CN1063205C - Nanometer silicon dioxide polishing agent and its preparing method - Google Patents
Nanometer silicon dioxide polishing agent and its preparing method Download PDFInfo
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- CN1063205C CN1063205C CN98110778A CN98110778A CN1063205C CN 1063205 C CN1063205 C CN 1063205C CN 98110778 A CN98110778 A CN 98110778A CN 98110778 A CN98110778 A CN 98110778A CN 1063205 C CN1063205 C CN 1063205C
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- agent
- sio
- polishing
- surface treatment
- dispersion stabilizer
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Abstract
The present invention discloses a nanon silicon dioxide (SiO2) polishing agent and a preparation method thereof. The polishing agent is prepared from SiO2 powder, water, a dispersion stabilizer, a moistening regulating agent, a pH regulating agent and a surface treating agent. The content of SiO2 can reach 60 wt% at most, the viscosity of products is less than 0.1Pa. s, and the gravity settling property can keep more than one year. The polishing agent is a polishing material with good properties for the CMP technology, can be used for the rough polishing and the fine polishing of silicon chips and IC working processes, are especially suitable for the flat processing of multiple stratification thin films of large scale integrated circuits, and can be also used for working processes of semiconductor devices, such as the cleanness of the back track CMP of wafers, and working processes of panel displays, poly-crystallization die sets, micro motor systems, vidicon camera tubes, etc. The polishing quality and the polishing speed of the polishing agent are superior to those of native and foreign similar products.
Description
The invention belongs to electron device planarization process field, relate to the silicon-dioxide (SiO that the planarization process of multilayer insulating film and metal level is used in a kind of semiconductor device fabrication process
2) the polishing slip and preparation method thereof.
Along with the fast development of information industry, the integrated degree of electron device is more and more higher, and polylaminate wiring technique then becomes an indispensable technology.When electron device dwindled, the shape of device surface was also complicated, in order to improve the reliability of multilayer wiring, obtained higher qualification rate, and it is very important that the planarization process of device surface just seems.For this reason, numerous scientific and technical personnel have researched and developed planarization process technology separately, and the most successful is that in June, 1992 is by the mechanical mill of IBM and the joint development of Microtechnology company and the polishing technology that chemical corrosion combines, abbreviation CMP technology, (SiO
2) aqueous solution is the most representative at present CMP technology rumbling compound.Its major ingredient is nanometer (SiO
2) powder and water.Because (SiO
2) powder has very high specific surface area, generally at 100m
2More than/the g, has lower apparent density simultaneously, generally at 50kg/m
3About.Therefore, if use common nanometer (SiO
2) powder, just being difficult to prepare the high solid content and the low viscous water-sol, United States Patent (USP) 5116535 and 5246624 discloses two kinds of nanometer (SiO respectively
2) preparation method of colloidal dispersion, wherein (SiO
2) concentration be approximately 35%～65%, (the SiO that it adopts
2) specific surface area of powder requires less than 75m
2/ g is preferably 50m
2/ g, this is a kind of very special (SiO
2) powder, vapor phase process is difficult to reach so low specific surface area usually; United States Patent (USP) 2984629 discloses another kind of nanometer (SiO
2) preparation method of colloidal dispersion, wherein (SiO
2) concentration be approximately 40%, employing be a kind of through mechanically compress, apparent density is up to 100～250kg/m
3Vapor phase process (SiO
2) powder; English Patent 1326574 disclosed method (SiO
2) concentration be approximately 70%, also to (SiO
2) the powder specific surface area proposed specific requirement.
If therefore adopt common nanometer (SiO
2) powder, generally can only obtain (SiO
2) concentration is about 10% the water-sol, viscosity is easily reunited, sedimentation about 1Pa.s, instability, and mean particle size is big, is generally about 800nm, and size distribution is wide, can not satisfy CMP polishing requirement.Other are as only brother's 3050 rumbling compounds of Japan, and adopting white carbon black of industry or water glass is raw material, equally also exists shortcomings such as pulp density is low, viscosity is high, the grinding and polishing performance is not ideal enough.For this reason, research and develop high performance nanometer rumbling compound and become pressing for of branch of industry.
The objective of the invention is to overcome the above-mentioned shortcoming of prior art, disclose a kind of employing vapor phase process or liquid phase method nanometer SiO
2Powder preparing, the powder specific surface area do not need strict restriction, its SiO
2Concentration reach as high as the generally high-performance CMP technology SiO below 0.1Pa.s of 60% (quality), viscosity
2Rumbling compound and preparation method thereof.
