WO2014132641A1 - コバルト除去のための研磨スラリー - Google Patents
コバルト除去のための研磨スラリー Download PDFInfo
- Publication number
- WO2014132641A1 WO2014132641A1 PCT/JP2014/001026 JP2014001026W WO2014132641A1 WO 2014132641 A1 WO2014132641 A1 WO 2014132641A1 JP 2014001026 W JP2014001026 W JP 2014001026W WO 2014132641 A1 WO2014132641 A1 WO 2014132641A1
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- WIPO (PCT)
- Prior art keywords
- polishing composition
- acid
- polishing
- composition according
- complexing agent
- Prior art date
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- 238000005498 polishing Methods 0.000 title claims abstract description 141
- 229910017052 cobalt Inorganic materials 0.000 title abstract description 10
- 239000010941 cobalt Substances 0.000 title abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000002002 slurry Substances 0.000 title description 5
- 239000000203 mixture Substances 0.000 claims abstract description 83
- 239000008139 complexing agent Substances 0.000 claims abstract description 35
- 239000006061 abrasive grain Substances 0.000 claims abstract description 21
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphonic acid group Chemical group P(O)(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 3
- 125000000524 functional group Chemical group 0.000 claims abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 26
- 150000003839 salts Chemical class 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 125000005842 heteroatom Chemical group 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 15
- 150000003007 phosphonic acid derivatives Chemical class 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 11
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 11
- 230000007797 corrosion Effects 0.000 claims description 11
- 238000005260 corrosion Methods 0.000 claims description 11
- 125000005647 linker group Chemical group 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003112 inhibitor Substances 0.000 claims description 10
- 239000007800 oxidant agent Substances 0.000 claims description 10
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- LMHAGAHDHRQIMB-UHFFFAOYSA-N 1,2-dichloro-1,2,3,3,4,4-hexafluorocyclobutane Chemical compound FC1(F)C(F)(F)C(F)(Cl)C1(F)Cl LMHAGAHDHRQIMB-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 125000006659 (C1-C20) hydrocarbyl group Chemical group 0.000 claims description 6
- VKOLOHZSJAZWHC-UHFFFAOYSA-N 2-methyl-4-phosphonobutanoic acid Chemical compound OC(=O)C(C)CCP(O)(O)=O VKOLOHZSJAZWHC-UHFFFAOYSA-N 0.000 claims description 5
- 125000002947 alkylene group Chemical group 0.000 claims description 5
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- QQVDJLLNRSOCEL-UHFFFAOYSA-N (2-aminoethyl)phosphonic acid Chemical compound [NH3+]CCP(O)([O-])=O QQVDJLLNRSOCEL-UHFFFAOYSA-N 0.000 claims description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 4
- 239000012964 benzotriazole Substances 0.000 claims description 4
- -1 oxypropylene groups Chemical group 0.000 claims description 4
- MGRVRXRGTBOSHW-UHFFFAOYSA-N (aminomethyl)phosphonic acid Chemical compound NCP(O)(O)=O MGRVRXRGTBOSHW-UHFFFAOYSA-N 0.000 claims description 3
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 3
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 3
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims description 3
- OXHDYFKENBXUEM-UHFFFAOYSA-N glyphosine Chemical compound OC(=O)CN(CP(O)(O)=O)CP(O)(O)=O OXHDYFKENBXUEM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- NLBSQHGCGGFVJW-UHFFFAOYSA-N 2-carboxyethylphosphonic acid Chemical compound OC(=O)CCP(O)(O)=O NLBSQHGCGGFVJW-UHFFFAOYSA-N 0.000 claims description 2
- FOEWAQDQXRTJTP-UHFFFAOYSA-N 2-iminoethylphosphonic acid Chemical compound OP(O)(=O)CC=N FOEWAQDQXRTJTP-UHFFFAOYSA-N 0.000 claims description 2
- FDQQNNZKEJIHMS-UHFFFAOYSA-N 3,4,5-trimethylphenol Chemical compound CC1=CC(O)=CC(C)=C1C FDQQNNZKEJIHMS-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- BJFLSHMHTPAZHO-UHFFFAOYSA-N benzotriazole Chemical compound [CH]1C=CC=C2N=NN=C21 BJFLSHMHTPAZHO-UHFFFAOYSA-N 0.000 claims description 2
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 2
- 229940042400 direct acting antivirals phosphonic acid derivative Drugs 0.000 claims description 2
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 125000006353 oxyethylene group Chemical group 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 30
- 238000005530 etching Methods 0.000 abstract description 12
- 229910052802 copper Inorganic materials 0.000 abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 5
- 230000003068 static effect Effects 0.000 abstract description 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 14
- 230000004888 barrier function Effects 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000011164 primary particle Substances 0.000 description 9
- 125000004432 carbon atom Chemical group C* 0.000 description 7
- 239000008119 colloidal silica Substances 0.000 description 6
- 239000011163 secondary particle Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 125000000753 cycloalkyl group Chemical group 0.000 description 4
- 229920002635 polyurethane Polymers 0.000 description 4
- 239000004814 polyurethane Substances 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000000872 buffer Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000000645 desinfectant Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004475 Arginine Substances 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 2
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 150000005215 alkyl ethers Chemical class 0.000 description 2
- 125000000304 alkynyl group Chemical group 0.000 description 2
- 229940121375 antifungal agent Drugs 0.000 description 2
- 239000003429 antifungal agent Substances 0.000 description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 2
- 235000018417 cysteine Nutrition 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- UDPGUMQDCGORJQ-UHFFFAOYSA-N (2-chloroethyl)phosphonic acid Chemical compound OP(O)(=O)CCCl UDPGUMQDCGORJQ-UHFFFAOYSA-N 0.000 description 1
