WO2018136511A1 - Compositions and methods for removing ceria particles from a surface - Google Patents
Compositions and methods for removing ceria particles from a surface Download PDFInfo
- Publication number
- WO2018136511A1 WO2018136511A1 PCT/US2018/014049 US2018014049W WO2018136511A1 WO 2018136511 A1 WO2018136511 A1 WO 2018136511A1 US 2018014049 W US2018014049 W US 2018014049W WO 2018136511 A1 WO2018136511 A1 WO 2018136511A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- removal composition
- aqueous removal
- acid
- contaminants
- microelectronic device
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 149
- 239000002245 particle Substances 0.000 title claims abstract description 69
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 44
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004377 microelectronic Methods 0.000 claims abstract description 52
- 239000000356 contaminant Substances 0.000 claims abstract description 42
- 238000004140 cleaning Methods 0.000 claims abstract description 24
- 238000005498 polishing Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 12
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 8
- -1 poly(methacrylic acid) Polymers 0.000 claims description 49
- 239000003002 pH adjusting agent Substances 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 239000006259 organic additive Substances 0.000 claims description 31
- 239000003638 chemical reducing agent Substances 0.000 claims description 30
- 239000008139 complexing agent Substances 0.000 claims description 27
- 229940123973 Oxygen scavenger Drugs 0.000 claims description 21
- 229920000642 polymer Polymers 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 9
- IBLKWZIFZMJLFL-UHFFFAOYSA-N 1-phenoxypropan-2-ol Chemical compound CC(O)COC1=CC=CC=C1 IBLKWZIFZMJLFL-UHFFFAOYSA-N 0.000 claims description 8
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 7
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- HMBHAQMOBKLWRX-UHFFFAOYSA-N 2,3-dihydro-1,4-benzodioxine-3-carboxylic acid Chemical compound C1=CC=C2OC(C(=O)O)COC2=C1 HMBHAQMOBKLWRX-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
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- 235000019252 potassium sulphite Nutrition 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 3
- 150000008044 alkali metal hydroxides Chemical group 0.000 claims description 3
- XEVRDFDBXJMZFG-UHFFFAOYSA-N carbonyl dihydrazine Chemical group NNC(=O)NN XEVRDFDBXJMZFG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- DCZFGQYXRKMVFG-UHFFFAOYSA-N cyclohexane-1,4-dione Chemical class O=C1CCC(=O)CC1 DCZFGQYXRKMVFG-UHFFFAOYSA-N 0.000 claims description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 3
- 150000002429 hydrazines Chemical class 0.000 claims description 3
- WHIVNJATOVLWBW-UHFFFAOYSA-N n-butan-2-ylidenehydroxylamine Chemical compound CCC(C)=NO WHIVNJATOVLWBW-UHFFFAOYSA-N 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
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- 238000007865 diluting Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 15
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
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- 235000012431 wafers Nutrition 0.000 description 11
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- 238000001446 dark-field microscopy Methods 0.000 description 8
- 239000003989 dielectric material Substances 0.000 description 8
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 8
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- 230000000052 comparative effect Effects 0.000 description 6
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- 125000002768 hydroxyalkyl group Chemical group 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
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- 150000001412 amines Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- 238000002955 isolation Methods 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 4
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- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 4
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- MPNBXFXEMHPGTK-UHFFFAOYSA-N pyrimidine-4,5,6-triamine Chemical compound NC1=NC=NC(N)=C1N MPNBXFXEMHPGTK-UHFFFAOYSA-N 0.000 description 1
- 150000003230 pyrimidines Chemical class 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- 229940054269 sodium pyruvate Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- PWEBUXCTKOWPCW-UHFFFAOYSA-N squaric acid Chemical compound OC1=C(O)C(=O)C1=O PWEBUXCTKOWPCW-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 description 1
- 229910001866 strontium hydroxide Inorganic materials 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- ZOMVKCHODRHQEV-UHFFFAOYSA-M tetraethylphosphanium;hydroxide Chemical compound [OH-].CC[P+](CC)(CC)CC ZOMVKCHODRHQEV-UHFFFAOYSA-M 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- CRUVUWATNULHFA-UHFFFAOYSA-M tetramethylphosphanium;hydroxide Chemical compound [OH-].C[P+](C)(C)C CRUVUWATNULHFA-UHFFFAOYSA-M 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- OORMKVJAUGZYKP-UHFFFAOYSA-M tetrapropylphosphanium;hydroxide Chemical compound [OH-].CCC[P+](CCC)(CCC)CCC OORMKVJAUGZYKP-UHFFFAOYSA-M 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- IJGSGCGKAAXRSC-UHFFFAOYSA-M tris(2-hydroxyethyl)-methylazanium;hydroxide Chemical compound [OH-].OCC[N+](C)(CCO)CCO IJGSGCGKAAXRSC-UHFFFAOYSA-M 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0084—Antioxidants; Free-radical scavengers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
- H01L21/02065—Cleaning during device manufacture during, before or after processing of insulating layers the processing being a planarization of insulating layers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/14—Other polishing compositions based on non-waxy substances
- C09G1/16—Other polishing compositions based on non-waxy substances on natural or synthetic resins
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0047—Other compounding ingredients characterised by their effect pH regulated compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/54—Aqueous solutions or dispersions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/40—Specific cleaning or washing processes
Definitions
- the present invention relates generally to compositions for removing ceria particles and other chemical mechanical polishing slurry contaminants from microelectronic devices having same thereon.