Design of the present invention is such: because nanometer SiO
2The powder specific surface area is big, and easily reuniting in dispersion medium such as empty G﹠W forms macrobead, therefore, and with nanometer SiO
2When powder is the main raw material of rumbling compound, (1). must be to SiO
2Powder carries out surface treatment, (2). must carry out water quality modulation, (3) to the water that adds. must add dispersion agent, so that SiO
2In water, can keep good dispersion state, make SiO simultaneously
2The aqueous solution have the characteristics of high density, low viscosity and high dispersion stability.
According to above-mentioned design, the present invention proposes a kind of new SiO
2Rumbling compound, said rumbling compound is by nanometer SiO
2Powder, water, dispersion stabilizer, wetting conditioning agent, pH regulator agent and surface treatment agent are formed, wherein:
(1) .SiO
2Content can be determined according to the requirement of the finished product, reach as high as 60% (wt.);
(2). dispersion stabilizer and surface treatment agent and SiO in the solution
2Proportioning as follows:
Dispersion stabilizer: (SiO
2)=0.01～8.0% (wt.)
Surface treatment agent: (SiO
2)=0.01～8.0% (wt.)
(3). the amount that wetting conditioning agent adds can make the pH value of initial pure water reach 2～4
(4) amount of .pH conditioning agent adding can make the pH value of the finished product reach 8.5～13;
(5). the viscosity＜0.1Pa.s of product
Said dispersion stabilizer is a kind of polymeric surface active agent, one or more in polyoxyethylene, polyvinylpyrrolidone, polypropylene hydrochloric acid, polyvinyl alcohol and the polystyrene block copolymer of commonly used is polyvinyl alcohol, phenol modification, polypropylene glycol or the polyether-modified polydimethylsiloxanecopolymer copolymer.
Said surface treatment agent is a kind of small molecules tensio-active agent, commonly used is thanomin, trolamine, 1,2-propylene glycol, glycerol, 1,3 butylene glycol, 1, one or more in 4-butyleneglycol, ten dihydroxystearic acids, oleic acid, the diisopropanolamine (DIPA).
Said wetting conditioning agent is a kind of acidic substance, one or more that commonly used is in tartrate, saltpetre, Whitfield's ointment, vitriolate of tartar, acetic acid, hydrochloric acid, sulfuric acid, Repone K or the nitric acid.
Said pH regulator agent is a kind of alkaline matter, one or more that commonly used is in ammoniacal liquor, thanomin, trolamine, Yi Bingchunan, aminopropanol, potassium hydroxide or the diisopropanolamine (DIPA).
Said rumbling compound also is preparation like this:
(1). in high purity deionized water, add wetting conditioning agent, high purity deionized water is carried out wettability handle, regulate between pH to 2～4 of water, make deionized water nanometer SiO
2Powder has best wettability;
(2). in dispersator, make high purity deionized water and nanometer SiO
2The powder thorough mixing disperses;
(3). add surface treatment agent, less coacervate in the dispersion system and primary nanoparticle are carried out surface modification treatment, stop less coacervate and primary nanoparticle to be reunited once more;
(4). add dispersion stabilizer dispersion system is carried out the stably dispersing processing, improve the gravity settling performance of dispersion system;
(5). add the pH regulator agent, the pH that regulates dispersion system is 8.5～13.0;
(6). dispersion system is sieved,, promptly obtain the said nanometer SiO of the present invention to remove large granular impurity
2Rumbling compound.
Below will the invention will be further elaborated by embodiment.
Embodiment 1
Add nitric acid in the high purity deionized water of 250 grams, the pH that makes solution is 2.0, adds nanometer SiO
2Powder 250 grams, 1,3-butyleneglycol 2.5 grams and polyvinyl alcohol 2.5 grams, dispersed with stirring is 1.5 hours in stirring dispersion machine, add 325 gram water again, restir disperseed 2.5 hours, added potassium hydroxide, the pH to 10.0 of regulator solution, dispersed with stirring obtained the CMP polishing slip of 30.0% (wt.) after 10 minutes after screening in stirring dispersion machine.Through the gravity settling performance test, sedimentation can not take place in 1 year, the viscosity of slip is 3.50 * 10
-2Pa.s, density is 1.20 * 10
3Kg/m
3, slip is tested on the ZetaSizer4 particle size analyzer of Britain Malvern company, and mean particle size is 150nm, and polydispersity index is 1.26.
