CN107699138A - A kind of preparation method of the alumina polishing solution of water-based controlled particle size - Google Patents

A kind of preparation method of the alumina polishing solution of water-based controlled particle size Download PDF

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Publication number
CN107699138A
CN107699138A CN201711051419.XA CN201711051419A CN107699138A CN 107699138 A CN107699138 A CN 107699138A CN 201711051419 A CN201711051419 A CN 201711051419A CN 107699138 A CN107699138 A CN 107699138A
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China
Prior art keywords
polishing solution
preparation
particle size
water
alumina
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CN201711051419.XA
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Chinese (zh)
Inventor
贺文兵
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Noo (shanghai) New Material Technology Co Ltd
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Noo (shanghai) New Material Technology Co Ltd
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Priority to CN201711051419.XA priority Critical patent/CN107699138A/en
Publication of CN107699138A publication Critical patent/CN107699138A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The present invention provides a kind of preparation method of the alumina polishing solution of water-based controlled particle size.Surfactant is added in deionized water first, alpha alumina powder is poured into wherein after stirring, continue stirring to milky white suspension, lubricant stearic acid or zinc stearate are added, hydrogenated triglyceride regulation viscosity is added after the mixed liquor of stabilization to be formed, is stirred, pH adjusting agent is added to adjust pH in the range of 7~9, continue to stir, be eventually adding defoamer de-bubble, you can obtain the alumina polishing solution with excellent polishing performance.