- Microelectronic device wafers are used to form integrated circuits.
- the microelectronic device wafer includes a substrate, such as silicon, into which regions are patterned for deposition of different materials having insulative, conductive or semi -conductive properties.
- CMP Chemical Mechanical Polishing or Planarization
- a chemical process such as oxidation or chelation.
- CMP involves applying an abrasive slurry having an active chemistry to a polishing pad that buffs the surface of a microelectronic device wafer during the removal, planarization, and polishing processes. Removal or polishing processes using purely physical or purely chemical action are not as effective as the synergistic combination of both in order to achieve fast, uniform removal.
- the CMP slurry should also be able to preferentially remove films that comprise complex layers of metals and other materials so that highly planar surfaces can be produced for subsequent photolithography, or patterning, etching and thin-film processing.
- a pad oxide film and a pad nitride film are deposited on a semiconductor substrate and patterned to expose portions of the substrate, which correspond to an isolation region. Then, the exposed regions of the substrate are etched to form a trench. Thereafter, the substrate is subjected to a sacrificial oxidation process to remove damage caused by the substrate etching followed by formation of a wall oxide film on the surface of the trench.
- a sacrificial oxidation process to remove damage caused by the substrate etching followed by formation of a wall oxide film on the surface of the trench.
- a trench-buried oxide film e.g., an oxide film formed by high density plasma chemical vapor deposition referred to as an HDP-oxide film
- an HDP-oxide film is deposited on the surface of the substrate in such a manner as to be buried in the trench.
- the surface of the HDP-oxide film is subjected to chemical mechanical polishing until the pad nitride film is exposed.
- the resulting substrate is then cleaned and the pad nitride film which was used as an etch barrier during the trench etch is removed, completing the formation of an isolation region.
- a CMP slurry using ceria particles achieves a faster polishing speed for an insulator, relative to a silica-containing slurry. Moreover, a ceria-based slurry is most often used because of the ability to achieve STI pattern planarization with minimal oxide erosion. Disadvantageous ⁇ , ceria- based slurries are difficult to remove from STI structures because of the oppositely charged zeta potentials of the ceria particles relative to the silicon oxide and silicon nitride surfaces. If a device is manufactured with these residues remaining on the wafer, the residues will lead to short circuits and an increase in electric resistance. Ceria particles are also a problem with FinFET structures following CMP processing using ceria slurries.
- DHF dilute hydrofluoric acid
- the ceria particle removal composition should also efficaciously remove CMP slurry contaminants from the surface of the microelectronic device.
- the present invention generally relates to a removal composition and process, particularly useful for cleaning ceria particles and CMP contaminants from microelectronic devices having said particles and CMP contaminants thereon.
- an aqueous removal composition comprising at least one pH adjusting agent, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, and optionally at least one oxygen scavenger.
- a method of removing ceria particles and CMP contaminants from a microelectronic device having said particles and contaminants thereon comprising contacting the microelectronic device with a removal composition for sufficient time to at least partially clean said particles and contaminants from the microelectronic device, wherein said removal composition comprises at least one pH adjusting agent, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, and optionally at least one oxygen scavenger.
- an article of manufacture comprising an aqueous removal composition, a microelectronic device wafer, and material selected from the group consisting of ceria particles, CMP contaminants and combinations thereof, wherein the cleaning composition comprises at least one pH adjusting agent, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, and optionally at least one oxygen scavenger.
- the present invention relates generally to compositions useful for the removal of ceria particles and CMP contaminants from a microelectronic device having such material(s) thereon.
- the ceria particles and CMP contaminants are efficaciously removed using the compositions and further the compositions are compatible with silicon nitride and low-k dielectric (e.g., silicon oxide) layers.
- microelectronic device corresponds to semiconductor substrates, flat panel displays, phase change memory devices, solar panels and other products including solar substrates, photovoltaics, and microelectromechanical systems (MEMS), manufactured for use in microelectronic, integrated circuit, or computer chip applications.
- Solar substrates include, but are not limited to, silicon, amorphous silicon, polycrystalline silicon, monocrystalline silicon, CdTe, copper indium selenide, copper indium sulfide, and gallium arsenide on gallium.
- the solar substrates may be doped or undoped. It is to be understood that the term "microelectronic device” is not meant to be limiting in any way and includes any substrate that will eventually become a microelectronic device or microelectronic assembly.
