CN102585706B - Acidic chemical and mechanical polishing composition - Google Patents
Acidic chemical and mechanical polishing composition Download PDFInfo
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- CN102585706B CN102585706B CN2012100048016A CN201210004801A CN102585706B CN 102585706 B CN102585706 B CN 102585706B CN 2012100048016 A CN2012100048016 A CN 2012100048016A CN 201210004801 A CN201210004801 A CN 201210004801A CN 102585706 B CN102585706 B CN 102585706B
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- Prior art keywords
- mechanical polishing
- polishing composition
- polishing
- acidic chemical
- modification
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- 238000005498 polishing Methods 0.000 title claims abstract description 108
- 239000000203 mixture Substances 0.000 title claims abstract description 58
- 239000000126 substance Substances 0.000 title claims abstract description 25
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 91
- 230000004048 modification Effects 0.000 claims abstract description 40
- 238000012986 modification Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000003082 abrasive agent Substances 0.000 claims abstract description 11
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- 239000008119 colloidal silica Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims abstract description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 43
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 28
- 229920001515 polyalkylene glycol Polymers 0.000 claims description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- 238000002242 deionisation method Methods 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000012964 benzotriazole Substances 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 17
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003957 anion exchange resin Substances 0.000 claims description 15
- 239000003729 cation exchange resin Substances 0.000 claims description 15
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical group NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 238000004581 coalescence Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003002 pH adjusting agent Substances 0.000 claims description 6
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
- 150000007530 organic bases Chemical class 0.000 claims description 5
- 229960004418 trolamine Drugs 0.000 claims description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 235000005985 organic acids Nutrition 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 150000007522 mineralic acids Chemical group 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 150000003440 styrenes Chemical class 0.000 claims description 2
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims 1
- 239000007800 oxidant agent Substances 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 14
- 239000002002 slurry Substances 0.000 abstract description 9
- 230000009471 action Effects 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 4
- 230000003746 surface roughness Effects 0.000 abstract description 3
- 239000003112 inhibitor Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 42
- 239000010949 copper Substances 0.000 description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 24
- 229910052802 copper Inorganic materials 0.000 description 23
- 238000007670 refining Methods 0.000 description 19
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 16
- 229960001866 silicon dioxide Drugs 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003643 water by type Substances 0.000 description 14
- 239000004471 Glycine Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- -1 peroxy compound Chemical class 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 2
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 description 2
- 229940043276 diisopropanolamine Drugs 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- CCVYRRGZDBSHFU-UHFFFAOYSA-N (2-hydroxyphenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC=C1O CCVYRRGZDBSHFU-UHFFFAOYSA-N 0.000 description 1
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 1
- MXZROAOUCUVNHX-UHFFFAOYSA-N 2-Aminopropanol Chemical compound CCC(N)O MXZROAOUCUVNHX-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 description 1
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 1
- NNIVFXCKHNRSRL-VKHMYHEASA-N Hydroxyglutamic acid Chemical compound ON[C@H](C(O)=O)CCC(O)=O NNIVFXCKHNRSRL-VKHMYHEASA-N 0.000 description 1
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 description 1
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- YIKSCQDJHCMVMK-UHFFFAOYSA-N Oxamide Chemical compound NC(=O)C(N)=O YIKSCQDJHCMVMK-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Inorganic materials [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- HCPOCMMGKBZWSJ-UHFFFAOYSA-N ethyl 3-hydrazinyl-3-oxopropanoate Chemical compound CCOC(=O)CC(=O)NN HCPOCMMGKBZWSJ-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229960002989 glutamic acid Drugs 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007521 mechanical polishing technique Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 150000003053 piperidines Chemical class 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 229940093916 potassium phosphate Drugs 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical compound CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- XYJRNCYWTVGEEG-UHFFFAOYSA-N trimethoxy(2-methylpropyl)silane Chemical compound CO[Si](OC)(OC)CC(C)C XYJRNCYWTVGEEG-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention provides an acidic chemical and mechanical polishing composition. The pH value of the acidic chemical and mechanical polishing composition is 2-7, and the acidic chemical and mechanical polishing composition comprises 1-20% by weight of abrasive material, 0.5-10% by weight of oxidant, 0.1-10% by weight of complexing agent, 0.001-1% by weight of corrosion inhibitor, 0.001-5% by weight of organic film-forming auxiliaries and the balance of pH regulator and deionized or distilled water, wherein the abrasive material is of colloidal silica sol after modification in the special step, and the average particle size is of 10-200nm. According to the chemical and mechanical polishing composition provided by the invention, the abrasive material is refined and modified; by using the method, the stability of the abrasive material in polishing slurry can be effectively upgraded, and polishing removal rate and surface roughness degree are respectively optimized to a certain extent; and the unique adding effect of the organic film-forming auxiliaries can well balance the strength of chemical corrosion action and the strength of mechanical grinding action, and achieve the effects of improving polishing removal efficiency and performing global planarization.