Embodiment 2
Add nitric acid in the high purity deionized water of 250 grams, the pH that makes solution is 2.5, adds nanometer SiO
2Powder 5 grams, trolamine 0.05 gram and polyvinyl alcohol 0.05 gram, dispersed with stirring is 1.5 hours in stirring dispersion machine, add 745 gram water again, restir disperseed 2.5 hours, add ammoniacal liquor, the pH to 10.0 of regulator solution, dispersed with stirring obtained the CMP polishing slip of 0.5% (wt.) after 10 minutes after screening in stirring dispersion machine.Through the gravity settling performance test, sedimentation can not take place in 1 year, the viscosity of slip is 3.0 * 10
-2Pa.s, density is 1.18 * 10
3Kg/m
3, slip is tested on the ZetaSicer of Britain Malvern company 4 particle size analyzers, and mean particle size is 185nm, and polydispersity index is 1.12.
Embodiment 3
Add hydrochloric acid in the high purity deionized water of 300 grams, the pH that makes solution is 4.0, adds nanometer SiO
2Powder 700 grams, 1, polyoxyethylene 7.0 grams of 4-butyleneglycol 7.0 grams and phenol modification, dispersed with stirring is 1.5 hours in stirring dispersion machine, add 150 gram water again, restir disperseed 2.5 hours, added potassium hydroxide, the pH to 10.0 of regulator solution, dispersed with stirring obtained the CMP polishing slip of 60.0% (wt.) after 10 minutes after screening in stirring dispersion machine.Through the gravity settling performance test, sedimentation can not take place in 1 year, the viscosity of slip is 3.2 * 10
-2Pa.s, density is 1.19 * 10
3Kg/m
3, slip is tested on the ZetaSizer of Britain Malvern company 4 particle size analyzers, and mean particle size is 175nm, and polydispersity index is 1.12.
Embodiment 4～9
When preparation process identical with condition with embodiment 1, and prepared rumbling compound when adopting different dispersion stabilizers, wetting conditioning agent, pH regulator agent and surface treatment agent, its every index is as follows:
Table 1.
A--polyvinyl alcohol and polystyrene block copolymer in the table 1.
The polydimethylsiloxanecopolymer copolymer that B--is polyether-modified
C--polyvinylpyrrolidone+polyvinyl alcohol
Embodiment 10
Preparation process is identical with embodiment 1 with condition, and adopting (aminopropanol+oxygen potassium oxide) is the pH regulator agent, regulates pH=8.5, and mean particle size is 160nm, and polydispersity index is 1.25.
Embodiment 11
When preparation process is identical with embodiment 1 with condition, adopting (aminopropanol+potassium hydroxide) be the pH regulator agent, adjusting pH=8.5, and the result is as follows: mean particle size is 150nm.
When adopting blended dispersion stabilizer, wetting conditioning agent, pH regulator agent and surface treatment agent, the mass ratio of each component is 1: 1.
Embodiment 12～14
Preparation process is identical with embodiment 1 with condition, and the surface treatment dosage of employing is respectively 0.25 gram, 25 grams and 5 grams, and the result is as follows: mean particle size is 180nm, and polydispersity index is 1.2.
Embodiment 15～17
Preparation process is identical with embodiment 1 with condition, and the stably dispersing dosage of employing is respectively 0.25 gram, 25 grams and 5 grams, and the result is as follows: mean particle size is 175nm, and polydispersity index is 1.15.
Through the gravity settling performance test, sedimentation can not take place in 1 year by the prepared rumbling compound of embodiment 4～17.
Embodiment 18
Add sulfuric acid in the high purity deionized water of 200 grams, the pH that makes solution is 2.2, adds nanometer SiO
2Polyoxyethylene 2.0 grams of powder 200 grams, Diisopropylamine 2.0 grams and nonyl phenol modification, dispersed with stirring is 1.5 hours in stirring dispersion machine, add 395 gram water again, restir disperseed 2.5 hours, add potassium hydroxide, the pH to 13.0 of regulator solution, dispersed with stirring obtained the CMP polishing slip of 25.0% (wt.) after 10 minutes after screening in stirring dispersion machine.Through the gravity settling performance test, sedimentation can not take place in 1 year, the viscosity of slip is 2.24 * 10
-2Pa.s, density is 1.17 * 10
3Kg/m
3, slip is tested on the ZetaSizer of Britain Malvern company 4 particle size analyzers, and mean particle size is 170nm, and polydispersity index is 1.12.