- ceria particles corresponds to cerium-based abrasive particles that may be used in chemical mechanical polishing slurries, including, for example, a cerium oxide having the formula Ce203 and Ce02. It should be appreciated that the “ceria particles” may comprise, consist of, or consist essentially of cerium oxide.
- contaminants correspond to chemicals present in the CMP slurry, reaction by-products of the polishing slurry, post-CMP residue, chemicals present in the wet etching composition, reaction by products of the wet etching composition, and any other materials that are the by-products of the CMP process, the wet etching, the plasma etching or the plasma ashing process.
- post-CMP residue corresponds to particles from the polishing slurry, e.g., chemicals present in the slurry, reaction by-products of the polishing slurry, carbon-rich particles, polishing pad particles, brush deloading particles, equipment materials of construction particles, metal, organic residues, and any other materials that are the by-products of the CMP process.
- the post-CMP residue can further comprise tungsten-containing particles.
- low-k dielectric material corresponds to any material used as a dielectric material in a layered microelectronic device, wherein the material has a dielectric constant less than about 3.5.
- the low-k dielectric materials include low-polarity materials such as silicon- containing organic polymers, silicon-containing hybrid organic/inorganic materials, organosilicate glass (OSG), TEOS, fluorinated silicate glass (FSG), silicon dioxide, and carbon-doped oxide (CDO) glass. It is to be appreciated that the low-k dielectric materials may have varying densities and varying porosities.
- complexing agent includes those compounds that are understood by one skilled in the art to be complexing agents, chelating agents and/or sequestering agents. Complexing agents will chemically combine with or physically hold the metal atom and/or metal ion to be removed using the compositions described herein.
- substantially devoid is defined herein as less than 2 wt. %, preferably less than 1 wt. %, more preferably less than 0.5 wt. %, and most preferably less than 0.1 wt. %. "Devoid” is intended to correspond to less than 0.001 wt% to account for environmental contamination.
- Oxidizing agents correspond to compounds that oxidize exposed metal(s) resulting in corrosion of the metal or oxide formation on the metal. Oxidizing agents include, but are not limited to: hydrogen peroxide; other percompounds such as salts and acids containing peroxomonosulfate, perborate, perchlorate, periodate, persulfate, permanganate, and peracetate anions; and amine-N-oxides.
- fluoride containing compounds correspond to salts or acid compounds comprising a fluoride ion (F ) that is ionically bonded to another atom.
- barrier material corresponds to any material used in the art to seal the metal lines (e.g., copper interconnects) to minimize the diffusion of said metal (e.g., copper) into the dielectric material.
- Preferred barrier layer materials include tantalum, titanium, ruthenium, hafnium, tungsten, and other refractory metals and their nitrides and silicides.
- degradation products of adenosine and adenosine derivatives includes, but is not limited to, adenine (C5H5N5), methylated adenine (e.g., N-methyl-7H- purin-6-amine, C6H7N5), dimethylated adenine (e.g., N,N-dimethyl-7H-purin-6-amine, C7H9N5), N4,N4-dimethylpyrimidine-4,5,6-triamine (CeHnNs), 4,5,6-triaminopyrimidine, allantoin (C 4 H 6 N 4 03), hydroxylated C-O-O-C dimers C-C bridged dimers ((C 5 H 4 N 5 )2 or (C5H4N50)2), ribose (C5H10O5), methylated ribose (e.g., 5-(methoxymethyl)tetrahydrofur
- surfactants correspond to amphiphilic species having hydrophobic groups and hydrophilic groups, as readily understood by those skilled in the art, but do not include polymers.
- polymers correspond to species that have repeating monomelic groups, and can be natural or synthetic. It should be appreciated that a “polymer” can be a homopolymer, having only one type of repeating monomer, or a co-polymer, having more than one type of repeating monomer.
- suitable for removing ceria particles and CMP contaminants from a microelectronic device having said particles and contaminants thereon corresponds to at least partial removal of said particles/contaminants from the microelectronic device.
- Cleaning efficacy is rated by the reduction of objects on the microelectronic device. For example, pre- and post-cleaning analysis may be carried out using an atomic force microscope. The particles on the sample may be registered as a range of pixels. A histogram (e.g., a Sigma Scan Pro) may be applied to filter the pixels in a certain intensity (e.g., 231-235) and the number of particles counted. The particle reduction may be calculated using:
- the method of determination of cleaning efficacy is provided for example only and is not intended to be limited to same.
- the cleaning efficacy may be considered as a percentage of the total surface that is covered by particulate matter.
- AFM's may be programmed to perform a z-plane scan to identify topographic areas of interest above a certain height threshold and then calculate the area of the total surface covered by said areas of interest.
- AFM's may be programmed to perform a z-plane scan to identify topographic areas of interest above a certain height threshold and then calculate the area of the total surface covered by said areas of interest.
- At least 75% of the particles/contaminants are removed from the microelectronic device using the compositions described herein, more preferably at least 90%, even more preferably at least 95%, and most preferably at least 99% of the particles/contaminants are removed.