- MLIWQXBKMZNZNF-KUHOPJCQSA-N (2e)-2,6-bis[(4-azidophenyl)methylidene]-4-methylcyclohexan-1-one Chemical compound O=C1\C(=C\C=2C=CC(=CC=2)N=[N+]=[N-])CC(C)CC1=CC1=CC=C(N=[N+]=[N-])C=C1 MLIWQXBKMZNZNF-KUHOPJCQSA-N 0.000 description 1
- PZIVQNCOTRXRLT-UHFFFAOYSA-N 1-(4-iodophenyl)-n,n,2-trimethylpropan-2-amine Chemical compound CN(C)C(C)(C)CC1=CC=C(I)C=C1 PZIVQNCOTRXRLT-UHFFFAOYSA-N 0.000 description 1
- 229940100555 2-methyl-4-isothiazolin-3-one Drugs 0.000 description 1
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 1
- GUUULVAMQJLDSY-UHFFFAOYSA-N 4,5-dihydro-1,2-thiazole Chemical compound C1CC=NS1 GUUULVAMQJLDSY-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- 229940120146 EDTMP Drugs 0.000 description 1
- AZIHIQIVLANVKD-UHFFFAOYSA-N N-(phosphonomethyl)iminodiacetic acid Chemical compound OC(=O)CN(CC(O)=O)CP(O)(O)=O AZIHIQIVLANVKD-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- KIDJHPQACZGFTI-UHFFFAOYSA-N [6-[bis(phosphonomethyl)amino]hexyl-(phosphonomethyl)amino]methylphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCCCCCN(CP(O)(O)=O)CP(O)(O)=O KIDJHPQACZGFTI-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- DHNRXBZYEKSXIM-UHFFFAOYSA-N chloromethylisothiazolinone Chemical compound CN1SC(Cl)=CC1=O DHNRXBZYEKSXIM-UHFFFAOYSA-N 0.000 description 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 1
- 238000004690 coupled electron pair approximation Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002356 laser light scattering Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 125000003226 pyrazolyl group Chemical group 0.000 description 1
- 125000000714 pyrimidinyl group Chemical group 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
Classifications
-
- 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
- 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
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Definitions
- the present invention relates to a polishing composition for removing cobalt (Co) selectively with respect to, for example, copper (Cu) and a method for using the same.
- a semiconductor wafer has a silicon wafer and an insulating layer including a large number of trenches provided in order to form a pattern for circuit wiring.
- the barrier layer usually covers the patterned insulating layer, and the metal layer covers the barrier layer.
- the metal layer is at least thick enough to fill the patterned trench with metal to form circuit wiring.
- the CMP process removes the metal layer from the underlying barrier layer and, in the next step, removes the metal layer while at the same time leaving a smooth surface with the metal-filled trench on the wafer. Provide circuit wiring that is flat against the surface.
- the barrier layer remaining on the semiconductor wafer is removed from the insulating layer of the underlying semiconductor wafer to provide a flat polished surface on the insulating layer.
- an efficient removal method of a metal layer (copper) and a barrier layer (tantalum) as described in Patent Document 1 below has been proposed.
- the metal layer usually includes a Cu connection line, and the barrier layer is formed of Ta, nitride or the like.
- the barrier layer is formed of Ta, nitride or the like.
- each layer in the wiring formation process tends to become thinner.
- the “Ta or TaN” layer used as the wiring material is thinned, the effect of preventing the diffusion of Cu is lowered, and the adhesion with the Cu layer is also lowered. Therefore, as an alternative to the Ta (or TaN) layer, or by sandwiching a Co (cobalt) layer that is familiar with Cu between the Ta (or TaN) layer and the Cu layer, the diffusion of Cu is suppressed, and the adhesion to the upper layer is achieved. A process to supplement sex has come out.
- the Co barrier layer When selectively polishing and removing such a Co barrier layer from the copper connection line, the Co barrier layer is not only efficiently polished and removed, but also selective to the Cu connection line while suppressing the etching rate of Co. In addition, it is required to stably polish and remove the Co barrier layer.
- compositions and methods provided by the present invention are directed to solving these and related problems.
- the present invention provides an abrasive composition having a pH of 9 or more comprising abrasive grains and one or more Co complexing agents.
- the Co complexing agent has one or more functional groups selected from a phosphonic acid (—P ( ⁇ O) (OH) 2 ) group or a carboxyl (—C ( ⁇ O) OH) group.
- the Co complexing agent comprises one or more phosphonic acid derivatives.
- the phosphonic acid derivative contains one or more phosphonic acid (—P ( ⁇ O) (OH) 2 ) groups or salts thereof covalently bonded to the nucleus by a bond or a linker
- the nucleus is selected from a heteroatom or a C 1 -C 20 hydrocarbyl moiety, wherein the hydrocarbyl moiety is optionally substituted by one or more of 1-5 heteroatoms and 1-5 hydroxy groups
- the linker is a divalent or trivalent heteroatom or a divalent or trivalent C 1 -C 20 hydrocarbyl moiety, wherein the hydrocarbyl moiety is optional by one or more of 1-5 heteroatoms and 1-5 hydroxy groups Is replaced with
- the heteroatoms are independently selected from N, O, S, P and oxides of N, S and P.
- the Co complexing agent is citric acid, citrate, ethylenediaminetetraacetic acid (EDTA), 2-hydroxyphosphonoacetic acid (HPAA), phosphonobutane-3 carboxylic acid (PBTC) and aminotri (methylenephosphonic acid). (ATMP) is included. Further, in one embodiment, the Co complexing agent is selected from citric acid, citrate, ethylenediaminetetraacetic acid (EDTA).
- the polishing composition can further include ammonia, or bicarbonate or a salt thereof as a Co polishing accelerator. In other embodiments, the polishing composition comprises a Co complexing agent and no ammonia. In yet another embodiment, the polishing composition comprises a Co complexing agent and no bicarbonate and salts thereof. In yet another embodiment, the polishing composition includes a Co complexing agent and does not include ammonia and bicarbonate and salts thereof.
