CN106147616A - The preparation method of solvent-borne type modified aluminum oxide polishing fluid - Google Patents
The preparation method of solvent-borne type modified aluminum oxide polishing fluid Download PDFInfo
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- CN106147616A CN106147616A CN201510223481.7A CN201510223481A CN106147616A CN 106147616 A CN106147616 A CN 106147616A CN 201510223481 A CN201510223481 A CN 201510223481A CN 106147616 A CN106147616 A CN 106147616A
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Abstract
The preparation method of solvent-borne type modified aluminum oxide polishing fluid, it is characterized in that: first this preparation method carries out grain size grading to alumina particle, add dispersant and alumina surface is carried out coating modification, it is subsequently added into organic solvent and oxidant stirs, make it fully dispersed through supersonic vibration again, by pH adjusting agent, the pH of polishing fluid is transferred to 2.5-12.5 afterwards, polishing fluid prepared by this invention has good suspended dispersed, can be applicable under water-less environment, aluminium alloy, copper, rustless steel and Sapphire Substrate polishing, there is polishing efficiency high, surface roughness is little, substrate surface is damaged the advantages such as little.
Description
Technical field
The present invention relates to the preparation of modified aluminum oxide polishing fluid, particularly relate to the preparation method of a kind of solvent-borne type polishing fluid.
Polishing fluid prepared by this invention has good suspended dispersed, can be applicable under water-less environment, aluminium alloy, copper, stainless
Steel and Sapphire Substrate polishing, have polishing efficiency high, and surface roughness is little, and material surface is damaged the advantages such as little.
Background technology
The preparation of abrasive and the dispersion stabilization of polishing fluid are the keys of CMP technique, and they directly affect the polishing of CMP
Effect, to indices such as the degree of injury of substrate surface.Aluminium oxide is the most widely used abrasive material, and aluminium oxide hardness is only
Inferior to diamond, and the price of aluminium oxide is diamond price 1/2 even 1/3, the most alternative diamond polishing liquid is applied
In metallic articles such as hard metal and the glossings of metal alloy, such as copper, aluminum, rustless steel, aluminium alloy, nickel-phosphor
Polishing；The hardness ratio Ludox of aluminium oxide big, its polishing speed is higher than the polishing speed of Ludox, the most alternative silicon
Colloidal sol polishing fluid is applied to quasiconductor monomer and semiconducting compound glossing, such as silicon, GaAs, sapphire, carbon
The polishing of the material such as SiClx, boron carbide, alumina polishing solution can be additionally used in the polishing of insulator workpiece, such as glass, moulds
Material etc..
But aluminium oxide exists the shortcomings such as bad, the easy reunion of dispersion stabilization, cause the surface tear of substrate in polishing serious,
Damage layer depth.To this end, the present invention has carried out modification to alumina surface, improve the dispersion stabilization of aluminium oxide particles, and
It is configured to solvent-borne type polishing fluid.Now the application of a lot of fields is all aqueous polishing liquid, for solvent-borne type polishing fluid report very
Few, and certain fields must use solvent-borne type polishing fluid.
Accordingly, it is necessary to a kind of solvent-borne type polishing fluid of invention, there is good suspended dispersed, polish simultaneously
Efficiency is high, surface roughness is little, damage little to material surface, it is adaptable to the polishing requirement under anhydrous condition.
Summary of the invention
It is an object of the invention to: the preparation method of a kind of solvent-borne type modified aluminum oxide polishing fluid is provided, makes modified
Alpha-alumina dispersion stabilization improve, surface roughness reduces, little to material surface damage, for a kind of solvent-borne type oxidation
The polishing fluid of aluminum.Its principle is to utilize alumina particulate surface-OH to be formed with the acid in modifying agent to have certain stability
Covalent bond and molecular separating force (hydrogen bond, induction force, dispersion force and dipole-dipole force), thus reduce reunion, improve point
Dissipate property and the stability of solution.The purpose using solvent-borne type polishing fluid is the polishing requirement being applicable under anhydrous condition.