- compositions described herein may be embodied in a wide variety of specific formulations, as hereinafter more fully described.
- compositions wherein specific components of the composition are discussed in reference to weight percentage ranges including a zero lower limit, it will be understood that such components may be present or absent in various specific embodiments of the composition, and that in instances where such components are present, they may be present at concentrations as low as 0.00001 weight percent, based on the total weight of the composition in which such components are employed.
- a removal composition is described, which, in some embodiments, is preferably an aqueous removal composition, comprising, consisting of, or consisting essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, optionally at least one complexing agent, optionally at least one polymer, and optionally at least one oxygen scavenger.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, and at least one organic additive.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, and at least one complexing agent.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, and at least one polymer.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, and at least one oxygen scavenger.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, at least one complexing agent, and at least one oxygen scavenger.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, at least one complexing agent, and at least one polymer.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, at least one polymer, and at least one oxygen scavenger.
- the removal composition comprises, consists of, or consists essentially of at least one pH adjusting agent, at least one reducing agent, at least one organic additive, at least one complexing agent, at least one polymer, and at least one oxygen scavenger. It is understood by those skilled in the art that the aqueous cleaning compositions described herein further comprise water, preferably deionized water.
- the removal composition can be substantially devoid of at least one of oxidizing agents; fluoride-containing sources; surfactants; tetramethylammonium hydroxide; chemical mechanical polishing abrasive materials (e.g., silica, alumina, etc.); and corrosion inhibitors selected from the group consisting of cyanuric acid, barbituric acid and derivatives thereof, glucuronic acid, squaric acid, alpha-keto acids, adenosine and derivatives thereof, ribosylpurines and derivatives thereof, purine compounds and derivatives thereof, degradation products of adenosine and adenosine derivatives, triaminopyrimidine and other substituted pyrimidines, purine -saccharide complexes, phosphonic acid and derivatives thereof, phenanthroline, glycine, nicotinamide and derivatives thereof, flavonoids such as flavonols and anthocyanins and derivatives thereof,
- Complexing agents when present, include species having the general formula NR3 ⁇ 4 2 R 3 , wherein R 1 , R 2 and R 3 may be the same as or different from one another and are selected from the group consisting of hydrogen, straight-chain or branched Ci-Ce alkyl (e.g., methyl, ethyl, propyl, butyl, pentyl, and hexyl) groups, straight-chain or branched Ci-Ce hydroxyalkyl (e.g., hydroxymethyl, hydroxyethyl, hydroxypropyl, hydroxybutyl, hydroxypentyl, and hydroxyhexyl) groups, and Ci-Ce alkyl ethers of straight chain or branched Ci-Ce hydroxyalkyl groups as defined above.
- Ci-Ce alkyl e.g., methyl, ethyl, propyl, butyl, pentyl, and hexyl
- Ci-Ce hydroxyalkyl
- R 1 , R 2 and R 3 is a straight-chain or branched Ci-Ce hydroxyalkyl group.
- alkanolamines such as aminoethylethanolamine, N- methylaminoethanol, aminoethoxyethanol, dimethylaminoethoxyethanol, diethanolamine, N- methyldiethanolamine, monoethanolamine (MEA), triethanolamine (TEA), l-amino-2-propanol, 2-amino-l-butanol, isobutanolamine, triethylenediamine, other Ci - Cs alkanolamines and combinations thereof.
- alkanolamines such as aminoethylethanolamine, N- methylaminoethanol, aminoethoxyethanol, dimethylaminoethoxyethanol, diethanolamine, N- methyldiethanolamine, monoethanolamine (MEA), triethanolamine (TEA), l-amino-2-propanol, 2-amino-l-butanol, isobutan
- the amine When the amine includes the alkylether component, the amine may be considered an alkoxyamine, e.g., l-methoxy-2-aminoethane.
- the complexing agent may be a multi-functional amine including, but not limited to, 4-(2-hydroxyethyl)morpholine (HEM), l,2-cyclohexanediamine-N,N,N ' ,N ' -tetraacetic acid (CDTA), ethylenediaminetetraacetic acid (EDTA), m-xylenediamine (MXDA), iminodiacetic acid (IDA), 2-(hydroxyethyl)iminodiacetic acid (HIDA), nitrilotriacetic acid, thiourea, 1, 1,3,3- tetramethylurea, urea, urea derivatives, uric acid, alanine, arginine, asparagine, aspartic acid
- HEM 4-(2-hydroxyethyl
- additional complexing agents can include phosphonates (e.g., l-hydroxyethylidene-l, l-diphosphonic acid (HEDP), l,5,9-triazacyclododecane-N,N',N"- tris(methylenephosphonic acid) (DOTRP), l,4,7, 10-tetraazacyclododecane-N,N',N",N"'- tetrakis(methylenephosphonic acid) (DOTP), nitrilotris(methylene)triphosphonic acid, diethylenetriaminepentakis(methylenephosphonic acid) (DETAP), aminotri(methylenephosphonic acid), bis(hexamethylene)triamine pentamethylene phosphonic acid, 1,4,7-triazacyclononane- N,N',N"-tris(methylenephosphonic acid (NOTP), hydroxyethyldiphosphonate, nitrilotris(
- the at least one complexing agent comprises a species selected from the group consisting of monoethanolamine, triethanolamine, sulfuric acid, citric acid and combinations thereof.