- the Co complexing agent enables high polishing removal rates, especially by complexing cobalt metal ions in solution.
- Salts can act as removal rate enhancers by functioning as coordination complexes and / or electrolytes.
- ammonia added at high pH can facilitate complexing cobalt in solution.
- Bicarbonate or a salt thereof can act to compress the bilayer around the particles to enhance mechanical removal during polishing.
- the salts of any complex can function as an electrolyte in solution.
- the phosphonic acid derivative further comprises one or more carboxylic acid groups or salts thereof.
- the phosphonic acid derivative is a compound represented by the following formula (I) or a salt thereof, and in the following formula (I), ⁇ is a nucleus, and each L is a bond or a linker, respectively. Wherein the nucleus and linker are defined above, each u is 0-3, each v is 0-3, and y is 1-5, provided that the derivative is at least It contains at least one of phosphonic acid or a salt thereof.
- the nucleus is a heteroatom. In other embodiments, the nucleus is a hydrocarbyl moiety selected from alkylene optionally substituted with 1-3 hydroxy groups. In other embodiments, the Co complexing agent is present by weight percent to 5% or less, 3% or less or 1% or less, or even lower, 0.1% or 0.01% or less in the polishing composition. .
- complexing agent means one or more complexing agents.
- “About” means ⁇ 1%, ⁇ 5% or ⁇ 10% of the amount, as indicated by the context. As used herein, every amount and each range is followed by the term “about”.
- “Hydrocarbyl” refers to a moiety containing carbon and hydrogen atoms. The number of carbon atoms is usually about 1 to 30 (C 1 to C 30 ). Examples of hydrocarbyl groups include, but are not limited to, alkyl, alkenyl, alkynyl, aryl, cycloalkyl, alkylene, and combinations thereof.
- Alkyl refers to a saturated, linear or branched, monovalent hydrocarbyl moiety. The number of carbon atoms is usually 1-20.
- Alkenyl refers to a straight or branched, monovalent hydrocarbyl moiety. The number of carbon atoms is usually 1-20 and contains up to 3 carbon double bonds.
- Alkynyl refers to a straight or branched, monovalent hydrocarbyl moiety. The number of carbon atoms is usually 1-20 and contains up to 3 carbon triple bonds.
- Aryl means an aromatic cyclic hydrocarbyl moiety. The number of carbon atoms is usually 6-10.
- Cycloalkyl means a cyclic, non-aromatic hydrocarbyl moiety.
- Cycloalkyls can be fully saturated or partially unsaturated. The number of carbon atoms is usually 3-15. Partially unsaturated cycloalkyl groups have 1 to 4 carbon-carbon double bonds.
- Alkylene means a saturated, divalent, straight chain or branched hydrocarbyl moiety. The number of carbon atoms is usually 2-20.
- the present invention provides a polishing composition
- a polishing composition comprising colloidal silica, a Co complexing agent, an oxidizing agent, a surfactant, and optionally a corrosion inhibitor.
- the Co complexing agent includes one or more of a phosphonic acid derivative, citric acid or a salt thereof and ethylenediaminetetraacetic acid (EDTA), and optionally further includes ammonia, or bicarbonate or a salt thereof
- Derivatives contain one or more phosphonic acid (—P ( ⁇ O) (OH) 2 ) groups or salts thereof that are each covalently attached to the nucleus by a bond or linker.
- the nucleus is selected from a heteroatom or a C 1 -C 20 hydrocarbyl moiety, wherein the hydrocarbyl moiety is optionally substituted with 1 to 5 heteroatoms and / or 1 to 5 hydroxy groups, and the linker is divalent or trivalent hetero It is an atomic or divalent or trivalent C 1 -C 20 hydrocarbyl moiety.
- the hydrocarbyl moiety is optionally substituted with 1 to 5 heteroatoms and / or 1 to 5 hydroxy groups, and the heteroatoms are each selected from N, O, S, P and oxides thereof.
- the polishing composition optionally includes ammonia, bicarbonate or a salt thereof, glycine, arginine, cysteine, or the like as a Co polishing accelerator. In other embodiments, the polishing composition does not include ammonia. In yet other embodiments, the polishing composition does not include bicarbonate and salts thereof. In yet another embodiment, the polishing composition does not include a Co polishing accelerator such as ammonia or bicarbonate. In other embodiments, the phosphonic acid derivative further comprises one or more carboxylic acid groups or salts thereof.
- the phosphonic acid derivative is a compound represented by the following formula (I) or a salt thereof, and in the following formula (I), ⁇ is a nucleus, and each L is a bond or a linker. And the nucleus and linker are defined above, each u is 1 to 5 each, each v is 0 to 3 and y is 1 to 5, respectively.
- the derivative contains at least one of phosphonic acid or a salt thereof.
- the phosphonic acid derivative as the Co complexing agent is 2-aminoethylphosphonic acid (AEPn, molecular weight 125.06 g / mol), dimethyl methylphosphonate (DMMP, molecular weight 124.08 g / mol), 1-hydroxyethylidene -1,1-diphosphonic acid (HEDP, molecular weight 206.03 g / mol), aminotri (methylenephosphonic acid) (ATMP, molecular weight 299.05 g / mol), ethylenediaminetetra (methylenephosphonic acid) (EDTMP, molecular weight 436.12 g / mol), tetramethylenediaminetetra (methylenephosphonic acid) (TDTMP, molecular weight 464.18 g / mol), hexamethylenediaminetetra (methylenephosphonic acid) (HDTMP, molecular weight 492.23 g / mol), diethylenetriaminepe.
- the nucleus is a heteroatom. In other embodiments, the nucleus is a hydrocarbyl moiety selected from alkylene optionally substituted with 1-3 hydroxy groups.