In order to achieve the above object, its concrete preparation process is as follows: first this preparation method carries out particle diameter to alumina particle
Classification, utilizes the supersonic vibration of liquid phase grain diameter grading device that polishing fluid carries out grain size grading, alumina particle before modified
The little granule of minority can be there is, it is carried out grain size grading and can improve polishing precision and reduce bulky grain to greatest extent to polishing
The scuffing of parts.Add dispersant (polyacrylic acid and derivant thereof or polyacrylic acid and derivant thereof and hydroxy acid mixed
Compound) alumina surface is carried out coating modification, it is subsequently added into organic solvent and oxidant stirs, then through Under Ultrasonic Vibration
Moving makes it be fully contacted, and stands 24 hours, adds stirring mixing 1-3 hour in homogenizer.After use pH adjusting agent
The pH of polishing fluid is transferred to 2.5-12.5, i.e. can get modified aluminum oxide polishing fluid.
In the polishing fluid of the present invention, aluminium oxide crystal formation is the nano aluminium oxide of α type, and even particle size distribution, purity are high, high score
Dissipate, there is resistant to elevated temperatures inertia.
Consisting of of described polishing fluid mixture: the aluminum oxide polishing powder of 1-25%, the organic solvent of 60-90%, 0.1-5%
Dispersant, the oxidant of 0.1-5%.
Described aluminium oxide be average primary particle diameter be the aluminium oxide of the alpha-crystal form structure of 0.5-3 μm.It it is preferably 0.5-3 μm
The aluminium oxide of alpha-crystal form structure.
Described dispersant is one or both 0.5-2 μm in polyacrylic acid and derivant, hydroxy acid；Described
Hydroxy acid is the one in lactic acid, citric acid, tartaric acid, salicylic acid.
Described organic solvent be DMF (DMF), N-Methyl pyrrolidone, ethanol, isopropanol, third
One or more in ketone, methyl methacrylate, isopropyl acetate, ethyl acetate.
The pH value of polishing fluid of the present invention is to be regulated by acid/base, and described pH adjusting agent includes in organic acid, mineral acid
One or more and organic base, inorganic base in one or more.Organic acid includes formic acid, acetic acid, propanoic acid and oxalic acid,
Mineral acid includes phosphoric acid, sulphuric acid, hydrochloric acid, and organic base includes monoethanolamine, triethanolamine, inorganic base include potassium hydroxide,
Sodium hydroxide, sodium carbonate, ammonia, sodium hexameta phosphate.During the pH value of alumina polishing solution one of solution suspension stability
Key factor, it determines the size of zata current potential.The pH of polishing fluid is preferably 2-5, within the range polishing fluid point
Scattered stability is preferably also.
Described oxidant is hydrogen peroxide.
Detailed description of the invention
Analytical procedure:
Dispersion stabilization
Sedimentation experiment is used to weigh solvent-borne type polishing fluid dispersion stabilization.Described polishing fluid is loaded and carries graduated graduated cylinder
In, the precipitation of polishing fluid or degeee of stratification in observed and recorded different time.
Embodiment:
Following example are further describing of the present invention, and the material wherein chosen is mass percent.
Following example are to use DMF as the embodiment of organic solvent, and DMF is
Well polar organic solvent, can be with the multiple immiscible organic solvent such as water, ethanol, chloroform and ether, N, N-dimethyl methyl
Without active hydrogen in amide, chain transfer reaction can be reduced, and, when 25 DEG C, the surface tension of DMF
For the half of the surface tension (71.81mN/m) of 36.2mN/m, almost water, when it is as the solvent of polishing fluid,
The aluminium oxide polishing particles in initial polishing fluid can be made to have limited contractility.Activated alumina easy moisture absorption deliquescence, makes
Solvent is made, it is possible to decrease the harsh dry requirement of aluminium oxide with DMF.
Embodiment 1
First alumina particle is carried out grain size grading, by 1 part of polyacrylic acid and the mixture of citric acid, 88 parts of N, N-diformazans
Base Methanamide, 10 parts of particle diameters are the alumina powder granule of 0.8 μm, the hydrogen peroxide of 1 part, after ultrasonic 0.5 hour, stand 24
Hour, rear addition stirs mixing 1-3 hour in homogenizer.With triethanolamine, pH value is transferred to about 4.5.