- the amount of complexing agent(s) in the removal composition is in a range from about 0.01 wt% to about 10 wt%, based on the total weight of the removal composition.
- pH adjusting agents include acids and/or bases.
- Bases include, but are not limited to, alkali metal hydroxides (e.g., LiOH, KOH, RbOH, CsOH), alkaline earth metal hydroxides (e.g., Be(OH)2, Mg(OH)2, Ca(OH)2, Sr(OH)2, Ba(OH)2), ammonium hydroxide (i.e., ammonia), and a tetraalkylammonium hydroxide compound having the formula NR 1 R 2 R 3 R 4 OH, wherein R 1 , R 2 , R 3 and R 4 may be the same as or different from one another and are selected from the group consisting of hydrogen, straight-chain or branched Ci-Ce alkyl (e.g., methyl, ethyl, propyl, butyl, pentyl, and hexyl) groups, Ci-Ce hydroxyalkyl (e.g., hydroxymethyl, hydroxyethyl,
- Tetraalkylammonium hydroxides that are commercially available include tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TP AH), tetrabutylammonium hydroxide (TBAH), tributylmethylammonium hydroxide (TBMAH), benzyltrimethylammonium hydroxide (BTMAH), choline hydroxide, ethyltrimethylammonium hydroxide, tris(2-hydroxyethyl)methyl ammonium hydroxide, diethyldimethylammonium hydroxide, and combinations thereof, may be used.
- TMAH tetramethylammonium hydroxide
- TEAH tetraethylammonium hydroxide
- TP AH tetrapropylammonium hydroxide
- TBAH tetrabutylammonium hydroxide
- the pH adjusting agent may be a quaternary base having the formula (PR 1 R 2 R 3 R 4 )OH, wherein R 1 , R 2 , R 3 , and R 4 may be the same as or different from one another and are selected from the group consisting of hydrogen, straight-chain Ci-Ce alkyl (e.g., methyl, ethyl, propyl, butyl, pentyl, and hexyl) groups, branched Ci-Ce alkyl groups, Ci-Ce hydroxyalkyl (e.g., hydroxymethyl, hydroxyethyl, hydroxypropyl, hydroxybutyl, hydroxypentyl, and hydroxyhexyl) groups, substituted C6-C 1 0 aryl groups, unsubstituted C6-C 1 0 aryl groups (e.g., benzyl groups), and any combination thereof, such as tetrabutylphosphonium hydroxide (TBPH),
- TBPH
- Acids include, but are not limited to, nitric acid, sulfuric acid, phosphoric acid, hydrochloric acid, hydrobromic acid, methanesulfonic acid, benzene sulfonic acid, p-toluenesulfonic acid, trifluoromethanesulfonic acid, acetic acid, lactic acid, gly colic acid, and any combination thereof.
- the pH adjusting agent comprises KOH.
- the pH adjusting agent comprises choline hydroxide.
- the pH adjusting agent comprises ammonium hydroxide.
- the pH adjusting agent comprises at least one alkali metal hydroxide and at least one additional hydroxide enumerated herein.
- the pH adjusting agent comprises KOH and at least one additional hydroxide enumerated herein.
- the pH adjusting agent comprises KOH and at least one of choline hydroxide and ammonium hydroxide.
- the pH adjusting agent can further include at least one acid, for example, sulfuric acid, citric acid, or a combination of citric acid and sulfuric acid.
- Organic additives contemplated include, but are not limited to, 2-pyrrolidinone, l-(2- hydroxyethyl)-2-pyrrolidinone (HEP), glycerol, 1,4-butanediol, tetramethylene sulfone (sulfolane), dimethyl sulfone, ethylene glycol, propylene glycol, dipropylene glycol, tetraglyme, diglyme, methyl isobutyl ketone, methyl ethyl ketone, acetone, isopropanol, octanol, ethanol, butanol, methanol, isophorone, a glycol ether (e.g., diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, diethylene glycol monoethyl ether, triethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, di
- Polymers when present, include, but are not limited to, methacrylic acid homopolymer and copolymers with, for example, acrylamidomethylpropane sulfonic acid and maleic acid; maleic acid/vinyl ether copolymer; polyvinylpyrrolidone )/vinyl acetate; homopolymers such as phosphonated polyethyleneglycol oligomers, poly(acrylic acid) (PAA), poly(acrylamide), poly(vinyl acetate), poly(ethylene glycol) (PEG), poly (propylene glycol) (PPG), poly(styrene sulfonic acid), poly(vinyl sulfonic acid), poly(vinyl phosphonic acid), poly(vinyl phosphoric acid), poly(ethyleneimine), poly(propyleneimine), polyallylamine, polyethylene oxide (PEO), polyvinyl pyrrolidone (PVP); PPG-PEG-PPG block copolymers
- Oxygen scavengers when present, include, but are not limited to, dialkylhydroxylamines, hydroxyalkylhydroxylamines, carbohydrazide, 2-aminoethylpiperazine (AEP), methylethylketoxime, hydroquinone, hydrazines, 1,3-, 1,4- and 2,5-cyclohexanediones alone or in combination with 3- methoxypropylamine, aminophenols, linear water-soluble polyethyleneamines (e.g., triethylenetetramine, tetraethylenepentamine, pentaethylenehexamines), sodium sulfite, ammonium sulfite, potassium sulfite, and combinations thereof.
