CN101974296A - Core/shell type composite nano abrasive silicon slice polishing liquid - Google Patents
Core/shell type composite nano abrasive silicon slice polishing liquid Download PDFInfo
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- CN101974296A CN101974296A CN2010105430281A CN201010543028A CN101974296A CN 101974296 A CN101974296 A CN 101974296A CN 2010105430281 A CN2010105430281 A CN 2010105430281A CN 201010543028 A CN201010543028 A CN 201010543028A CN 101974296 A CN101974296 A CN 101974296A
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Abstract
The invention discloses a core/shell type composite nano abrasive silicon slice polishing liquid which can lower the roughness of a polished surface, is convenient for cleaning, has no corrosion on equipment, and is prepared from the following components by weight percent: 5-40% of core/shell type composite nano abrasive, 0.5-5% of chelant, 1-5% of dispersing agent, 1-5% of polyether surfactant, 1-10% of pH regulator and the balance pure water, wherein the core/shell type composite nano abrasive is an inorganic core/shell type composite nano particle with the particle size of 200-2000nm, the core thereof is one of SiO2, Al2O3 or diamond, and the shell thereof is an acrylate main-chain polymer; and the pH value of the polishing liquid is 9.0-12.0.
Description
Technical field
The present invention relates to a kind of Wafer Chemical Mechanical Polishing polishing fluid, especially a kind ofly reduce the glazed surface roughness, clean convenient, to the free from corrosion core/shell type composite Nano of equipment abrasive material silicon slice polishing liquid.
Background technology
Silicon chip is the main substrate material of unicircuit (IC), and its surfaceness is one of important factor that influences unicircuit etching live width.Along with improving constantly of unicircuit integrated level, constantly the reducing of characteristic dimension, also more and more higher to the requirement of the working accuracy of silicon chip and surface quality.At present, semicon industry association (SIA) for characteristic dimension be the silicon chip of 0.065 ~ 0.13 μ m require be: overall planeness (GBIR) reaches nanometer and Subnano-class, very little unrelieved stress and affected layer or the not damaged in surface less than 2 μ m, surfaceness, promptly the surface finish of silicon chip processing, surfaceness, surface imperfection etc. is proposed higher requirements.
At present, utilize chemically machinery polished (CMP) technology that silicon chip surface is carried out planarization, become ic manufacturing technology and entered deep-submicron one of requisite processing step of Age of Technology later on.CMP (Chemical Mechanical Polishing) process is under certain downward pressure silicon chip and polishing block/polishing pad to be kept rotation, and polishing fluid is imported on the polishing pad, under the synergy of chemistry and machinery, obtains high-quality polished silicon slice.In chemical mechanical polishing liquid, abrasive material plays keying action, and the abrasive material that uses is mainly selected the solid inorganic abrasive material for use at present, as silicon oxide, aluminum oxide, diamond, oxidation decorations, silicon nitride etc.In the polishing process of silicon chip, because the hardness of abrasive material is bigger in the polishing fluid, the damage to the surface in the polishing process is more serious, not only causes surfaceness bigger, also is prone to surface imperfection such as polishing cut, pit.Therefore, how to address the above problem is the research focus of industry always.
Summary of the invention
The present invention is in order to solve the above-mentioned technical problem of existing in prior technology, provide a kind of and reduce the glazed surface roughness, clean convenient, to the free from corrosion core/shell type composite Nano of equipment abrasive material silicon slice polishing liquid.
Technical solution of the present invention is: a kind of core/shell type composite Nano abrasive material silicon slice polishing liquid, it is characterized in that forming by core/shell type composite Nano abrasive material, promoting agent, dispersion agent, sequestrant, pH regulator agent and pure water, the pH value is 9.0 ~ 12.0, and the mass percent of each raw material is:
Core/shell type composite Nano abrasive material 5% ~ 40%
Sequestrant 0.5% ~ 5%
Dispersion agent 1% ~ 5%
Polyethet surfactant 1% ~ 5%
PH regulator agent 1% ~ 10%
The pure water surplus
Described core/shell type composite Nano abrasive material is that particle diameter is inorganic-organic core/shell type composite nanometer particle of 200 ~ 2000nm, and kernel is SiO
2, Al
2O
3Or a kind of in the diamond, shell is an acrylate polymeric chain polymerization thing.
