CN101671527A - Copper chemical mechanical polishing solution with high removing rate and low damage, and preparation method thereof - Google Patents
Copper chemical mechanical polishing solution with high removing rate and low damage, and preparation method thereof Download PDFInfo
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- CN101671527A CN101671527A CN200910187630A CN200910187630A CN101671527A CN 101671527 A CN101671527 A CN 101671527A CN 200910187630 A CN200910187630 A CN 200910187630A CN 200910187630 A CN200910187630 A CN 200910187630A CN 101671527 A CN101671527 A CN 101671527A
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Abstract
The invention discloses a copper chemical mechanical polishing solution with high removing rate and low damage, which comprises the raw materials by mass percent: 0.1-20% of grinding material, 0.1-2%of complexing agent, 0.01-2% of film forming agent, 0.1-3% of dispersing agent, 0.01-10% of oxidizing agent and less than or equal to 90% of purified water. The polishing solution has the characteristics of high removing rate (with the polishing speed of 600-800nm) and low surface damage (such as local and whole corrosion, butterfly-shaped defect and scratch), thus improving the excellence rate ofthe product, being beneficial to realizing whole planarization of copper, and ensuring the cleaning to be simple and convenient after polishing.
Description
Technical field:
The present invention relates to a kind of copper chemical mechanical polishing solution, especially the copper chemical mechanical polishing solution and the preparation method of convenience, high clearance, low damage cleaned in the polishing back.
Background technology:
Along with the development of super large-scale integration (ULSI), the improving constantly of chip integration, circuit element is also more and more intensive, and chip interconnect becomes the key factor that influences chip manufacturing gradually.In service the playing an important role of the operation of chip interconnect in chip is as transmitting logical signal, carry power supply and distributing clocksignal to carry out sequential control and synchronous operation etc.The high integration of chip causes interconnection line to increase and sectional area reduces, if still continue to use the traditional aluminum interconnecting method of ULSI, will cause the resistance increase and produce stray capacitance because of distance between centers of tracks reduces, thereby increased substantially the time constant RC of interconnection line, the travelling speed of unicircuit then postpones to change into the time lag that is caused by interconnection line by logical gate.At present, the time lag that causes because of interconnection line for fear of high density integrated circuit having, copper is substitution of Al and become the preferred material that the deep submicron integrated circuit interconnect technology further develops, it can make the transmission speed of local interconnect improve 10%, make the transmission speed of overall interconnect improve 50%, when not only having guaranteed the circuit high integration but also can improve travelling speed.
(chemical mechanical polishing CMP) is considered to the most effective and the most practical working method of present copper interconnecting line in chemically machinery polished.Existing copper CMP all is made up of raw materials such as abrasive material, oxygenant, passivator, etching reagent and promoting agents basically with polishing fluid, though have the high advantage of material removal rate, but exist the shortcoming of glazed surface generation, how to realize that the copper CMP of high clearance and low damage is a big difficult point of industry than macrolesion.
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 polish the back clean convenient, material removal rate is high and the copper chemical mechanical polishing solution of low damage.
Technical solution of the present invention is: the copper chemical mechanical polishing solution and the preparation method of a kind of high clearance and low damage, after it is characterized in that mixing by abrasive material, complexing agent, membrane-forming agent, dispersion agent, oxygenant and pure water again with KOH or HNO
3Regulate pH value to 1.0～7.0, the mass percent of each raw material is:
Abrasive material 0.1%～20%
Complexing agent 0.1%～2%
Membrane-forming agent 0.01%～2%
Dispersion agent 0.1%～3%
Oxygenant 0.01%～10%
Pure water is less than or equal to 90%.
Described abrasive material is SiO
2, Al
2O
3Or surface coverage aluminium SiO
2At least a in the hydrosol particle.
The particle diameter of described abrasive material is 20～150nm.
Described complexing agent 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.
The described membrane-forming agent mixture that to be anion surfactant form with benzotriazole or benzotriazole derivative, the weight ratio of anion surfactant and benzotriazole or benzotriazole derivative is 0.1～10.
Described anion surfactant is at least a in alkylsurfuric acid ammonium salt, alkylsulphonic acid ammonium salt or the benzene sulfonamide acid ammonium salt.
Described dispersion agent is at least a in aliphatic alcohol polyethenoxy polyethenoxy ether block polyether nonionogenic tenside, polyvinyl alcohol and polystyrene block copolymer, polyacrylic acid and salt thereof, polyoxyethylene glycol, polymine or the quaternary ammonium salt cationic surfactant.