- dialkylhydroxylamines hydroxyalkylhydroxylamines
- carbohydrazide 2-aminoethylpiperazine (AEP)
- AEP 2-aminoethylpiperazine
- methylethylketoxime hydro
- the oxygen scavenger includes carbohydrazide, 2-aminoethylpiperazine (AEP), methylethylketoxime, hydroquinone, hydrazines, 1,3-, 1,4- and 2,5-cyclohexanediones alone or in combination with 3-methoxypropylamine, aminophenols, linear water-soluble polyethyleneamines such as triethylenetetramine, tetraethylenepentamine, pentaethylenehexamines, and combinations thereof.
- the oxygen scavengers assist with the stabilization of the reducing agent.
- the amount of oxygen scavenger(s) in the removal composition is in a range from about 0.0001 wt% to about 1 wt%, based on the total weight of the removal composition.
- Reducing agents include, but are not limited to, ascorbic acid, L(+)-ascorbic acid, isoascorbic acid, ascorbic acid derivatives, sulfurous acid, ammonium sulfite, potassium sulfite, sodium sulfite, dopamine HC1, phosphorous acid, phosphinic acid, potassium metabisulfite, sodium metabisulfite, ammonium metabisulfite, hydroxylamine, reducing sugars (e.g., galactose, ribose, arabinose, xylose, fucose, rhamnose, mannose, fructose, sorbose, galacturonic acid, glucosamine, maltose, lactose), potassium pyruvate, sodium pyruvate, ammonium pyruvate, formic acid, sodium formate, potassium formate, ammonium formate, dopamine, sulfur dioxide solution, and any combination thereof.
- reducing sugars
- the at least one reducing agent comprises at least one sulfite ion and at least one other enumerated reducing agent, for example, sulfurous acid, potassium sulfite, ammonium sulfite, phosphinic acid, and any combination thereof.
- sulfurous acid potassium sulfite
- ammonium sulfite ammonium sulfite
- phosphinic acid phosphinic acid
- An aqueous removal composition including the components described above, is particularly useful for removing ceria particles and contaminants (e.g., post-CMP residue and contaminants) from a microelectronic device structure.
- the pH of the aqueous removal compositions described herein can be in a range from about 1 to about 13.9. In one embodiment, the pH is in a range from about 3 to about 13.9, preferably about 3.5 to about 13.9. In another embodiment, the pH is in a range from about 3.5 to about 5.5. In still another embodiment, the pH is in a range from about 4.5 to about 8.5, preferably about 7.5 to 8.5. In another embodiment, the pH is in a range from about 9 to about 13.7.
- the aqueous removal composition comprises, consists of, or consists essentially of reducing agent(s), at least one pH adjusting agent, at least one organic additive, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of a compound comprising a sulfite ion, at least one pH adjusting agent, at least one organic additive, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of reducing agent(s), at least one pH adjusting agent, propylene glycol phenyl ether, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of a compound comprising a sulfite ion, at least one pH adjusting agent, propylene glycol phenyl ether, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of reducing agent(s), at least one complexing agent, at least one pH adjusting agent, at least one organic additive, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of a compound comprising a sulfite ion, at least one complexing agent, at least one pH adjusting agent, at least one organic additive, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of a compound comprising a sulfite ion, citric acid, at least one pH adjusting agent, at least one organic additive, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of a compound comprising a sulfite ion, citric acid, at least one pH adjusting agent, propylene glycol phenyl ether, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of reducing agent(s) (e.g., a compound comprising a sulfite ion), at least one pH adjusting agent, at least one organic additive, at least one oxygen scavenger, and water.
- the aqueous removal composition comprises, consists of, or consists essentially of reducing agent(s) (e.g., a compound comprising a sulfite ion), at least one pH adjusting agent, at least one organic additive, at least one complexing agent (e.g., citric acid), at least one oxygen scavenger, and water.
- the weight percent ratios of organic additive(s) to reducing agent(s) is in a range from about 0.001 : 1 to about 10: 1, preferably about 0.1 : 1 to about 5: 1.
- the amount of the pH adjusting agent is dependent on the final pH sought when preparing the removal composition for use, based on the pH values disclosed herein, and the knowledge of the person skilled in the art.