- the phosphonic acid derivative as the Co complexing agent in the present invention preferably has a smaller molecular weight. More specifically, the molecular weight of the Co complexing agent is preferably 350.00 g / mol or less, more preferably 300.00 g / mol, and even more preferably 280.00 g / mol. When the molecular weight is 350.00 g / mol or less, there is a tendency that a practical level of Co polishing rate and the effect of suppressing etching can be compatible.
- the phosphonic acid derivative as the Co complexing agent in the present invention preferably has 3 or less phosphonic acid (—P ( ⁇ O) (OH) 2 ) groups.
- the Co complexing agent comprises citric acid or a salt thereof, EDTA, 2-hydroxyphosphonic acid (HPAA), phosphonobutane-3carboxylic acid (PBTC), or aminotri (methylenephosphonic acid) (ATMP).
- a Co polishing accelerator ammonia, bicarbonate or a salt thereof, glycine, arginine, cysteine and the like are included.
- the content of the Co complexing agent is preferably 5% or less in the polishing composition, more preferably 3% or less, and even more preferably 1% or less.
- the content of the optional Co polishing accelerator is preferably% by mass and 5% or less in the polishing composition, more preferably 3% or less, and even more preferably 1% or less. is there.
- the content of the Co polishing accelerator exceeds 5%, the Co etching rate tends to increase.
- the abrasive is silica, such as, but not limited to, colloidal silica, alumina, or ceria. Of these abrasive grains, colloidal silica is preferred.
- the content of the abrasive grains is% by mass, preferably 0.1% or more in the polishing composition, more preferably 0.5% or more, and further preferably 1.0% or more. As the abrasive content increases, the mechanical action increases, so the Co polishing rate tends to improve. Further, the content of the abrasive grains is preferably% by mass, and preferably 20% or less, more preferably 10% or less in the polishing composition. As the content of the abrasive grains decreases, the dispersibility of the abrasive grains in the polishing composition tends to improve.
- the average primary particle diameter of the abrasive grains is preferably 5 nm or more, more preferably 7 nm or more, and further preferably 10 nm or more. As the average primary particle diameter of the abrasive grains increases, the Co polishing rate tends to improve. In addition, the value of the average primary particle diameter of an abrasive grain can be calculated based on the specific surface area of the abrasive grain measured by BET method, for example. The average primary particle diameter of the abrasive grains is also preferably 150 nm or less, more preferably 110 nm or less, and still more preferably 100 nm or less. As the average primary particle diameter of the abrasive grains decreases, it tends to be easier to obtain a polished surface with fewer defects such as scratches by polishing the object to be polished.
- the average secondary particle diameter of the abrasive grains is preferably 300 nm or less, more preferably 270 nm or less, and further preferably 250 nm or less. As the average secondary particle diameter of the abrasive grains decreases, it tends to be easier to obtain a polished surface with fewer defects such as scratches by polishing the object to be polished.
- the value of the average secondary particle diameter of the abrasive grains can be measured by, for example, a laser light scattering method.
- the shape of the abrasive grains may be spherical or non-spherical.
- non-spherical shape examples include a so-called cocoon shape having a constriction at the center, a confetti shape having a plurality of protrusions on the surface, a rugby ball shape, an aggregate shape, and the like.
- the non-spherical abrasive grains may be aggregates of primary particles.
- the polishing composition can further comprise one or more of an oxidizing agent, a corrosion inhibitor, and a surfactant.
- the content of the oxidizing agent is preferably 0.1% or more, more preferably 0.5% or more in the polishing composition in terms of mass%.
- the content of the oxidizing agent is preferably% by mass, and is preferably 4% or less, more preferably 3% or less in the polishing composition.
- oxidants include H 2 O 2 , persulfate, nitric acid, potassium periodate, hypochlorous acid and ozone water. In other embodiments, the oxidant is H 2 O 2 .
- the content of the corrosion inhibitor is% by mass, preferably 0.1% or more, more preferably 0.2% or more in the polishing composition. Moreover, content of a corrosion inhibitor is the mass%, and 0.4% or less is preferable in polishing composition, More preferably, it is 0.3%. When the content of the corrosion inhibitor is less than 0.2% or more than 0.4%, it tends to be difficult to obtain a practical level of corrosion inhibition effect.
- the corrosion inhibitor is a heterocyclic or heteroaryl compound having at least a 5-6 membered ring, having two or more double bonds, and having one or more nitrogen atoms.
- Non-limiting examples include compounds having a pyridine ring, a pyrazole ring, a pyrimidine ring, an imidazole ring, and a triazole or benotriazole ring.
- the corrosion inhibitor is benzotriazole (BTA).
- content of surfactant is the mass%, and 0.01% or more is preferable in polishing composition, More preferably, it is 0.02% or more. Further, the content of the surfactant is, by mass, preferably 2% or less, more preferably 1% or less in the polishing composition.
- the surfactant consists of a compound of formula (II): R 1 —O— [CH 2 CH (CH 3 ) O] m — [CH 2 CH 2 O] n —H (II)
- R 1 is C 1 -C 10 alkyl
- m and n are selected such that the oxyethylene and oxypropylene groups are present in a mass ratio of 1: 1 to 3: 1.
- the surfactant comprises a polyethylene glycol alkyl ether and / or a polypropylene glycol alkyl ether.
- the pH of the polishing composition is preferably 9 or more, more preferably 9.5 or more. Moreover, it is preferable that pH of polishing composition is 14 or less, More preferably, it is 12 or less. When the pH of the polishing composition is less than 9 or exceeds 14, it tends to be difficult to achieve both a practical level of Co polishing rate and etching suppression.
- the pH is maintained using acids or alkalis such as ammonia, alkalis, organic bases, carbonates or bicarbonates, optionally buffers.