Described acrylate polymeric chain polymerization thing is at least a polymkeric substance in methoxy polyethylene glycol methacrylate-styrene polymer, oxyethyl group polyethylene glycol methacrylate-styrene polymer, methacrylic ester, the ethyl propylene acid esters.
Described sequestrant is at least a in ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, nitrilotriacetic acid(NTA) and ammonium salt thereof or the sodium salt.
Described dispersion agent is at least a in ethylene oxide-propylene oxide block copolymer, polyvinyl alcohol, polyvinyl alcohol segmented copolymer or polystyrene block copolymer, polyacrylic acid or polyacrylate, polyoxyethylene glycol, polymine, the quaternary ammonium salt cationic surfactant.
Described polyethet surfactant is at least a in isomery polyoxyethylenated alcohol, the aliphatic alcohol polyethenoxy polyethenoxy ether, and general molecular formula is respectively R
1O (C
2H
4O)
mH, R
2O (C
2H
4O)
m(C
3H
6O)
nH, wherein R
1Be the alkyl of C10-C14, R
2Be the alkyl of C10-C18, m and n are 3 ~ 20, are respectively the aggregate number of Oxyranyle and propylene oxide.
Described pH regulator agent is at least a in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl benzyl ammonium hydroxide, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, diethylamine, triethylamine, quadrol, monoethanolamine, diethanolamine, trolamine, Yi Bingchunan, diisopropanolamine (DIPA), the tri-isopropanolamine.
Of the present invention inorganic-shell of organic core/shell type composite Nano abrasive material is that hardness is low and viscoelastic acrylate polymeric chain polymerization thing is arranged, and has reduced hardness of grain.Under pressurization, acceleration polishing condition, shell has played shock absorption, substitutes " the hard impact " with workpiece surface with " Elastic Contact ", thereby has avoided polishing cut and surface damage.Carrying out along with polishing process, the localized hyperthermia that friction condition produces down can make the branch chain molecule of shell rupture, expose kernel (inorganic abrasive particle) surface gradually, the progressive mode that makes polishing be able to a kind of " flexible polishing " carries out, thereby improve the microcosmic situation of surface of polished, reduce roughness.Simultaneously, polishing fluid of the present invention is an alkalescence, and it is convenient that the polishing back is cleaned, and equipment is not had corrosion, can prolong service life of equipment, cut down finished cost.
Embodiment:
Embodiment 1:
Be made up of core/shell type composite Nano abrasive material, promoting agent, dispersion agent, sequestrant, pH regulator agent and pure water, the pH value is 9.0 ~ 12.0, and the mass percent of each raw material is:
Core/shell type composite Nano abrasive material 5% ~ 40%
Sequestrant 0.5% ~ 5%
Dispersion agent 1% ~ 5%
Polyethet surfactant 1% ~ 5%
PH regulator agent 1% ~ 10%
The pure water surplus
Described core/shell type composite Nano abrasive material is that particle diameter is inorganic-organic core/shell type composite nanometer particle of 200 ~ 2000nm, and kernel is for carrying out the SiO of surface modification with propylene phthalein chlorine
2, Al
2O
3Or a kind of in the diamond, shell is an acrylate polymeric chain polymerization thing.
The making method of core/shell type composite Nano abrasive material is to adopt conventional nanometer abrasive method of emulsion polymerization to obtain, and concrete grammar is as follows: with inorganic abradant (SiO
2, Al
2O
3Or diamond) carries out surface modification with propylene phthalein chlorine, be positioned over subsequently in the acrylate polymeric chain polymerization thing solution, utilize surface-modifying agent such as silane to make coupling agent, under 110 ℃ of temperature, carry out emulsion polymerization, reaction times is 12 hours, its percentage of grafting is 12%, obtains inorganic-organic core/shell type composite Nano abrasive particle that the surface coats acrylate polymeric chain polymerization thing, and median size is 1889nm.