- a concentrated removal composition that can be diluted for use as a cleaning solution.
- a concentrated composition, or "concentrate,” advantageously permits a user (e.g. a CMP process engineer) to dilute the concentrate to the desired strength and pH at the point of use.
- Dilution of the concentrated aqueous removal composition may be in a range from about 1 : 1 to about 2500: 1, preferably about 5: 1 to about 200: 1, and most preferably about 20: 1 to about 120: 1, wherein the aqueous removal composition is diluted at or just before the tool with solvent, e.g., deionized water. It is to be appreciated by one skilled in the art that following dilution, the range of weight percent ratios of the components disclosed herein should remain unchanged.
- compositions described herein may have utility in applications including, but not limited to, post-etch residue removal, post-ash residue removal surface preparation, post-plating cleaning and post-CMP residue removal.
- aqueous cleaning compositions described herein may be useful for the cleaning and protection of other metal (e.g., copper-containing and tungsten-containing) products including, but not limited to, decorative metals, metal wire bonding, printed circuit boards and other electronic packaging using metal or metal alloys.
- the aqueous removal compositions described herein further includes ceria particles and/or CMP contaminants.
- the ceria particles and contaminants become a component of the removal composition after cleaning has begun and will be dissolved and/or suspended in the compositions.
- the aqueous removal compositions are easily formulated by simple addition of the respective ingredients and mixing to homogeneous condition. Furthermore, the compositions may be readily formulated as single -package formulations or multi-part formulations that are mixed at or before the point of use, e.g., the individual parts of the multi-part formulation may be mixed at the tool or in a storage tank upstream of the tool.
- concentrations of the respective ingredients may be widely varied in specific multiples of the composition, i.e., more dilute or more concentrated, and it will be appreciated that the compositions described herein can variously and alternatively comprise, consist or consist essentially of any combination of ingredients consistent with the disclosure herein.
- kits including, in one or more containers, one or more components adapted to form the compositions described herein.
- the kit may include, in one or more containers, at least one pH adjusting agent, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, optionally at least one polymer, and optionally at least one oxygen scavenger, for combining with additional solvent (e.g., water) at the fab or the point of use.
- additional solvent e.g., water
- the kit may include, in one or more containers, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, optionally at least one polymer, and optionally at least one oxygen scavenger, for combining with at least one pH adjusting agent and additional solvent (e.g., water) at the fab or the point of use.
- the containers of the kit must be suitable for storing and shipping the compositions and may be, for example, NOWPak® containers (Entegris, Inc., Billerica, Mass., USA).
- the one or more containers which contain the components of the aqueous removal composition preferably include means for bringing the components in said one or more containers in fluid communication for blending and dispense.
- gas pressure may be applied to the outside of a liner in said one or more containers to cause at least a portion of the contents of the liner to be discharged and hence enable fluid communication for blending and dispense.
- gas pressure may be applied to the head space of a conventional pressurizable container or a pump may be used to enable fluid communication.
- the system preferably includes a dispensing port for dispensing the blended removal composition to a process tool.
- the aqueous removal compositions described herein are usefully employed to clean ceria particles and/or CMP contaminants (e.g., post- CMP residue and contaminants) from the surface of the microelectronic device.
- the aqueous removal compositions do not damage low-k dielectric materials (e.g., silicon oxide), silicon nitride layers, or tungsten-containing layers on the device surface.
- the aqueous removal compositions remove at least 85 % of the ceria particles present on the device prior to particle removal, more preferably at least 90 %, even more preferably at least 95 %, and most preferably at least 99%.
- the aqueous removal composition described herein may be used with a large variety of conventional cleaning tools such as megasonics and brush scrubbing, including, but not limited to, Verteq single wafer megasonic Goldfinger, OnTrak systems DDS (double-sided scrubbers), SEZ or other single wafer spray rinse, Applied Materials Mirra-MesaTM /ReflexionTM/Reflexion LKTM, and Megasonic batch wet bench systems.
- megasonics and brush scrubbing including, but not limited to, Verteq single wafer megasonic Goldfinger, OnTrak systems DDS (double-sided scrubbers), SEZ or other single wafer spray rinse, Applied Materials Mirra-MesaTM /ReflexionTM/Reflexion LKTM, and Megasonic batch wet bench systems.
- the aqueous removal composition typically is contacted with the device for a time of from about 5 sec to about 10 minutes, preferably about 1 sec to 20 min, preferably about 15 sec to about 5 min at temperature in a range of from about 20°C to about 90°C, preferably about 20°C to about 50°C.
- Such contacting times and temperatures are illustrative, and any other suitable time and temperature conditions may be employed that are efficacious to at least partially remove the ceria particles and CMP contaminants from the device, within the broad practice of the method.
- At least partially clean and substantially removal both correspond to at removal of at least 85 % of the ceria particles present on the device prior to particle removal, more preferably at least 90 %, even more preferably at least 95 %, and most preferred at least 99 %
- the aqueous removal composition may be readily removed from the device to which it has previously been applied, as may be desired and efficacious in a given end use application of the compositions described herein.