Description

A kind of preparation method of the alumina polishing solution of water-based controlled particle size
Technical field
The present invention relates to a kind of preparation method of the alumina polishing solution of water-based controlled particle size, belong to chemical mechanical polishing liquid Field.
Background technology
Alpha-alumina is also known as corundum, and the 9th grade is ranked in Mohs scale, has very big hardness, and the brill that compares Stone is less expensive, so aluminum oxide turns into the good material of polishing.The high polishing speed of alumina polishing solution can remove backing material Mechanical damage, the processing efficiency of integrated circuit hard material can be improved, the surface smoothness after processing is better than white fused alumina Polishing effect.But industrial alumina polishing solution free settling, granularity heterogeneity at this stage, easily produce new cut after a polish Damage, has a strong impact on polishing effect and stability.
This patent adjusting process project, is strictly controlled by improving traditional preparation methods while surfactant is introduced Viscosity, the dosage of acid-base value and addition step processed, while the suspension stability of alumina particle is improved, can also strictly be controlled Particle size processed and distributed area, improve the particle homogeneity of alumina particle.This method had both reduced the use of surfactant Amount, it also avoid that polishing speed present in conventional polishing fluid is low, processes the problems such as secondary scratch damage, substantially increase oxidation The stability and polishing performance of aluminium polishing fluid.
The content of the invention
It is an object of the invention to overcome prior art to prepare particle heterogeneity, surface-active existing for alumina polishing solution A kind of defects such as agent dosage is big, polishing efficiency is low, there is provided the polishing fluid that homogeneous grain diameter is controllable, reaction time is short and polishing efficiency is high Preparation method.Alumina polishing solution prepared by this method has good stability and polishing performance.
To reach above-mentioned expected purpose, the present invention adopts the following technical scheme that:
A kind of preparation method of the alumina polishing solution of water-based controlled particle size, it is characterised in that the specific steps of this method For:
1~5 part of (being mass ratio below) surfactant is added in 40~80 parts of deionized waters first, stirring is equal It is even that mixed liquor is made;
10~30 parts of alpha-alumina powders are poured into liquid made from step a, continue stirring to controllable milky white of granularity Color suspension;
5~15 parts of lubricant stearic acids or zinc stearate are added in suspension made from step b, stabilization to be formed is mixed 1~5 part of hydrogenated triglyceride regulation viscosity is added after closing liquid, is stirred;
Add 1~10 part of pH adjusting agent and adjust pH value between 7~9, continue to stir;
Finally, 0.1~1 part of defoamer de-bubble is added, you can obtain the alumina polishing solution with excellent polishing performance.
The preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that institute The surfactant for stating step a is embedding for OP serial (condensation product of alkyl phenol and oxirane), sodium hexadecyl sulfate, propane diols Section polyester, polyoxyethylene polyoxypropylene copolymer or sodium polymethacrylate.
The preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that institute The controllable key point of granularity for stating step b is the mixing time of mixed liquor, and mixing time is that 30 minutes granularities are 1.2 microns, Mixing time is that 60 minutes granularities are 0.9 micron, and mixing time is that 90 minutes granularities are 0.6 micron;To control to 300 nanometers Left and right needs to emulsify 10 minutes using mulser.
The preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that institute The viscosity for stating step c is controlled in 10~1000 centipoises.
The preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that institute The pH adjusting agent for stating step d is monoethanolamine, one kind in triethanolamine or its combination.
The preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that institute It is DOW CORNING AFE-7820, BYK333, extra large name Si De modest 7072 or Clariant RA-101X to state defoamer in step e.
The present invention, can be notable using adjusting process project, the dosage of strict control viscosity and acid-base value and addition step Ground improves the uniformity of alumina particle, can be obviously improved particle agglomeration phenomenon of the powder body material in polishing fluid, increases grain The homogeneity in footpath.Alumina polishing solution prepared by the present invention has good stability and polishing performance.
Embodiment
The present invention is described in detail below by instantiation, but protection scope of the present invention is not only restricted to these Examples of implementation.
Embodiment 1:5 parts of (being mass ratio below) Surfactant OPs 9 are added in 40 parts of deionized waters, stirred first Mix and mixed liquor uniformly is made;30 parts of alpha-alumina powders are poured into liquid obtained above, continue stirring 90 minutes to milky white Color suspension, particle diameter is in 0.6 microns;15 parts of lubricant stearic acids or zinc stearate are added in suspension, it is to be formed 1 part of hydrogenated triglyceride regulation viscosity is added after stable mixed liquor, is stirred;Add 8 parts of pH adjusting agent triethanolamines PH value is adjusted to 9, continues to stir;Finally, 1 part of defoamer DOW CORNING AFE-7820 de-bubble is added, you can obtain that there is excellent throwing The alumina polishing solution of optical property.
Embodiment 2:3 parts of (being mass ratio below) surfactant sodium hexadecyl sulfates are added to 55 parts and gone first In ionized water, stir and mixed liquor is made;23 parts of alpha-alumina powders are poured into liquid obtained above, continue stirring 60 Minute, particle diameter was in 0.9 microns to milk-white coloured suspension;10 parts of lubricant stearic acids or zinc stearate are added to suspension In, 2 parts of hydrogenated triglyceride regulation viscosity are added after the mixed liquor of stabilization to be formed, are stirred;Add 6 parts of pH adjusting agents Monoethanolamine adjusts pH value to 8, continues to stir;Finally, 1 part of defoamer BYK333 de-bubble is added, you can obtain that there is excellent polishing The alumina polishing solution of performance.
Embodiment 3:2 parts of (being mass ratio below) surfactant polyoxyethylene polyoxypropylene copolymers are added first Into 60 parts of deionized waters, stir and mixed liquor is made;20 parts of alpha-alumina powders are poured into liquid obtained above, after To milk-white coloured suspension, particle diameter is in 0.6 microns within 30 minutes for continuous stirring;8 parts of lubricant stearic acids or zinc stearate are added 5 parts of hydrogenated triglyceride regulation viscosity are added into suspension, after the mixed liquor of stabilization to be formed, are stirred;Add 4.5 Part pH adjusting agent triethanolamine adjusts pH value to 8, continues to stir;Finally, 0.5 part of defoamer sea name Si De modest 7072 is added to remove Bubble, you can obtain the alumina polishing solution with excellent polishing performance.
Embodiment 4:1 part of (being mass ratio below) surfactant sodium polymethacrylate is added to 80 parts and gone first In ionized water, stir and mixed liquor is made;10 parts of alpha-alumina powders are poured into liquid obtained above, continue mulser To milk-white coloured suspension, particle diameter is in 300 rans within 10 minutes for emulsification;5 parts of lubricant stearic acids or zinc stearate are added to 2.9 parts of hydrogenated triglyceride regulation viscosity are added in suspension, after the mixed liquor of stabilization to be formed, are stirred;Add 1 part PH adjusting agent monoethanolamine adjusts pH value to 7, continues to stir;Finally, 0.1 part of defoamer Clariant RA-101X de-bubble is added, you can Obtain the alumina polishing solution with excellent polishing performance.
Above example is used for illustrative purposes only, rather than limitation of the present invention, the technology people about technical field Member, without departing from the spirit and scope of the present invention, can also make various conversion or modification, therefore all equivalent Technical scheme should also belong to scope of the invention, should be limited by each claim.