- acids, including organic and inorganic acids, and buffers, including but not limited to acidic, neutral and alkaline buffers, are beneficial for this purpose.
- one compound may be sufficient as the compound for adjusting these pH, and what mixed two or more compounds may be sufficient as it.
- other additives for example, Co complexing agent, Co polishing accelerator, etc.
- the additive is used as a part of the compound for adjusting the pH. can do.
- the static etching of cobalt is close to zero at pH 9 and above due to the protective nature of the cobaltous hydroxide film formed during polishing.
- metal CMP processes are deployed to ensure a high polishing rate while maintaining a low etch rate.
- a polishing method comprising selectively polishing Co in the presence of Cu using the composition provided by the present invention.
- the Co removal rate is between 200 ⁇ / min and 2400 ⁇ / min.
- the Cu removal rate is less than 100 ⁇ / min, or less than 80 ⁇ / min.
- the Co: Cu removal selectivity is 5 or more, 10 or more, or 15 or more.
- Co: Cu selectivity is determined by dividing the Co removal rate by the Cu removal rate. Due to the limitations of measurement sensitivity, the removal rate of Cu below 100 ⁇ / min is approximated to 100 ⁇ / min, so that the determined Co / Cu selectivity can be higher than the values provided herein.
- the polishing composition of the present invention may further comprise a disinfectant or antifungal agent.
- disinfectants and antifungal agents include 2-methyl-4-isothiazolin-3-one and 5-chloro-methyl-4-isothiazolin-3-one, p-hydroxybenzoate, and phenoxyethanol These are isothiazoline-based disinfectants.
- the polishing composition used in polishing is prepared by diluting the stock solution (concentrated product) of the polishing composition 2 to 10 times or more with a diluent such as an aqueous solution or water.
- the abrasive grains and Co complexing agent are mixed in water and the pH of the composition is adjusted by a pH adjusting agent (eg potassium hydroxide, ammonia, etc.) Adjust appropriately.
- the temperature at which each component is mixed is not particularly limited, but is preferably 10 to 40 ° C., and may be heated to increase the dissolution rate. Further, the mixing time is not particularly limited.
- a polishing apparatus a general holder having a polishing surface plate on which a holder for holding a substrate having a polishing object and a motor capable of changing the number of rotations are attached and a polishing pad (polishing cloth) can be attached.
- a polishing apparatus can be used.
- the polishing conditions are not particularly limited.
- the rotation speed of the polishing platen is preferably 10 to 500 rpm, and the pressure (polishing pressure) applied to the substrate having the object to be polished is preferably 0.5 to 10 psi.
- the method of supplying the polishing composition to the polishing pad is not particularly limited, and for example, a method of continuously supplying with a pump or the like is employed. Although the supply amount is not limited, it is preferable that the surface of the polishing pad is always covered with the polishing composition of the present invention. After the polishing is completed, the substrate is washed in running water, and water droplets adhering to the substrate are removed by a spin dryer or the like and dried to obtain a substrate.
- the wafer is polished for a fixed time, and the polishing rate of the surface of another wafer described in the example of Co or the like is measured.
- the wafer is immersed in the polishing composition for a fixed time, and the etching rate of other wafers described in the examples such as Co is measured.
- the polishing rate or etching rate is calculated by measuring the difference in wafer thickness before and after polishing or immersion and the polishing or immersion time. The difference in thickness is measured using, for example, an optical interference type film thickness measuring device.
- Example 1 Using the polishing compositions of Invention Examples 1 to 12 and Comparative Examples 1 to 9 having the compositions shown in Table 1, respectively, using a soft porometric polyurethane pad, a Co wafer having a diameter of 200 mm, Table 1 shows the polishing rates when polishing was performed at a slurry supply rate of 200 mL / min, a polishing pressure of 2 psi, a platen rotation speed of 127 rpm, and a head rotation speed of 122 rpm.
- the supply rate of the polishing composition slurry is a value obtained by assigning the total supply amount of all the supply liquids per unit time (the same applies to the following examples).
- the colloidal silica used in Example 1 has an average primary particle size of about 35 nm and an average secondary particle size of about 70 nm, and potassium hydroxide was used as a compound for adjusting pH. It can be seen that by using Invention Examples 1 to 12, which are polishing compositions of the present invention, Co can be efficiently removed while suppressing the etching rate of Co. In contrast, Comparative Examples 1 to 4, 7 and 8 have a high Co etching rate, Comparative Examples 5 and 9 show no improvement in the Co removal rate, and Comparative Example 6 has a Co removal rate and a Co etching rate. It fluctuated greatly and was unstable
- Example 2 Using the polishing compositions of Invention Examples 13 to 20 having the compositions shown in Table 2, each using a soft porometric polyurethane pad, copper (Cu), Co, tantalum (Ta), tetraethyl ortho having a diameter of 200 mm
- polishing composition slurry feed rate is 200 mL / min
- polishing pressure is 2 psi
- platen rotation speed is 127 rpm
- head rotation Table 3 shows the polishing speed when polishing was performed at a speed of 121 rpm.
- the colloidal silica used in Example 2 has an average primary particle size of about 35 nm and an average secondary particle size of about 70 nm, and potassium hydroxide was used as a compound for adjusting pH. It can be seen that a high polishing rate ratio of Co to Cu can be obtained by using the polishing composition of the present invention. It can be seen that the smaller the molecular weight of the Co complexing agent, the higher the polishing rate of Co and the higher polishing rate ratio of Co to Cu. It can also be seen that the inclusion of two or more Co complexing agents or a Co polishing accelerator can provide a high Co polishing rate and a high Co polishing rate ratio of Co to Cu.
- Example 3 Polishing compositions for Cu, Co, Ta, TEOS and BD wafers with a diameter of 200 mm using the polishing compositions of Invention Examples 21 and 22 having the compositions shown in Table 4, respectively, using soft porometric polyurethane pads.