Embodiment 2
First alumina particle is carried out grain size grading, by 2 parts of polyacrylic acid, 78 parts of DMFs, 20 parts of grains
Footpath is the alumina powder granule of 0.8 μm, the hydrogen peroxide of 1 part, after ultrasonic 0.5 hour, stands 24 hours, adds afterwards at a high speed
Stirring mixing 1-3 hour in blender.With oxalic acid, pH value is transferred to about 3.0.
Embodiment 3
First alumina particle is carried out grain size grading, by 2 parts of citric acids and polyacrylic mixture, 68 parts of N, N-diformazans
Base Methanamide, 30 parts of particle diameters are the alumina powder granule of 0.8um, the hydrogen peroxide of 1 part, after ultrasonic 0.5 hour, stand 24
Hour, rear addition stirs mixing 1-3 hour in homogenizer.With triethanolamine, pH value is transferred to about 5.0.
Between the sedimentation value that above example records is in the range of 2-4.Polishing fluid prepared by above example has excellence
Dispersion stabilization, after 1 month, sedimentation value change is inconspicuous.
Above the specific embodiment of the present invention is described in detail, but described content has been only presently preferred embodiments of the present invention,
It is not to be regarded as the practical range for limiting the present invention.All equalizations made according to the application range of the present invention change and change
Enter, within the patent covering scope of the present invention all should be belonged to.
Claims (8)
1. the preparation method of solvent-borne type modified aluminum oxide polishing fluid, it is characterised in that: this preparation method is first to oxidation
Alumina particles carries out grain size grading, adds dispersant and alumina surface is carried out coating modification, be subsequently added into organic solvent and
Oxidant stirs, then makes it be fully contacted through supersonic vibration, after by pH adjusting agent, the pH of polishing fluid is transferred to
2.5-12.5。
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that:
Consisting of of described solvent-borne type polishing fluid mixture: the aluminum oxide polishing powder of 1-25%, the organic solvent of 60-80%, 0.1-5%
Dispersant, the oxidant of 0.1-5%.
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that:
Described aluminium oxide be average primary particle diameter be the aluminium oxide of the alpha-crystal form structure of 0.5-3 μm.
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that:
Described dispersant is one or both in polyacrylic acid and derivant, hydroxy acid；Described hydroxy acid be lactic acid,
One in citric acid, tartaric acid, salicylic acid.
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that:
Described organic solvent be DMF (DMF), N-Methyl pyrrolidone, ethanol, isopropanol, acetone,
One or more in methyl methacrylate, isopropyl acetate, ethyl acetate.
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that:
Described pH adjusting agent includes one or more in organic acid, mineral acid and one or more in organic base, inorganic base.
Organic acid includes formic acid, acetic acid, propanoic acid and oxalic acid, and mineral acid includes phosphoric acid, sulphuric acid, hydrochloric acid, and organic base includes a second
Hydramine, triethanolamine, inorganic base includes potassium hydroxide, sodium hydroxide, sodium carbonate, ammonia, sodium hexameta phosphate.
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that: institute
The oxidant stated is hydrogen peroxide.