Description
Technical field
The present invention relates to the chemical-mechanical polishing compositions field, especially relate to the acidic chemical mechanical polishing composition.
Background technology
Integrated circuit (IC) chip by on silicon substrate or millions of activation elements that form in silicon substrate form, the method interconnection of these activation elements disconnected from each other by metal line forms functional circuit and parts., because Cu has low resistivity and high electromigration resisting property, make it become a kind of desirable intraconnections material and replace tradition aluminium wiring commonly used.Cu is metal after hydrogen, is difficult for being etched, and therefore generally adopts in the world at present inlay to connect up, and by chemical Mechanical Polishing Technique, removes the unnecessary copper in upper strata and diffusion impervious layer.Along with the development of microelectronics, characteristic dimension has entered nano level, and nearly hundred procedures that this requires in microelectronic technique, must carry out leveling.Traditional planarization technique can only provide part plan, and smooth effect is extremely limited.Chemically machinery polished (CMP) technology for planarization, has brought ic manufacturing technology to change greatly.
CMP is the polishing technology that the mechanical effect of particle combines with the chemical action of etching reagent, its principle is that workpiece rotates with respect to polishing pad under the existence of pressure and polishing composition (containing abrasive particle, etching reagent etc.), thereby utilizes abrasive particle grinding and chemical composition corrosive nature to realize the removal of workpiece surface material is reached the effect of planarization.The performance of CMP is determined by the operational condition of CMP device, the type of polishing composition and the factors such as type of polishing pad.
Polishing composition is a kind of important influence factor in the CMP step.Can regulate polishing composition according to the oxygenant of choosing, abrasive material and other additive that is fit to, with the polishing speed by required, provide effective polishing, simultaneously surface imperfection, corrosion are down to minimumly, and obtain best complanation effect.In recent years, more existing patent reports the polishing composition that uses in integrated circuit multilayer copper wiring CMP process, for example CN101240147A, CN1256765C, CN100491072C, CN101333419A, CN101368068A.
Along with integrated circuit technique enters into deep-submicron, the interconnection performance of being brought by continuous down feature sizes reduces more and more obvious.Adopting medium with low dielectric constant material (being low k dielectric materials) is one of effective way that improves the interconnection performance.But when k＜2.2, the physical strength of low k dielectric layer descends, and is prone to low k film delamination, so must exploitation low pressure polissoir and polishing composition.
Generally, reducing overdraft can have a negative impact to the CMP overall performance that comprises polishing speed, has a strong impact on throughput.There have been some patents to propose the low downforce pressure polishing composition, for example CN201110065350.2, US6,620,037, CN1644644A, but research in this respect still need be strengthened.The development of semicon industry is to can still existing demand by the improvement polishing waterborne compositions of copper on polishing of semiconductor wafers under 0.5Psi (3.45kPa) and above polish pressure condition, particularly below 2.0Psi, as effective polish copper interconnection layer under 0.5Psi pressure, thereby adapt to the dielectric introducing of low-k and development.
Summary of the invention
The present invention is intended to solve at least one of technical problem that exists in prior art.
The invention provides a kind of acidic chemical mechanical polishing composition, its pH value is 2-7, and its composition comprises abrasive material 1-20wt%, oxygenant 0.5-10wt%, complexing agent 0.1-10wt%, inhibiter 0.001-1wt%, organic film coalescence aid 0.001-5wt%, pH adjusting agent and deionized water or distilled water.wherein abrasive material is the colloidal silica sol of modification, mean particle size is the 10-200 nanometer, its preparation method is as follows: (1) deionization: the strong acid type styrene type cation exchange resin post of having regenerated and strong base styrene series anion exchange resin post are washed till with deionized water to flow out water pH value be neutrality, again raw silicon colloidal sol is flow through successively cation exchange resin column and anion-exchange resin column through having regenerated, flow rate control is at 1-10 m/h, namely obtain the silicon dioxide gel of deionization, adopt organic bases to regulate the pH value to 9.0-10.0, to extend its stable storage period, (2) modification: after described deionization silicon dioxide gel is heated to 50-60 ℃, under agitation slowly splash into organosilicon liquid, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% water silica sol solution.