Action principle is that the acrylate polymeric polymkeric substance is by silane-modified, and then can carry out conventional Raolical polymerizable with nano-oxide (aluminum oxide, silicon-dioxide etc.) abrasive surface through surface modification, thereby the formation kernel is an inorganic particle, and shell is the composite Nano abrasive material of organic polymer.Can regulate the size, hardness, wetting ability of core/shell type composite Nano abrasive material etc. by the size of control grafting polymer segment.
Described acrylate polymeric chain polymerization thing is at least a polymkeric substance in methoxy polyethylene glycol methacrylate-styrene polymer, oxyethyl group polyethylene glycol methacrylate-styrene polymer, methacrylic ester, the ethyl propylene acid esters.
Described sequestrant is at least a in ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, nitrilotriacetic acid(NTA) and ammonium salt thereof or the sodium salt.
Described dispersion agent is at least a in ethylene oxide-propylene oxide block copolymer, polyvinyl alcohol, polyvinyl alcohol segmented copolymer or polystyrene block copolymer, polyacrylic acid or polyacrylate, polyoxyethylene glycol, polymine, the quaternary ammonium salt cationic surfactant.
Described polyethet surfactant is at least a in isomery polyoxyethylenated alcohol, the aliphatic alcohol polyethenoxy polyethenoxy ether, and general molecular formula is respectively R
1O (C
2H
4O)
mH, R
2O (C
2H
4O)
m(C
3H
6O)
nH, wherein R
1Be the alkyl of C10-C14, R
2Be the alkyl of C10-C18, m and n are 3 ~ 20, are respectively the aggregate number of Oxyranyle and propylene oxide.
Described pH regulator agent is at least a in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl benzyl ammonium hydroxide, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, diethylamine, triethylamine, quadrol, monoethanolamine, diethanolamine, trolamine, Yi Bingchunan, diisopropanolamine (DIPA), the tri-isopropanolamine.
Pure water is that its resistance is 18 M at least through the filtering water of ion exchange resin.
Embodiment 1pH value is preferably 10.0-11.5.
Each raw material is selected in its mass range, and total mass is 100%.
Preparation method: under the mechanical stirring condition, the core/shell type composite Nano abrasive material of metering is added to the water, adopt ultra-sonic dispersion, in scattered core/shell type composite Nano abrasive material dispersion liquid, add dispersion agent, polyethet surfactant, sequestrant, after stirring, add the pH value scope that the pH regulator agent is adjusted to be needed, get final product.
Carry out polishing experiments with the embodiment of the invention 1: adopt ZYP280 type polishing machine, polish pressure 3Psi, lower wall rotating speed 100rpm, polishing fluid flow 8 ml/min, adopt Sartorius CP225D type precise electronic balance (precision 0.01mg) that silicon chip before and after the polishing is weighed, calculate its material removing rate, surface of polished is by ZYGO5022 test polishing back silicon chip surface roughness (RMS).
Polishing back material removal rate is R=460 ~ 810nm, surfaceness R
a=0.13 ~ 0.20nm.
Embodiment 2:
Raw material and weight percent are as follows:
(kernel is SiO to core/shell type composite Nano abrasive material
2) 6%;
Disodium EDTA 1%;
Sodium polyacrylate 2%;
Aliphatic alcohol polyethenoxy polyethenoxy ether (L64, BASF AG produces) 2%;
Tetramethylammonium hydroxide 3%;
The pure water surplus.
Method according to embodiment 1 prepares polishing fluid and carries out polishing experiments, and polishing back material removal rate is
R=620nm, surfaceness R
a=0.18nm.