Described oxygenant is at least a in hydrogen peroxide, urea peroxide, Peracetic Acid or the ammonium persulphate.
The preparation method of the copper chemical mechanical polishing solution of a kind of high clearance and low damage is characterized in that: abrasive material is added in the agitator, under agitation add pure water and other component by mass percentage and stir, with KOH or HNO
3Regulating the pH value is 1.0～7.0, and the pH value is more excellent to be 2.0～5.0, continues to be stirred to evenly, and static 30min gets final product.
The present invention adopts the mixture of anion surfactant and benzotriazole or derivatives thereof as membrane-forming agent, with other component reasonable compatibilities, (polishing speed can reach 600～800nm) both can to have guaranteed height in the copper CMP process to remove speed, reduced surface damage (local and general corrosion, butterfly defective and scratch) again, improved the product fine rate, help realizing copper overall planarization (surfaceness can reach 20～40nm) and polishing back clean simple, convenient.
Embodiment:
Embodiment 1:
The copper chemical mechanical polishing solution of a kind of high clearance and low damage, be made up of abrasive material, complexing agent, membrane-forming agent, dispersion agent, oxygenant and pure water, the mass percent of each raw material is: abrasive material 0.1%～20%, complexing agent 0.1%～2%, membrane-forming agent 0.01%～2%, dispersion agent 0.1%～3%, oxygenant 0.01%～10% and pure water are less than or equal to 90%.
Each raw material is selected in its mass range, and gross weight is 100%.
The preparation method adds abrasive material in the agitator, under agitation adds pure water and other component by mass percentage and stirs, with KOH or HNO
3Regulating the pH value is 1.0～7.0, and the pH value is more excellent to be 2.0～5.0, continues to be stirred to evenly, and static 30min gets final product.
Described abrasive material is SiO
2, Al
2O
3Or surface coverage aluminium SiO
2At least a in the hydrosol particle, the particle diameter of abrasive material is 20～150nm, optimum grain-diameter is 30～130nm.
Described complexing agent is ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, nitrilotriacetic acid(NTA) and at least a in ammonium salt or the sodium salt separately thereof.
The described membrane-forming agent mixture that to be anion surfactant form with benzotriazole (BTA) or benzotriazole derivative, the weight ratio of anion surfactant and benzotriazole or benzotriazole derivative is 0.1～10.
Described anion surfactant is at least a in alkylsurfuric acid ammonium salt, alkylsulphonic acid ammonium salt or the benzene sulfonamide acid ammonium salt.
Described dispersion agent is at least a in aliphatic alcohol polyethenoxy polyethenoxy ether block polyether nonionogenic tenside, polyvinyl alcohol and polystyrene block copolymer, polyacrylic acid and salt thereof (PAA), polyoxyethylene glycol (PEG), polymine (PEA) or the quaternary ammonium salt cationic surfactant.
Described oxygenant is hydrogen peroxide (H
2O
2), at least a in urea peroxide, Peracetic Acid or the ammonium persulphate.
Described pure water is that its resistance is 18M Ω at least through the filtering water of ion exchange resin.
Polishing experiments: adopt the CP-4 polishing machine of U.S. CE TR company, polishing pad is an IC1000/Suba IV polishing pad, polish pressure 3Psi, and lower wall rotating speed 100rpm, polishing fluid flow 200ml/min, surface of polished is tested its surfaceness (RMS) by AFM.
Polishing back material removal rate is R=600～800nm, surfaceness R
a=20～40nm.
Embodiment 2:
Raw material and weight percent are as follows:
Abrasive material is the SiO of particle diameter 60nm
2Hydrosol particle 2%;
Complexing agent is an ethylenediamine tetraacetic acid (EDTA) 0.99%;
Membrane-forming agent is the mixture 0.01% of ammonium lauryl sulfate salt and benzotriazole (BTA), and the weight ratio of ammonium lauryl sulfate salt and benzotriazole (BTA) is 1: 1 (weight ratio is 1);
Dispersion agent is aliphatic alcohol polyethenoxy polyethenoxy ether block polyether nonionogenic tenside 2% (model F38, BASF Co.Ltd. produce)
Oxygenant is hydrogen peroxide (H
2O
2) 5%;
Pure water surplus (90%).
Method according to embodiment 1 prepares polishing fluid and carries out polishing experiments, and polishing back material removal rate is R=780nm, surfaceness R
a=32nm.