- Table 5 shows the polishing rates when polishing was performed at a supply rate of 200 mL / min, a polishing pressure of 2 psi, a platen rotation speed of 127 rpm, and a head rotation speed of 121 rpm.
- the colloidal silica used in Example 2 has an average primary particle size of about 35 nm and an average secondary particle size of about 70 nm, and the compounds shown in Table 4 were used as the compounds for adjusting the pH.
- each of the polishing composition slurry for 200 mm diameter Cu, Co, Ta, TEOS and BD wafers using a soft porometric polyurethane pad Table 7 shows the polishing speed when polishing was performed at a supply speed of 200 mL / min, a polishing pressure of 2 psi, a platen rotation speed of 127 rpm, and a head rotation speed of 121 rpm. It can be seen that a high polishing rate ratio of Co to Cu can be obtained by using the polishing composition of the present invention.
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Abstract
Description
このようなCoバリア層を銅の接続線から選択的に研磨除去する際には、単に効率的に研磨、除去することだけでなく、Coのエッチング速度を抑えつつCu接続線に対して選択的にCoバリア層を安定して研磨、除去することが要求されている。
一実施形態では、Co錯化剤は、一つ以上のホスホン酸誘導体を含む。ホスホン酸誘導体は、結合手又はリンカーによって核に共有結合した一つ以上のホスホン酸(―P(=O)(OH)2)基またはその塩の一つ以上を含み、
核はヘテロ原子またはC1~C20ヒドロカルビル部から選択され、ヒドロカルビル部は1~5のヘテロ原子および1~5のヒドロキシ基の一つ以上によって任意に置換され、
リンカーは二価または三価のヘテロ原子または二価のまたは三価のC1~C20ヒドロカルビル部であり、ヒドロカルビル部は1~5のヘテロ原子および1~5のヒドロキシ基の一つ以上によって任意に置換され、
ヘテロ原子はN、O、S、PおよびN、S及びPの酸化物から独立して選択される。
一実施形態において、研磨組成物は、さらに、Co研磨促進剤としてアンモニア、または重炭酸またはその塩を含むことができる。他の実施形態では、研磨組成物は、Co錯化剤を含み、アンモニアを含まない。さらに別の実施形態では、研磨組成物は、Co錯化剤を含み、重炭酸およびその塩を含まない。さらに別の実施形態では、研磨組成物は、Co錯化剤を含んで、アンモニアおよび重炭酸およびその塩を含まない。
他の実施形態では、Co錯化剤は、質量%で、研磨組成物中5%以下、3%以下または1%の以下、または、さらに低く0.1%、0.01%以下まで存在する。
単数で表される用語は前後関係から示されるように複数形を含む。例えば、錯化剤は、一つ以上の錯化剤を意味する。
「約」は前後関係から示されるように、量の±1%、±5%または±10%を意味する。本明細書で使用されるように、あらゆる量および各々その範囲は、「約」の用語に続く。
「ヒドロカルビル」は、炭素および水素原子を含有する部位を示す。炭素原子数は、通常約1~30(C1~C30)である。ヒドロカルビル基の例としては、アルキル、アルケニル、アルキニル、アリール、シクロアルキル、アルキレンおよびそれらの組み合わせが挙げられるが、これに限定されるものではない。
「アルケニル」は、直鎖または分岐、一価のヒドロカルビル部を示す。炭素原子数は、通常1~20であり、炭素二重結合を3つまで含有する。
「アルキニル」は、直鎖または分岐、一価のヒドロカルビル部を示す。炭素原子数は、通常1~20であり、炭素三重結合を3つまで含有する。
「アリール」は、芳香族の環状ヒドロカルビル部を意味する。炭素原子数は、通常6~10である。
「シクロアルキル」は、環状、非芳香族ヒドロカルビル部を意味する。シクロアルキルは、完全に飽和か、または、部分的に不飽和であることができる。炭素原子数は、通常3~15である。部分的に不飽和なシクロアルキル基は、1~4の炭素―炭素二重結合を有する。
「アルキレン」は、飽和、二価、直鎖または分岐ヒドロカルビル部を意味する。炭素原子数は、通常2~20である。
他の実施形態では、ホスホン酸誘導体は、カルボン酸基またはその塩の一つ以上を更に含む。他の実施形態では、ホスホン酸誘導体は下記式(I)で示される化合物、または、その塩であり、下記式(I)において、○は核であり、各Lはそれぞれに結合手またはリンカーであり、核およびリンカーは上記で定義され、各uはそれぞれに1~5であり、各vはそれぞれに0~3であり、yは1~5である。ただし、誘導体はホスホン酸またはその塩の少なくとも一つを含む。
他の実施形態においては、本発明におけるCo錯化剤としてのホスホン酸誘導体は、分子量が小さい方が好ましい。より具体的には、Co錯化剤の分子量は、350.00g/mol以下が好ましく、より好ましくは300.00g/mol、さらに好ましくは280.00g/molである。分子量が350.00g/mol以下の場合には、実用的なレベルのCoの研磨速度とエッチング抑制の効果が両立できる傾向にある。