- the rinse solution includes deionized water.
- the device may be dried using nitrogen or a spin-dry cycle.
- Yet another aspect relates to the improved microelectronic devices made according to the methods described herein and to products containing such microelectronic devices.
- Another aspect relates to a recycled aqueous removal composition, wherein the removal composition may be recycled until particle and/or contaminant loading reaches the maximum amount the aqueous removal composition may accommodate, as readily determined by one skilled in the art.
- a still further aspect relates to methods of manufacturing an article comprising a microelectronic device, said method comprising contacting the microelectronic device with an aqueous removal composition for sufficient time to remove ceria particles and CMP contaminants from the microelectronic device having said particles and contaminants thereon, and incorporating said microelectronic device into said article, using a removal composition described herein.
- a method of removing ceria particles and CMP contaminants from a microelectronic device having same thereon is described.
- the method comprises polishing the microelectronic device with a CMP slurry, wherein the CMP slurry comprises ceria particles; contacting the microelectronic device with an aqueous removal composition comprising at least one pH adjusting agent, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, optionally at least one polymer, and optionally at least one oxygen scavenger, for a sufficient time to remove ceria particles and CMP contaminants from the microelectronic device to form a post-CMP particle -containing composition; and continuously contacting the microelectronic device with the post-CMP particle-containing composition for a sufficient amount of time to effect substantial cleaning of the microelectronic device.
- Any of the components described above may be used in the present method of removing ceria particles and CMP contaminants.
- Another aspect relates to an article of manufacture comprising an aqueous removal composition, a microelectronic device wafer, and material selected from the group consisting of ceria particles, CMP contaminants and combinations thereof, wherein the removal composition comprises at least one pH adjusting agent, at least one reducing agent, at least one organic additive, water, optionally at least one complexing agent, optionally at least one polymer, and optionally at least one oxygen scavenger.
- the removal compositions shown below were prepared (the balance in each formulation was DI water) and diluted 100: 1 with water.
- the process involved immersing a TEOS substrate in a ceria- containing slurry for 5 minutes, rinsing the substrate in DI water for 30 seconds, immersing the substrate in the removal composition for 60 seconds, and then rinsing with a second DI water rinse for 30 seconds.
- the temperature during immersion was room temperature.
- the extent of cleaning was determined using Scanning Electron Microscopy (SEM), Inductively Coupled Plasma Mass Spectrometry (ICP-MS), and Dark Field Microscopy (DFM), and compared to Comparative Formulation 1.
- Formulation J had 150x improved performance relative to Comparative Formulation 1.
- Formulations D, F, H, I, and N-R were also more efficient than the comparative formulation at cleaning. Of note, these formulations had a higher pH, in a range from 4-6.
- the removal compositions shown below were prepared (the balance in each formulation was DI water) and diluted 100: 1 with water.
- the process involved immersing a TEOS substrate in a ceria- containing slurry for 5 minutes, rinsing the substrate in DI water for 30 seconds, immersing the substrate in the removal composition for 60 seconds, and then rinsing with a second DI water rinse for 30 seconds.
- the temperature during immersion was room temperature.
- the extent of cleaning was determined using Scanning Electron Microscopy (SEM), Inductively Coupled Plasma Mass Spectrometry (ICP-MS), and Dark Field Microscopy (DFM).
- SEM Scanning Electron Microscopy
- ICP-MS Inductively Coupled Plasma Mass Spectrometry
- DFM Dark Field Microscopy
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Abstract
Description
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CN201880007539.6A CN110234719A (en) | 2017-01-18 | 2018-01-17 | For the composition and method from surface removal cerium oxide particles |
KR1020247015873A KR20240074891A (en) | 2017-01-18 | 2018-01-17 | Composition and Methods for removing ceria particles from a surface |
KR1020217021809A KR20210090294A (en) | 2017-01-18 | 2018-01-17 | Composition and Methods for removing ceria particles from a surface |
KR1020197020532A KR20190094426A (en) | 2017-01-18 | 2018-01-17 | Compositions and Methods for Removing Ceria Particles from a Surface |
JP2019538379A JP2020504460A (en) | 2017-01-18 | 2018-01-17 | Compositions and methods for removing ceria particles from surfaces |
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Also Published As
Publication number | Publication date |
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TW201831666A (en) | 2018-09-01 |
KR20210090294A (en) | 2021-07-19 |
KR20240074891A (en) | 2024-05-28 |
US11164738B2 (en) | 2021-11-02 |
KR20190094426A (en) | 2019-08-13 |
TWI710629B (en) | 2020-11-21 |
CN110234719A (en) | 2019-09-13 |
JP7443300B2 (en) | 2024-03-05 |
JP2021192429A (en) | 2021-12-16 |
JP2020504460A (en) | 2020-02-06 |
US20180204736A1 (en) | 2018-07-19 |
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