Embodiment 3:
Raw material and weight percent are as follows:
Abrasive material is the Al of particle diameter 30nm
2O
3Hydrosol particle 5%;
Complexing agent is a diethylene triaminepentaacetic acid(DTPA) 0.5%;
Membrane-forming agent is the mixture 0.01% of Witco 1298 Soft Acid ammonium and benzotriazole derivative, and the weight ratio of Witco 1298 Soft Acid ammonium and benzotriazole derivative is 1: 10 (weight ratio is 0.1);
Dispersion agent is a polyoxyethylene glycol (PEG) 2%;
Oxygenant is an ammonium persulphate 5%;
Pure water surplus (87.49%).
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=22nm.
Embodiment 4:
Abrasive material is the SiO of particle diameter 30nm
2Hydrosol particle 10%;
Complexing agent is a triethylenetetraaminehexaacetic acid ammonium 1%;
Membrane-forming agent is the mixture 0.05% of Witco 1298 Soft Acid ammonium and benzotriazole (BTA); The weight ratio of Witco 1298 Soft Acid ammonium and benzotriazole (BTA) is 10: 1 (weight ratio is 10);
Dispersion agent is a polymine (PEA) 1%;
Oxygenant is an ammonium persulphate 5%;
Pure water surplus (82.95%).
Method according to embodiment 1 prepares polishing fluid and carries out polishing experiments, and polishing back material removal rate is R=720nm, surfaceness R
a=23nm.
Embodiment 5:
Abrasive material is the surface coverage aluminium SiO of particle diameter 130nm
2Hydrosol particle 2%;
Complexing agent is a diethylene triaminepentaacetic acid(DTPA) 1%;
Membrane-forming agent is the mixture 0.03% of Witco 1298 Soft Acid ammonium and benzotriazole (BTA); The weight ratio of Witco 1298 Soft Acid ammonium and benzotriazole (BTA) is 10: 5 (weight ratio is 2);
Dispersion agent is polyacrylic acid and salt (PAA) 2% thereof;
Oxygenant is hydrogen peroxide (H
2O
2) 5%
Pure water surplus (89.97%).
Method according to embodiment 1 prepares polishing fluid and carries out polishing experiments, and polishing back material removal rate is R=780nm, surfaceness R
a=36nm.
Claims (9)
1. the copper CMP polishing fluid of a high clearance, low damage, it is characterized in that by after abrasive material, complexing agent, membrane-forming agent, dispersion agent, oxygenant and the pure water mixing again with KOH or HNO
3Regulate pH value to 1.0～7.0, the mass percent of each raw material is:
Abrasive material 0.1%～20%
Complexing agent 0.1%～2%
Membrane-forming agent 0.01%～2%
Dispersion agent 0.1%～3%
Oxygenant 0.01%～10%
Pure water is less than or equal to 90%.
2. the copper chemical mechanical polishing solution of high clearance according to claim 1, low damage, it is characterized in that: described abrasive material is SiO
2, Al
2O
3Or surface coverage aluminium SiO
2Hydrosol particle at least a.
3. the copper chemical mechanical polishing solution of high clearance according to claim 1 and 2, low damage, it is characterized in that: the particle diameter of described abrasive material is 20～150nm.
4. the copper chemical mechanical polishing solution of high clearance according to claim 3, low damage is characterized in that: described complexing agent 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.
5. the copper chemical mechanical polishing solution of high clearance according to claim 4, low damage, it is characterized in that: the described membrane-forming agent mixture that to be anion surfactant form with benzotriazole or benzotriazole derivative, the weight ratio of anion surfactant and benzotriazole or benzotriazole derivative is 0.1～10.
6. the copper chemical mechanical polishing solution of high clearance according to claim 5, low damage is characterized in that: described anion surfactant is at least a in alkylsurfuric acid ammonium salt, alkylsulphonic acid ammonium salt or the benzene sulfonamide acid ammonium salt.
7. the copper chemical mechanical polishing solution of high clearance according to claim 6, low damage is characterized in that: described dispersion agent is at least a in aliphatic alcohol polyethenoxy polyethenoxy ether block polyether nonionogenic tenside, polyvinyl alcohol and polystyrene block copolymer, polyacrylic acid and salt thereof, polyoxyethylene glycol, polymine or the quaternary ammonium salt cationic surfactant.
8. the copper chemical mechanical polishing solution of high clearance according to claim 7, low damage is characterized in that: described oxygenant is at least a in hydrogen peroxide, urea peroxide, Peracetic Acid or the ammonium persulphate.