Embodiment 19
Add sulfuric acid in the high purity deionized water of 200 grams, the pH that makes solution is 2.0, adds nanometer SiO
2Polyoxyethylene 2.0 grams of powder 322 grams, Diisopropylamine 2.0 grams and nonyl phenol modification, dispersed with stirring is 1.5 hours in stirring dispersion machine, add 1620 gram water again, restir disperseed 2.5 hours, add potassium hydroxide, the pH to 10.2 of regulator solution, dispersed with stirring obtained the CMP polishing slip of 15.0% (wt.) after 10 minutes after screening in stirring dispersion machine.Through the gravity settling performance test, sedimentation can not take place in 1 year, the viscosity of slip is 3.0 * 10
-2Pa.s, density is 1.12 * 10
3Kg/m
3, slip is tested on the ZetaSizer of Britain Malvern company 4 particle size analyzers, and mean particle size is 164nm.
Embodiment 20
With embodiment 1 and 2 two kinds of slips of embodiment respectively with the dilution proportion of high purity deionized water by 1: 10 (quality), on TNJ80-21 type polishing machine, polish test, polish pressure is 0.250kg/cm
2, polish temperature is 30 ℃, and flow is 180 ml/min, and the result shows that two kinds of slips all have higher polishing speed and quality of finish, meet or exceed the processing request of microelectronic product, and are as follows:
As seen from the above-described embodiment, the concentration of the said rumbling compound of the present invention can reach 60%, viscosity less than the 0.1Pa.s mean particle size less than 200nm, the gravity settling performance is more than 1 year, it is the polishing material that a kind of CMP technology of excellent property is used, this rumbling compound can be used for the thick throwing and smart the throwing and the IC course of processing of silicon chip, be specially adapted to the planarization process of large-scale integrated circuit multiple stratification film, the course of processing that also can be used for the semiconducter device such as back road CMP cleaning in brilliant garden, flat-panel screens, the polycrystallization module, microelectromechanical-systems, the course of processing of vidicon etc., its quality of finish and polishing velocity all are better than similar products at home and abroad.
Claims (3)
1. nanometer silicon dioxide polishing agent is characterized in that:
(1) rumbling compound is by nanometer SiO
2Powder, water, dispersion stabilizer, wetting conditioning agent, pH regulator agent and surface treatment agent are formed;
(2). dispersion stabilizer and surface treatment agent and SiO in the rumbling compound
2Proportioning be:
Dispersion stabilizer: (SiO
2)=0.01～8.0% (wt.)
Surface treatment agent: (SiO
2)=0.01～8.0% (wt.);
The amount that wetting conditioning agent adds can make the pH value of initial pure water reach 2～4;
The amount that the pH regulator agent adds can make the pH value of the finished product reach 8.5～13;
Said dispersion stabilizer is a kind of polymeric surface active agent; Said surface treatment agent is a kind of small molecules tensio-active agent; Said wetting conditioning agent is a kind of acidic substance, and said pH regulator agent is a kind of alkaline matter;
Said dispersion stabilizer is polyoxyethylene, polyvinylpyrrolidone, polypropylene hydrochloric acid, polyvinyl alcohol and polystyrene block copolymer, the polypropylene glycol of polyvinyl alcohol, phenol modification or in the polyether-modified polydimethylsiloxanecopolymer copolymer one or more;
Said surface treatment agent is thanomin, trolamine, 1,2-propylene glycol, glycerol, 1,3 butylene glycol, 1, one or more in 4-butyleneglycol, ten dihydroxystearic acids, oleic acid, the diisopropanolamine (DIPA);
Said wetting conditioning agent is one or more in tartrate, saltpetre, Whitfield's ointment, vitriolate of tartar, acetic acid, hydrochloric acid, sulfuric acid, Repone K or the nitric acid;
Said pH regulator agent is one or more in ammoniacal liquor, thanomin, trolamine, Yi Bingchunan, aminopropanol, potassium hydroxide or the diisopropanolamine (DIPA).
2. rumbling compound as claimed in claim 1 is characterized in that: the viscosity＜0.1Pa.s of rumbling compound.
3. the preparation method of a nanometer silicon dioxide polishing agent is characterized in that mainly comprising the steps:
(1). in high purity deionized water, add wetting conditioning agent, regulate between pH to 2～4 of water;
(2). in dispersator, add nanometer SiO
2Powder, surface treatment agent, dispersion stabilizer and contain the high purity deionized water of wetting conditioning agent make it thorough mixing and disperse; The add-on of dispersion stabilizer and surface treatment agent is:
Dispersion stabilizer: (SiO
2)=0.01～8.0% (wt.)
Surface treatment agent: (SiO
2)=0.01～8.0% (wt.)