他の実施形態では、Co錯化剤は、クエン酸またはその塩、EDTA、2―ヒドロキシホスホン酸(HPAA)、ホスホノブタン―3カルボン酸(PBTC)、またはアミノトリ(メチレンホスホン酸)(ATMP)を含み、更に任意に、Co研磨促進剤として、アンモニア、重炭酸またはその塩、グリシン、アルギニン、システイン等を含む。
他の実施形態では、任意に含まれるCo研磨促進剤の含有量は、質量%で、研磨組成物中5%以下であることが好ましく、より好ましくは3%以下、さらに好ましくは1%以下である。Co研磨促進剤の含有量が5%を超えると、Coエッチング速度が高くなる傾向にある。
他の実施形態では、砥粒の形状は、球形(spherical)であってもよいし、非球形であってもよい。非球形状の例としては、中央部にくびれを有するいわゆる繭形状(Cocoon)や、表面に複数の突起を有する金平糖形状、ラグビーボール形状、凝集体形状(aggregate)などが挙げられる。非球形状の砥粒は、一次粒子の会合体であってもよい。
他の実施形態では、研磨組成物は更に、酸化剤、腐食抑制剤、および界面活性剤の1以上を含むことができる。
R1―O―[CH2CH(CH3)O]m―[CH2CH2O]n―H (II)
上記式(II)において、R1はC1~C10アルキルであり、mおよびnはオキシエチレン基およびオキシプロピレン基が1:1~3:1の質量比で存在するように選択される。一実施形態において、界面活性剤は、ポリエチレングリコールアルキルエーテルおよび/またはポリプロピレングリコールアルキルエーテルを含む。
いくつかの実施形態において、本発明の研磨組成物は更に、消毒剤又は抗真菌剤を含んでもよい。消毒剤及び抗真菌剤の限定的でない例としては、2-メチル-4-イソチアゾリン-3-オン及び5-クロロ-メチル-4-イソチアゾリン-3-オン、p-ヒドロキシ安息香酸エステル、及びフェノキシエタノール等のイソチアゾリン系消毒剤が挙げられる。
いくつかの実施形態では、研磨で使用される研磨組成物は、水溶液又は水等の希釈液を用いて、研磨組成物の原液(濃縮品)を2~10倍以上に希釈することによって調製される。
一般に、砥粒及びCo錯化剤を水中で混合し、組成物のpHをpH調製剤(例えば、水酸化カリウム、アンモニア等)によって適切に調整する。各成分を混合する際の温度は特に制限されないが、10~40℃が好ましく、溶解速度を上げるために加熱してもよい。また、混合時間も特に制限されない。
研磨装置としては、研磨対象物を有する基板等を保持するホルダーと回転数を変更可能なモータ等とが取り付けてあり、研磨パッド(研磨布)を貼り付け可能な研磨定盤を有する一般的な研磨装置を使用することができる。
研磨終了後、基板を流水中で洗浄し、スピンドライヤ等により基板上に付着した水滴を払い落として乾燥させることにより、基板が得られる。
表1に示される組成の発明例1~12及び比較例1~9の研磨組成物を使用して、それぞれ柔らかいポロメトリックポリウレタン・パッドを使用して、直径200mmのCoウェハについて、研磨組成物のスラリーの供給速度を200mL/分、研磨の圧力を2psi、プラテン回転速度を127rpm、ヘッド回転速度を122rpmとして研磨した際の研磨速度をそれぞれ表1に示した。なお、研磨組成物スラリーの供給速度とは、全供給液の供給量の合計を単位時間当たりで割り付けた値をいう(以下の実施例においても同様)。また、本実施例1で使用したコロイダルシリカは平均一次粒子径約35nm、平均二次粒子径約70nmであり、pHを調整するための化合物としては水酸化カリウムを使用した。
本発明の研磨組成物である発明例1~12を使用することにより、Coのエッチング速度を抑えつつ効率的にCoを除去できることがわかる。これに対して、比較例1~4、7および8ではCoエッチング速度が高く、比較例5および9ではCo除去速度の向上が見られず、比較例6では、Co除去速度およびCoエッチング速度が大きく変動し、不安定であった
表2に示される組成の発明例13~20の研磨組成物を使用して、それぞれ柔らかいポロメトリックポリウレタン・パッドを使用して、直径200mmの銅(Cu)、Co、タンタル(Ta)、テトラエチルオルソシリケート(TEOS)及びLow-k誘導体材料としてのブラックダイヤモンド(商標)(BD)ウェハについて、研磨組成物のスラリーの供給速度を200mL/分、研磨の圧力を2psi、プラテン回転速度を127rpm、ヘッド回転速度を121rpmとして研磨した際の研磨速度をそれぞれ表3に示した。なお、本実施例2で使用したコロイダルシリカは平均一次粒子径約35nm、平均二次粒子径約70nmであり、pHを調整するための化合物としては水酸化カリウムを使用した。
本発明の研磨組成物を使用することにより、特に、Cuに対するCoの高い研磨速度比を得られることがわかる。Co錯化剤の分子量がより小さい方が、Coの高い研磨速度とCuに対するCoの高い研磨速度比を得られることがわかる。また、Co錯化剤を2つ以上またはCo研磨促進剤を含む方が、Coの高い研磨速度とCuに対するCoの高い研磨速度比を得られることがわかる。
表4に示される組成の発明例21及び22の研磨組成物を使用して、それぞれ柔らかいポロメトリックポリウレタン・パッドを使用して、直径200mmのCu、Co、Ta、TEOS及びBDウェハについて、研磨組成物のスラリーの供給速度を200mL/分、研磨の圧力を2psi、プラテン回転速度を127rpm、ヘッド回転速度を121rpmとして研磨した際の研磨速度をそれぞれ表5に示した。なお、本実施例2で使用したコロイダルシリカは平均一次粒子径約35nm、平均二次粒子径約70nmであり、pHを調整するための化合物としては表4に記載の化合物を使用した。
本発明の研磨組成物を使用することにより、特に、Cuに対するCoの高い研磨速度比を得られることがわかる。また、pHを調整する機能を備えるCo研磨促進剤として添加しているアンモニアが、pHを調整するための化合物を兼ねていても、Coの高い研磨速度とCuに対するCoの高い研磨速度比を得られることがわかる。