Claims (6)

1. a kind of preparation method of the alumina polishing solution of water-based controlled particle size, it is characterised in that this method concretely comprises the following steps:
A. 1~5 part of (being mass ratio below) surfactant is added in 40~80 parts of deionized waters, stirred first Mixed liquor is made;
B. 10~30 parts of alpha-alumina powders are poured into liquid made from step a, continues stirring to the controllable milky of granularity Suspension;
C. 5~15 parts of lubricant stearic acids or zinc stearate are added in suspension made from step b, the mixing of stabilization to be formed 1~5 part of hydrogenated triglyceride regulation viscosity is added after liquid, is stirred;
D. add 1~10 part of pH adjusting agent and adjust pH value between 7~9, continue to stir;
E. it is last, add 0.1~1 part of defoamer de-bubble, you can obtain the alumina polishing solution with excellent polishing performance.
2. the preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that described Step a surfactant is OP serial (condensation product of alkyl phenol and oxirane), sodium hexadecyl sulfate, propylene glycol block Polyester, polyoxyethylene polyoxypropylene copolymer or sodium polymethacrylate.
3. the preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that described The controllable key point of step b granularity is the mixing time of mixed liquor, and mixing time is that 30 minutes granularities are 1.2 microns, is stirred It is that 60 minutes granularities are 0.9 micron to mix the time, and mixing time is that 90 minutes granularities are 0.6 micron;To control to 300 nanometers of left sides It is right to need to emulsify 10 minutes using mulser.
4. the preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that described Step c viscosity is controlled in 10~1000 centipoises.
5. the preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that described Step d pH adjusting agent is monoethanolamine, one kind in triethanolamine or its combination.
6. the preparation method of the alumina polishing solution of water-based controlled particle size according to claim 1, it is characterised in that described Defoamer is DOW CORNING AFE-7820, BYK333, extra large name Si De modest 7072 or Clariant RA-101X in step e.
CN201711051419.XA 2017-10-31 2017-10-31 A kind of preparation method of the alumina polishing solution of water-based controlled particle size Pending CN107699138A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109021834A (en) * 2018-08-29 2018-12-18 德米特(苏州)电子环保材料有限公司 A kind of resin lens polishing fluid of alumina host and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102746795A (en) * 2012-06-18 2012-10-24 工业和信息化部电子第五研究所华东分所 Polishing solution for printed circuit microsections and preparation method thereof
CN103937413A (en) * 2014-03-21 2014-07-23 深圳市宇泰隆科技有限公司 Aluminum oxide polishing solution for alloy polishing and preparation method thereof
CN103980819A (en) * 2014-05-28 2014-08-13 南京航空航天大学 Method for preparing high-dispersion ultrafine alumina polishing solution
CN104031560A (en) * 2013-03-07 2014-09-10 天津市乾宇超硬科技有限公司 Water-based diamond polishing solution used for crystal processing
CN104559798A (en) * 2014-12-24 2015-04-29 上海新安纳电子科技有限公司 Alumina-based chemical mechanical polishing slurry

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102746795A (en) * 2012-06-18 2012-10-24 工业和信息化部电子第五研究所华东分所 Polishing solution for printed circuit microsections and preparation method thereof
CN104031560A (en) * 2013-03-07 2014-09-10 天津市乾宇超硬科技有限公司 Water-based diamond polishing solution used for crystal processing
CN103937413A (en) * 2014-03-21 2014-07-23 深圳市宇泰隆科技有限公司 Aluminum oxide polishing solution for alloy polishing and preparation method thereof
CN103980819A (en) * 2014-05-28 2014-08-13 南京航空航天大学 Method for preparing high-dispersion ultrafine alumina polishing solution
CN104559798A (en) * 2014-12-24 2015-04-29 上海新安纳电子科技有限公司 Alumina-based chemical mechanical polishing slurry

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109021834A (en) * 2018-08-29 2018-12-18 德米特(苏州)电子环保材料有限公司 A kind of resin lens polishing fluid of alumina host and preparation method thereof

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