The preparation method of solvent-borne type modified aluminum oxide polishing fluid the most according to claim 1, it is characterised in that: institute
Addition preservative that also can be suitable in the polishing fluid stated, corrosion inhibiter.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587474A (en) * | 2018-03-25 | 2018-09-28 | 湖南皓志科技股份有限公司 | A kind of alumina powder polishing fluid and preparation method thereof |
| CN108997940A (en) * | 2018-06-04 | 2018-12-14 | 上海映智研磨材料有限公司 | Chemical mechanical polishing liquid suitable for sapphire polishing |
| CN109321141A (en) * | 2018-11-02 | 2019-02-12 | 山东天岳先进材料科技有限公司 | A method of preparing the stability-enhanced silicon carbide chemical mechanical polishing liquid of pH |
| CN109554119A (en) * | 2018-11-02 | 2019-04-02 | 山东天岳先进材料科技有限公司 | A kind of stability-enhanced silicon carbide chemical mechanical polishing liquid of pH and its application |
| CN110256968A (en) * | 2019-05-29 | 2019-09-20 | 湖南皓志科技股份有限公司 | A kind of alumina polishing solution and preparation method thereof for copper polishing |
| WO2020087721A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | Chemical-mechanical polishing solution for silicon carbide having increased ph stability, preparation method therefor, and use thereof |
| CN111518478A (en) * | 2020-06-15 | 2020-08-11 | 宁波日晟新材料有限公司 | Silicon carbide polishing solution and application thereof |
| CN112341994A (en) * | 2020-12-20 | 2021-02-09 | 长沙县新光特种陶瓷有限公司 | Production method of ultra-precise polishing abrasive |
| CN113499784A (en) * | 2021-08-05 | 2021-10-15 | 湖南立晟新材料有限公司 | Formula material of porous alumina and preparation method thereof |
| CN113563803A (en) * | 2021-08-31 | 2021-10-29 | 昆山捷纳电子材料有限公司 | Polishing solution containing alumina-boron carbide hybrid particles and preparation method thereof |
| CN115851135A (en) * | 2022-11-28 | 2023-03-28 | 宁波平恒电子材料有限公司 | Stainless steel polishing solution and preparation method and application thereof |
| CN116855176A (en) * | 2023-06-26 | 2023-10-10 | 东莞市海发科技发展有限公司 | Metal surface treatment polishing solution and preparation method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587474A (en) * | 2018-03-25 | 2018-09-28 | 湖南皓志科技股份有限公司 | A kind of alumina powder polishing fluid and preparation method thereof |
| CN108997940B (en) * | 2018-06-04 | 2021-01-19 | 上海映智研磨材料有限公司 | Chemical mechanical polishing solution suitable for sapphire polishing |
| CN108997940A (en) * | 2018-06-04 | 2018-12-14 | 上海映智研磨材料有限公司 | Chemical mechanical polishing liquid suitable for sapphire polishing |
| CN109321141A (en) * | 2018-11-02 | 2019-02-12 | 山东天岳先进材料科技有限公司 | A method of preparing the stability-enhanced silicon carbide chemical mechanical polishing liquid of pH |
| CN109554119A (en) * | 2018-11-02 | 2019-04-02 | 山东天岳先进材料科技有限公司 | A kind of stability-enhanced silicon carbide chemical mechanical polishing liquid of pH and its application |
| WO2020087721A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | Chemical-mechanical polishing solution for silicon carbide having increased ph stability, preparation method therefor, and use thereof |
| CN110256968A (en) * | 2019-05-29 | 2019-09-20 | 湖南皓志科技股份有限公司 | A kind of alumina polishing solution and preparation method thereof for copper polishing |
| CN111518478A (en) * | 2020-06-15 | 2020-08-11 | 宁波日晟新材料有限公司 | Silicon carbide polishing solution and application thereof |
| CN112341994A (en) * | 2020-12-20 | 2021-02-09 | 长沙县新光特种陶瓷有限公司 | Production method of ultra-precise polishing abrasive |
| CN113499784A (en) * | 2021-08-05 | 2021-10-15 | 湖南立晟新材料有限公司 | Formula material of porous alumina and preparation method thereof |
| CN113563803A (en) * | 2021-08-31 | 2021-10-29 | 昆山捷纳电子材料有限公司 | Polishing solution containing alumina-boron carbide hybrid particles and preparation method thereof |
| CN115851135A (en) * | 2022-11-28 | 2023-03-28 | 宁波平恒电子材料有限公司 | Stainless steel polishing solution and preparation method and application thereof |
| CN116855176A (en) * | 2023-06-26 | 2023-10-10 | 东莞市海发科技发展有限公司 | Metal surface treatment polishing solution and preparation method thereof |
| CN116855176B (en) * | 2023-06-26 | 2024-03-12 | 东莞市海发科技发展有限公司 | Metal surface treatment polishing solution and preparation method thereof |
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