本発明の研磨組成物を使用することにより、特に、Cuに対するCoの高い研磨速度比を得られることがわかる。
Claims (23)
- 砥粒および一つ以上のCo錯化剤を含む研磨組成物であって、
前記研磨組成物は9以上のpHを有し、
前記Co錯化剤は、ホスホン酸(―P(=O)(OH)2)基またはカルボキシル(―C(=O)OH)基から選ばれる一つ以上の官能基を有することを特徴とする研磨組成物。 - 前記Co錯化剤は一つ以上のホスホン酸誘導体を含み、
前記ホスホン酸誘導体は、結合手又はリンカーによってそれぞれ核に共有結合により付着した一つ以上のホスホン酸(―P(=O)(OH)2)基またはその塩を含み、
前記核はヘテロ原子またはC1~C20ヒドロカルビル部から選択され、前記ヒドロカルビル部は1~5のヘテロ原子および/または1~5のヒドロキシ基によって任意に置換され、
前記リンカーは二価または三価のヘテロ原子または二価のまたは三価のC1~C20ヒドロカルビル部であり、前記ヒドロカルビル部は1~5のヘテロ原子および/または1~5のヒドロキシ基によって任意に置換され、
前記ヘテロ原子はN、O、S、PおよびN、S及びPの酸化物から独立して選択される請求項1に記載の研磨組成物。 - 前記ホスホン酸誘導体が一つ以上のカルボン酸基またはその塩をさらに含む請求項2に記載の研磨組成物。
- 前記核がヘテロ原子である請求項2に記載の研磨組成物。
- 前記核が1~3のヒドロキシ基によって任意に置換されるアルキレンから選択されるヒドロカルビル部である請求項2に記載の研磨組成物。
- 前記Co錯化剤は、2―アミノエチルホスホン酸、メチルホスホン酸ジメチル、1―ヒドロキシエチリデン―1,1―ジホスホン酸、アミノトリ(メチレンホスホン酸)、エチレンジアミンテトラ(メチレンホスホン酸)、テトラメチレンジアミンテトラ(メチレンホスホン酸)、ヘキサメチレンジアミンテトラ(メチレンホスホン酸)、ジエチレントリアミンペンタ(メチレンホスホン酸)、ホスホノブタン―3カルボン酸、N―(ホスホノメチル)イミノジ酢酸、2―カルボキシエチルホスホン酸、2―ヒドロキシホスホノ酢酸、アミノメチルホスホン酸、N,N―ビス(ホスホノメチル)グリシン、イミノジメチレンホスホン酸およびエチレンジアミンテトラ(メチレンホスホン酸)またはこれらの塩からなる群から選択される少なくとも一つを含む請求項1に記載の研磨組成物。
- 前記Co錯化剤は、クエン酸、クエン酸塩、エチレンジアミン四酢酸(EDTA)、2―ヒドロキシホスホノ酢酸(HPAA)、ホスホノブタン―3カルボン酸(PBTC)およびアミノトリ(メチレンホスホン酸)(ATMP)の少なくとも一つを含む請求項1に記載の研磨組成物。
- 前記Co錯化剤がクエン酸、クエン酸塩、およびエチレンジアミン四酢酸(EDTA)から選ばれる一つ以上である請求項8に記載の研磨組成物。
- Co研磨促進剤としてアンモニアおよび重炭酸塩の一つ以上をさらに含む請求項1に記載の研磨組成物。
- 前記Co錯化剤は、質量%で、前記研磨組成物中5%以下存在する請求項1に記載の研磨組成物。
- 前記砥粒がシリカ、アルミナまたはセリアである請求項1に記載の研磨組成物。
- 酸化剤、界面活性剤および腐食抑制剤の一つ以上を更に含む請求項1の研磨組成物。
- 前記酸化剤は、質量%で、前記研磨組成物中0.1~4%存在する請求項13に記載の研磨組成物。
- 前記酸化剤がH2O2である請求項13に記載の研磨組成物。
- 前記腐食抑制剤は、質量%で、前記研磨組成物中0.1~0.4%存在する請求項13の研磨組成物。
- 腐食抑制剤がベンゾトリアゾール(BTA)である請求項13に記載の研磨組成物。
- 前記界面活性剤は、質量%で、前記研磨組成物中0.01~2%存在する請求項13に記載の研磨組成物。
- 前記界面活性剤が下記の式(II)の化合物を含み、下記式(II)において、オキシエチレンおよびオキシプロピレン基が1:1~3:1の質量比で存在するように、mおよびnが選択される請求項13に記載の研磨組成物。
R1―O―[CH2CH(CH3)O]m―[CH2CH2O]n―H
(II) - 請求項1~19のいずれかに記載の研磨組成物でCoを研磨し、任意にCuを研磨することを有する研磨方法。
- Coの除去速度が200Å/分~2400Å/分である請求項20に記載の方法。
- Cuの除去率が100Å/分未満または80Å/分未満である請求項21に記載の方法。
- CoのCuに対する除去選択性が、5以上である請求項22に記載の方法。
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JP2020164816A (ja) * | 2019-03-29 | 2020-10-08 | 株式会社フジミインコーポレーテッド | Cmp組成物およびこれを用いた方法 |
JP7409917B2 (ja) | 2019-03-29 | 2024-01-09 | 株式会社フジミインコーポレーテッド | Cmp組成物およびこれを用いた方法 |
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TWI650409B (zh) | 2019-02-11 |
JP6093846B2 (ja) | 2017-03-08 |
JPWO2014132641A1 (ja) | 2017-02-02 |
CN105144354A (zh) | 2015-12-09 |
US20140243250A1 (en) | 2014-08-28 |
US9576818B2 (en) | 2017-02-21 |
TW201437349A (zh) | 2014-10-01 |
CN105144354B (zh) | 2017-12-01 |
KR20150125930A (ko) | 2015-11-10 |
DE112014001038T5 (de) | 2015-11-26 |
KR102160024B1 (ko) | 2020-09-25 |
SG11201506102TA (en) | 2015-09-29 |
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