Embodiment 3:
Raw material and weight percent are as follows:
(kernel is Al to core/shell type composite Nano abrasive material
2O
3) 5%;
Diethylene triaminepentaacetic acid(DTPA) 0.5%;
Polyoxyethylene glycol (PEG) 2%;
Aliphatic alcohol polyethenoxy polyethenoxy ether (L64, BASF AG produces) 2%;
Trolamine 5%;
The pure water surplus.
Method according to embodiment 1 prepares polishing fluid and carries out polishing experiments, and polishing back material removal rate is
R=470nm, surfaceness R
a=0.17nm.
Claims (6)
1. a core/shell type composite Nano abrasive material silicon slice polishing liquid is characterized in that being made up of core/shell type composite Nano abrasive material, promoting agent, dispersion agent, sequestrant, pH regulator agent and pure water, and the pH value is 9.0 ~ 12.0, and the mass percent of each raw material is:
Core/shell type composite Nano abrasive material 5% ~ 40%
Sequestrant 0.5% ~ 5%
Dispersion agent 1% ~ 5%
Polyethet surfactant 1% ~ 5%
PH regulator agent 1% ~ 10%
The pure water surplus
Described core/shell type composite Nano abrasive material is that particle diameter is inorganic-organic core/shell type composite nanometer particle of 200 ~ 2000nm, and kernel is SiO
2, Al
2O
3Or a kind of in the diamond, shell is an acrylate polymeric chain polymerization thing.
2. core/shell type composite Nano abrasive material silicon slice polishing liquid according to claim 1 is characterized in that: described acrylate polymeric chain polymerization thing is at least a polymkeric substance in methoxy polyethylene glycol methacrylate-styrene polymer, oxyethyl group polyethylene glycol methacrylate-styrene polymer, methacrylic ester, the ethyl propylene acid esters.
3. core/shell type composite Nano abrasive material silicon slice polishing liquid according to claim 1 and 2 is characterized in that: described sequestrant is at least a in ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, nitrilotriacetic acid(NTA) and ammonium salt thereof or the sodium salt.
4. core/shell type composite Nano abrasive material silicon slice polishing liquid according to claim 3 is characterized in that: described dispersion agent is at least a in ethylene oxide-propylene oxide block copolymer, polyvinyl alcohol, polyvinyl alcohol segmented copolymer or polystyrene block copolymer, polyacrylic acid or polyacrylate, polyoxyethylene glycol, polymine, the quaternary ammonium salt cationic surfactant.
5. core/shell type composite Nano abrasive material silicon slice polishing liquid according to claim 4 is characterized in that: described polyethet surfactant is at least a in isomery polyoxyethylenated alcohol, the aliphatic alcohol polyethenoxy polyethenoxy ether, and general molecular formula is respectively R
1O (C
2H
4O)
mH, R
2O (C
2H
4O)
m(C
3H
6O)
nH, wherein R
1Be the alkyl of C10-C14, R
2Be the alkyl of C10-C18, m and n are 3 ~ 20, are respectively the aggregate number of Oxyranyle and propylene oxide.
6. core/shell type composite Nano abrasive material silicon slice polishing liquid according to claim 1 is characterized in that: described pH regulator agent is at least a in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl benzyl ammonium hydroxide, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, diethylamine, triethylamine, quadrol, monoethanolamine, diethanolamine, trolamine, Yi Bingchunan, diisopropanolamine (DIPA), the tri-isopropanolamine.