9. the preparation method of the copper chemical mechanical polishing solution of one kind high according to claim 1 clearance, low damage is characterized in that: abrasive material is added in the agitator, under agitation add pure water and other component by mass percentage and stir, with KOH or HNO
3Regulating the pH value is 1.0～7.0, continues to be stirred to evenly, and static 30min gets final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910187630A CN101671527A (en) | 2009-09-27 | 2009-09-27 | Copper chemical mechanical polishing solution with high removing rate and low damage, and preparation method thereof |
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|---|---|---|---|
| CN200910187630A CN101671527A (en) | 2009-09-27 | 2009-09-27 | Copper chemical mechanical polishing solution with high removing rate and low damage, and preparation method thereof |
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|---|---|
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Family
ID=42018953
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|---|---|---|---|
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974758A (en) * | 2010-11-04 | 2011-02-16 | 西北工业大学 | Water-soluble copper protective agent, preparation method and using method thereof |
| CN101974297A (en) * | 2010-11-12 | 2011-02-16 | 大连三达奥克化学股份有限公司 | Core/shell type composite nano-abrasive copper chemical-mechanical polishing liquid |
| CN102181232A (en) * | 2011-03-17 | 2011-09-14 | 清华大学 | Composition for low downforce chemically mechanical polishing of coppers in ULSI (Ultra Large Scale Integrated Circuit) multi-layered copper wiring |
| CN102585706A (en) * | 2012-01-09 | 2012-07-18 | 清华大学 | Acidic chemical and mechanical polishing composition |
| CN102888193A (en) * | 2012-06-25 | 2013-01-23 | 上海应用技术学院 | Chemical mechanical polishing solution for processing surface of sapphire or carborundum wafer for LED (Light Emitting Diode) substrate slice and preparation method thereof |
| CN103834306A (en) * | 2012-11-22 | 2014-06-04 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid for through-silicon-via planarization |
| CN103937414A (en) * | 2014-04-29 | 2014-07-23 | 杰明纳微电子股份有限公司 | Fine polishing liquid for hard disk substrate of computer |
| CN104479560A (en) * | 2014-12-30 | 2015-04-01 | 深圳市力合材料有限公司 | Integrated circuit copper polishing solution used at low down pressure |
| CN104592896A (en) * | 2014-12-31 | 2015-05-06 | 上海新安纳电子科技有限公司 | Chemical mechanical polishing solution |
| CN108085687A (en) * | 2017-12-01 | 2018-05-29 | 东方电气集团东方汽轮机有限公司 | Cupric piece surface processing polishing agent |
| CN108250978A (en) * | 2016-12-28 | 2018-07-06 | 安集微电子科技（上海）股份有限公司 | A kind of chemical mechanical polishing liquid and its application |
| WO2019006600A1 (en) * | 2017-07-03 | 2019-01-10 | 深圳市宏昌发科技有限公司 | Polishing agent, copper part and polishing process therefor |
| CN109233644A (en) * | 2018-09-19 | 2019-01-18 | 广州亦盛环保科技有限公司 | A kind of precise polishing solution and preparation method thereof |
| WO2019129103A1 (en) * | 2017-12-27 | 2019-07-04 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| WO2019129105A1 (en) * | 2017-12-27 | 2019-07-04 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing liquid |
| CN115160934A (en) * | 2022-07-29 | 2022-10-11 | 江苏山水半导体科技有限公司 | Super-hydrophilic large-size silicon fine polishing solution and preparation and application methods thereof |
| CN115537123A (en) * | 2022-11-09 | 2022-12-30 | 博力思(天津)电子科技有限公司 | Chemical mechanical polishing solution for polyether-ether-ketone material |
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| CN101016440A (en) * | 2006-02-08 | 2007-08-15 | 罗门哈斯电子材料Cmp控股股份有限公司 | Multi-component barrier polishing solution |
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2009
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016440A (en) * | 2006-02-08 | 2007-08-15 | 罗门哈斯电子材料Cmp控股股份有限公司 | Multi-component barrier polishing solution |
Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974758A (en) * | 2010-11-04 | 2011-02-16 | 西北工业大学 | Water-soluble copper protective agent, preparation method and using method thereof |
| CN101974297A (en) * | 2010-11-12 | 2011-02-16 | 大连三达奥克化学股份有限公司 | Core/shell type composite nano-abrasive copper chemical-mechanical polishing liquid |
| CN102181232B (en) * | 2011-03-17 | 2013-12-11 | 清华大学 | Composition for low downforce chemically mechanical polishing of coppers in ULSI (Ultra Large Scale Integrated Circuit) multi-layered copper wiring |
| CN102181232A (en) * | 2011-03-17 | 2011-09-14 | 清华大学 | Composition for low downforce chemically mechanical polishing of coppers in ULSI (Ultra Large Scale Integrated Circuit) multi-layered copper wiring |
| CN102585706A (en) * | 2012-01-09 | 2012-07-18 | 清华大学 | Acidic chemical and mechanical polishing composition |
| CN102585706B (en) * | 2012-01-09 | 2013-11-20 | 清华大学 | Acidic chemical and mechanical polishing composition |
| CN102888193A (en) * | 2012-06-25 | 2013-01-23 | 上海应用技术学院 | Chemical mechanical polishing solution for processing surface of sapphire or carborundum wafer for LED (Light Emitting Diode) substrate slice and preparation method thereof |
| CN103834306A (en) * | 2012-11-22 | 2014-06-04 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid for through-silicon-via planarization |
| CN103834306B (en) * | 2012-11-22 | 2017-08-11 | 安集微电子（上海）有限公司 | A kind of chemical mechanical polishing liquid planarized for silicon hole |
| CN103937414A (en) * | 2014-04-29 | 2014-07-23 | 杰明纳微电子股份有限公司 | Fine polishing liquid for hard disk substrate of computer |
| CN103937414B (en) * | 2014-04-29 | 2018-03-02 | 杰明纳微电子股份有限公司 | A kind of precise polishing solution of hard disc of computer disk substrate |
| CN104479560A (en) * | 2014-12-30 | 2015-04-01 | 深圳市力合材料有限公司 | Integrated circuit copper polishing solution used at low down pressure |
| CN104592896A (en) * | 2014-12-31 | 2015-05-06 | 上海新安纳电子科技有限公司 | Chemical mechanical polishing solution |
| CN108250978A (en) * | 2016-12-28 | 2018-07-06 | 安集微电子科技（上海）股份有限公司 | A kind of chemical mechanical polishing liquid and its application |
| WO2019006600A1 (en) * | 2017-07-03 | 2019-01-10 | 深圳市宏昌发科技有限公司 | Polishing agent, copper part and polishing process therefor |
| CN110809615A (en) * | 2017-07-03 | 2020-02-18 | 深圳市宏昌发科技有限公司 | Polishing agent, copper part and polishing treatment method thereof |
| CN108085687A (en) * | 2017-12-01 | 2018-05-29 | 东方电气集团东方汽轮机有限公司 | Cupric piece surface processing polishing agent |
| WO2019129103A1 (en) * | 2017-12-27 | 2019-07-04 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| WO2019129105A1 (en) * | 2017-12-27 | 2019-07-04 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing liquid |
| CN109971357A (en) * | 2017-12-27 | 2019-07-05 | 安集微电子（上海）有限公司 | A kind of chemical mechanical polishing liquid |
| CN109971357B (en) * | 2017-12-27 | 2021-12-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| US11746257B2 (en) | 2017-12-27 | 2023-09-05 | Anji Microelectronics (Shanghai) Co., Ltd. | Chemical mechanical polishing solution |
| CN109233644A (en) * | 2018-09-19 | 2019-01-18 | 广州亦盛环保科技有限公司 | A kind of precise polishing solution and preparation method thereof |
| CN109233644B (en) * | 2018-09-19 | 2021-03-12 | 广州亦盛环保科技有限公司 | Fine polishing solution and preparation method thereof |
| CN115160934A (en) * | 2022-07-29 | 2022-10-11 | 江苏山水半导体科技有限公司 | Super-hydrophilic large-size silicon fine polishing solution and preparation and application methods thereof |
| CN115160934B (en) * | 2022-07-29 | 2023-08-25 | 江苏山水半导体科技有限公司 | Super-hydrophilic large-size silicon fine polishing liquid and preparation and use methods thereof |
| CN115537123A (en) * | 2022-11-09 | 2022-12-30 | 博力思(天津)电子科技有限公司 | Chemical mechanical polishing solution for polyether-ether-ketone material |
| CN115537123B (en) * | 2022-11-09 | 2023-08-15 | 博力思(天津)电子科技有限公司 | Chemical mechanical polishing solution for polyether-ether-ketone material |
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Application publication date: 20100317 |