(3). add the pH regulator agent, the pH that regulates dispersion system is 8.5～13.0, promptly obtains nanometer SiO
2Rumbling compound;
Said dispersion stabilizer is polyoxyethylene, polyvinylpyrrolidone, polypropylene hydrochloric acid, polyvinyl alcohol and polystyrene block copolymer, the polypropylene glycol of polyvinyl alcohol, phenol modification or in the polyether-modified polydimethylsiloxanecopolymer copolymer one or more;
Said surface treatment agent is thanomin, trolamine, 1,2-propylene glycol, glycerol, 1,3 butylene glycol, 1, one or more in 4-butyleneglycol, ten dihydroxystearic acids, oleic acid, the diisopropanolamine (DIPA);
Said wetting conditioning agent is one or more in tartrate, saltpetre, Whitfield's ointment, vitriolate of tartar, acetic acid, hydrochloric acid, sulfuric acid, Repone K or the nitric acid;
Said pH regulator agent is one or more in ammoniacal liquor, thanomin, trolamine, Yi Bingchunan, aminopropanol, potassium hydroxide or the diisopropanolamine (DIPA).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98110778A CN1063205C (en) | 1998-04-16 | 1998-04-16 | Nanometer silicon dioxide polishing agent and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98110778A CN1063205C (en) | 1998-04-16 | 1998-04-16 | Nanometer silicon dioxide polishing agent and its preparing method |
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|---|---|
| CN1194288A CN1194288A (en) | 1998-09-30 |
| CN1063205C true CN1063205C (en) | 2001-03-14 |
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|---|---|---|---|
| CN98110778A Expired - Fee Related CN1063205C (en) | 1998-04-16 | 1998-04-16 | Nanometer silicon dioxide polishing agent and its preparing method |
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| CN1109651C (en) * | 2000-11-14 | 2003-05-28 | 北京化工大学 | Carbonization process to prepare nanometer silica |
| CN1100104C (en) * | 2000-12-01 | 2003-01-29 | 清华大学 | Nm-class polishing liquid and its preparing process |
| JP4083528B2 (en) * | 2002-10-01 | 2008-04-30 | 株式会社フジミインコーポレーテッド | Polishing composition |
| JP2004247605A (en) * | 2003-02-14 | 2004-09-02 | Toshiba Corp | Cmp slurry and manufacturing method of semiconductor device |
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| CN100556619C (en) * | 2006-05-31 | 2009-11-04 | 天津晶岭微电子材料有限公司 | Method for controlling surface roughness of sapphire substrate material |
| CN102101976A (en) * | 2009-12-18 | 2011-06-22 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN102101981B (en) * | 2009-12-18 | 2014-08-20 | 安集微电子（上海）有限公司 | Polishing solution used for planarization of dielectric material |
| CN103194148B (en) * | 2013-04-23 | 2014-10-22 | 清华大学 | Chemical-mechanical polishing aqueous composition and use thereof |
| CN103756570A (en) * | 2013-12-26 | 2014-04-30 | 常熟市美尔特金属制品有限公司 | Ultra-fine polished wax for stainless steel metal product |
| CN103740280B (en) * | 2013-12-31 | 2015-08-12 | 深圳市力合材料有限公司 | A kind ofly be applicable to polishing composition of silicon wafer edge polishing and preparation method thereof |
| CN104889898B (en) * | 2015-02-10 | 2017-04-05 | 衢州学院 | A kind of silicon polished hydrolytic sol gel method manufacture method of nanometer titanium dioxide |
| CN106757040A (en) * | 2016-12-01 | 2017-05-31 | 三达奥克化学股份有限公司 | Powder metallurgical stainless steel precision workpiece light decorations process agent and production method |
| CN108250972B (en) * | 2016-12-28 | 2021-09-21 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution for barrier layer planarization |
| CN110358453A (en) * | 2018-04-10 | 2019-10-22 | 蓝思科技（长沙）有限公司 | A kind of glass polishing nano-cerium oxide polishing fluid and preparation method thereof |
| US20200303198A1 (en) * | 2019-03-22 | 2020-09-24 | Fujimi Incorporated | Polishing composition and polishing method |
| CN115466530B (en) * | 2022-09-30 | 2023-10-27 | 武汉工程大学 | Modified silicon dioxide crystal face agent and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112151A (en) * | 1994-05-17 | 1995-11-22 | 舒海清 | Leather protecting agent |
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1998
- 1998-04-16 CN CN98110778A patent/CN1063205C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112151A (en) * | 1994-05-17 | 1995-11-22 | 舒海清 | Leather protecting agent |
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