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|---|---|---|---|
| CN2010105430281A CN101974296A (en) | 2010-11-12 | 2010-11-12 | Core/shell type composite nano abrasive silicon slice polishing liquid |
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|---|---|---|---|
| CN2010105430281A CN101974296A (en) | 2010-11-12 | 2010-11-12 | Core/shell type composite nano abrasive silicon slice polishing liquid |
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|---|---|
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Family
ID=43574209
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|---|---|---|---|
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| CN103897202A (en) * | 2012-12-28 | 2014-07-02 | 上海新安纳电子科技有限公司 | Preparation method and application of polystyrene/silicon oxide core-shell nano compound abrasive |
| CN104017499A (en) * | 2014-05-19 | 2014-09-03 | 贵州荣清工具有限公司 | Diamond grinding paste |
| CN105579548A (en) * | 2013-08-23 | 2016-05-11 | 戴蒙得创新股份有限公司 | Lapping slurry having a cationic surfactant |
| CN106590530A (en) * | 2016-12-15 | 2017-04-26 | 河北工业大学 | Water-soluble polymer coated special-shaped silica sol, preparation method and application |
| CN106757034A (en) * | 2016-11-28 | 2017-05-31 | 江南大学 | A kind of preparation method of alkalinous metal polishing fluid |
| CN108456508A (en) * | 2018-03-23 | 2018-08-28 | 长江存储科技有限责任公司 | Abrasive particles and its manufacturing method |
| CN108587478A (en) * | 2018-07-03 | 2018-09-28 | 中国人民解放军国防科技大学 | Modified nano silicon dioxide composite polishing solution and application thereof |
| CN110577823A (en) * | 2018-08-20 | 2019-12-17 | 蓝思科技（长沙）有限公司 | Nano abrasive, polishing solution, preparation method and application |
| CN110862773A (en) * | 2019-10-23 | 2020-03-06 | 宁波日晟新材料有限公司 | Core-shell structure nano abrasive polishing solution and preparation method thereof |
| CN110862772A (en) * | 2019-10-23 | 2020-03-06 | 宁波日晟新材料有限公司 | High-efficiency silica sol polishing solution not easy to crystallize and easy to clean and preparation method thereof |
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| CN111117494A (en) * | 2019-12-23 | 2020-05-08 | 肇庆乐华陶瓷洁具有限公司 | Antique brick polishing solution and preparation method and application thereof |
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| CN114163588A (en) * | 2021-12-27 | 2022-03-11 | 上海博莱纳润电子材料有限公司 | Composite abrasive particle of polyacrylamide grafted nano diamond and preparation method and application thereof |
| CN115895452A (en) * | 2022-11-01 | 2023-04-04 | 湖南三安半导体有限责任公司 | Composite polishing solution and preparation method thereof |
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| CN104017499A (en) * | 2014-05-19 | 2014-09-03 | 贵州荣清工具有限公司 | Diamond grinding paste |
| CN104017499B (en) * | 2014-05-19 | 2015-08-19 | 贵州荣清工具有限公司 | A kind of diamond paste |
| CN106757034A (en) * | 2016-11-28 | 2017-05-31 | 江南大学 | A kind of preparation method of alkalinous metal polishing fluid |
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| CN108456508A (en) * | 2018-03-23 | 2018-08-28 | 长江存储科技有限责任公司 | Abrasive particles and its manufacturing method |
| CN108587478B (en) * | 2018-07-03 | 2020-09-25 | 中国人民解放军国防科技大学 | Modified nano silicon dioxide composite polishing solution and application thereof |
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| TWI716185B (en) * | 2019-11-07 | 2021-01-11 | 多鏈科技股份有限公司 | Method for stably dispersing nsp in water |
| CN111117494A (en) * | 2019-12-23 | 2020-05-08 | 肇庆乐华陶瓷洁具有限公司 | Antique brick polishing solution and preparation method and application thereof |
| CN114163588A (en) * | 2021-12-27 | 2022-03-11 | 上海博莱纳润电子材料有限公司 | Composite abrasive particle of polyacrylamide grafted nano diamond and preparation method and application thereof |
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| CN117467410A (en) * | 2023-12-27 | 2024-01-30 | 甬江实验室 | Composite abrasive particles with core-shell structure, preparation method thereof and CMP (chemical mechanical polishing) slurry |
| CN117467410B (en) * | 2023-12-27 | 2024-04-23 | 甬江实验室 | Composite abrasive particles with core-shell structure, preparation method thereof and CMP (chemical mechanical polishing) slurry |
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Application publication date: 20110216 |