodiment 2
The specific surface area of autonomous roasting is added at 2-6m in 600 parts of water of high speed dispersion 2the zirconia powder of/g 260 parts, after being uniformly dispersed, adds the α-aluminum oxide polishing powder of 10 parts of cerium rouges and 2 parts of platy structures, is equipped with the ferric oxide powder accounting for oxidation powder weight part 0.5%, is uniformly dispersed; Enter Ball-stirring mill grinding, compounded abrasive being worn into granularity is that the rounding of D50:0.5-1.30um, D97≤3.60um is spherical; Then add the comprehensive auxiliary agent (wherein polyacrylic acid: ethanol: ethylene glycol: the weight ratio of water is 1:1:1:20) accounting for zirconia powder weight 32%, namely modulation evenly obtains zirconium aluminium cerium polishing fluid.
embodiment 3
The specific surface area of autonomous roasting is added at 2-6m in 650 parts of water of high speed dispersion 2the zirconia powder of/g 250 parts, after being uniformly dispersed, adds the α-aluminum oxide polishing powder of 8 parts of cerium rouges and 1 part of platy structure, is equipped with the ferric oxide powder accounting for oxidation powder weight part 0.4%, is uniformly dispersed; Enter Ball-stirring mill grinding, compounded abrasive being worn into granularity is that the rounding of D50:0.5-1.30um, D97≤3.60um is spherical; Then add the comprehensive auxiliary agent (wherein polyacrylic acid: ethanol: glycerol: the weight ratio of water is 1:1:1:20) accounting for zirconia powder weight 25%, namely modulation evenly obtains zirconium aluminium cerium polishing fluid.
embodiment 4
The specific surface area of autonomous roasting is added at 2-6m in 680 parts of water of high speed dispersion 2the zirconia powder of/g 260 parts, after being uniformly dispersed, adds the α-aluminum oxide polishing powder of the platy structure of 9 parts of cerium rouges and 1.5 parts, is equipped with the ferric oxide powder accounting for oxidation powder weight part 0.3%, is uniformly dispersed; Enter Ball-stirring mill grinding, compounded abrasive being worn into granularity is that the rounding of D50:0.5-1.30um, D97≤3.60um is spherical; Then add the comprehensive auxiliary agent (wherein poly amic acid: ethanol: glycerol: the weight ratio of water is 1:1:1:20) accounting for zirconia powder weight 20%, namely modulation evenly obtains zirconium aluminium cerium polishing fluid.

Claims (7)

1. a zirconium aluminium cerium polishing fluid, it is characterized in that, containing water 400-700 weight part, zirconia powder 240-260 weight part, cerium rouge 5-10 weight part, aluminum oxide polishing powder 0.1-2 weight part and the ferric oxide powder accounting for zirconia powder weight part 0.25-0.5%, accounting for the comprehensive auxiliary agent of zirconia powder weight part 16-32%;
Described comprehensive auxiliary agent is the functional agent for dispersion agent, alcohol mixture and deionized water composition, wherein said dispersion agent: alcohol mixture: the weight ratio of water is 1:2:20;
Described dispersion agent is the one in polyvidone, polyacrylic acid or poly amic acid;
Described alcohol mixture is Virahol and ethylene glycol, and wherein the ratio of Virahol and ethylene glycol is 1:(1-2).
2. a kind of zirconium aluminium cerium polishing fluid as claimed in claim 1, is characterized in that the specific surface area of described zirconia powder is 2-6m 2/ g.
3. a kind of zirconium aluminium cerium polishing fluid as claimed in claim 1, is characterized in that the purity of described cerium rouge and aluminum oxide polishing powder is 99-99.9%.
4. a kind of zirconium aluminium cerium polishing fluid as claimed in claim 1, it is characterized in that described zirconia powder and cerium rouge hardness be 5.5-6.0.
5. a kind of zirconium aluminium cerium polishing fluid as claimed in claim 1, is characterized in that described dispersion agent is the water-soluble high-molecular compound of pH5.0-8.0.
6. the preparation method of a kind of zirconium aluminium cerium polishing fluid as claimed in claim 1, is characterized in that comprising following steps:
Step 1) adds zirconia powder 240-260 part of autonomous roasting in 400-700 part water of high speed dispersion, is uniformly dispersed;
Step 2) add the aluminum oxide polishing powder of 5-10 part cerium rouge and 0.1-2 part, be equipped with the ferric oxide powder accounting for zirconia powder weight part 0.25-0.5%, be uniformly dispersed;
Step 3) enters Ball-stirring mill grinding, and rounding compounded abrasive being worn into certain granularity is spherical;
Step 4) adds the comprehensive auxiliary agent modulation accounting for zirconia powder weight 16-32% and evenly namely obtains zirconium aluminium cerium polishing fluid;
Wherein, the granularity described in step 3 is D50:0.5-1.30um, D97≤3.60um.
7. the purposes of zirconium aluminium cerium polishing fluid in space flight and aviation devitrified glass, accurate liquid crystal conductive glass, planar wave glass, optical spherical surface, optical lens glass, spectral filter, spectral window, the polishing of glass substrate precise finiss as described in as arbitrary in claim 1-5.
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CN104403575B (en) * 2014-12-23 2016-09-21 包头市华辰稀土材料有限公司 A kind of preparation method of high accuracy aluminum oxide polishing powder
CN107254259A (en) * 2017-06-08 2017-10-17 包头海亮科技有限责任公司 Novel rare-earth polishing powder and preparation method thereof
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CN108864949B (en) * 2018-08-29 2020-07-28 德米特(苏州)电子环保材料有限公司 Rare earth polishing solution for polishing glass and preparation method thereof
CN109439282A (en) * 2018-10-23 2019-03-08 蓝思科技(长沙)有限公司 Composite Nano abrasive material, polishing fluid and preparation method thereof, chip glass and electronic equipment
CN111454666A (en) * 2020-05-25 2020-07-28 安徽禾臣新材料有限公司 High-suspension polishing powder and preparation method thereof
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CN113897177A (en) * 2021-09-03 2022-01-07 永州市湘江稀土有限责任公司 Composite oxide abrasive particle and preparation method thereof
CN114591687A (en) * 2022-03-18 2022-06-07 深圳市瑞来稀土材料有限公司 Rare earth polishing powder for semiconductor wafer polishing treatment and preparation method thereof
CN115785818B (en) * 2022-11-10 2023-06-20 湖北五方光电股份有限公司 A kind of polishing liquid and its preparation method and application
CN115961318B (en) * 2022-12-20 2025-03-18 宁波韵升股份有限公司 A treatment method for increasing the dyne value of the nickel coating on the surface of NdFeB magnetic steel

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