Chemical-mechanical polishing compositions provided by the invention, its abrasive material have carried out refining and modification, and this method can effectively promote the stability of abrasive material in polishing slurries.
One of according to the embodiment of the present invention, in above-mentioned deionization step, organic bases is thanomin (MEA), Tetramethylammonium hydroxide (TMAH), trolamine.
According to another embodiment of the present invention, in above-mentioned modification step, organosilicon liquid is selected from the group that comprises methyltrimethoxy silane, dimethyldimethoxysil,ne, octyl group Trimethoxy silane, isobutyl-Trimethoxy silane, dodecyltrimethoxysilane, gamma-methyl allyl acyloxypropyl trimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane and the composition of their arbitrary proportions.
Preferably, organosilicon liquid is gamma-methyl allyl acyloxypropyl trimethoxysilane, and its add-on is 0.01-10wt%.More preferably, the add-on of gamma-methyl allyl acyloxypropyl trimethoxysilane is 0.1-1wt%.
One of according to the embodiment of the present invention, the content of colloidal silica sol described in chemical-mechanical polishing compositions is 3-5wt%, mean particle size is the 50-80 nanometer.
One of according to the embodiment of the present invention, oxygenant described in chemical-mechanical polishing compositions is inorganic or the organic peroxy compound, be to contain at least one peroxy-radical in molecule (compound O-O-) and contain the compound of the element that is in high oxidation state, include but not limited to hydrogen peroxide, Urea Peroxide, two persulphates, Peracetic Acid, benzoyl peroxide, di-t-butyl peroxide, sodium peroxide etc.; The high oxidation state compound comprises Periodic acid, periodate, hyperbromic acid, hyperbromic acid salt, perchloric acid, perchlorate, periodic acid, periodates, peroxyboric acid, perborate, iodate, bromate, oxymuriate, hypochlorite, nitrite, chromic salt, molysite and permanganate.Preferably, oxygenant is hydrogen peroxide, and its content is 0.9-3wt%.
In acidic chemical mechanical polishing composition provided by the invention, complexing agent refers to and can promote polishing composition to metal, copper for example, oxygenizement, increase Ammonia or the carboxylic class organic acids and base of polishing speed.One of according to the embodiment of the present invention, complexing agent described in chemical-mechanical polishing compositions is selected from the group that comprises Padil, L-Ala, L-glutamic acid, proline(Pro), hydroxyglutamic acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, Amino Trimethylene Phosphonic Acid, 2-HPAA, acetic acid, oxalic acid, citric acid, oxamide and the composition of their arbitrary proportions.Preferably, complexing agent is Padil, and its content is 0.5-3wt%.
In acidic chemical mechanical polishing composition provided by the invention, inhibiter refers to any compound or its mixture that helps to form on the surface of special metal layer such as Cu dense oxide passivation layer and dissolution inhibition layer.One of according to the embodiment of the present invention, inhibiter described in chemical-mechanical polishing compositions is selected from the group that comprises benzotriazole, benzoglyoxaline, imidazoles, benzothiazole, urea, thiocarbamide, ethylene thiourea and the composition of their arbitrary proportions.Preferably, inhibiter preferably contains the heterocyclic organic compounds of one or more 5 or 6 yuan of heterocycles as active function groups, and as benzotriazole or benzoglyoxaline or their mixture, content is 0.001-0.05wt%.
In acidic chemical mechanical polishing composition provided by the invention, organic film coalescence aid refers to can possess in the surperficial formation advantage absorption of metal level (as the Cu layer), institute's film forming the polymer organic polymer of outstanding oilness and wettability.One of according to the embodiment of the present invention, organic film coalescence aid described in chemical-mechanical polishing compositions is selected from the group that comprises polyvinyl alcohol, polyoxyethylene glycol, polyalkylene glycol, polyacrylic acid, polyacrylamide, fatty alcohol-polyoxyethylene ether, polyoxyethylenated alcohol sodium sulfate and the composition of their arbitrary proportions.Preferably, organic film coalescence aid is polyalkylene glycol, and its content is 0.01-1wt%.The organic film coalescence aid of polymer that the present invention adopts can effectively promote the polish removal rate of material.
in chemical-mechanical polishing compositions provided by the invention, pH adjusting agent can be any known acid, a kind of or the composition of alkali or amine and salt thereof, include but not limited to sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, Mono Chloro Acetic Acid, propanedioic acid, sodium hydroxide, potassium hydroxide, ammoniacal liquor, thanomin, diethanolamine, trolamine, α-amino isopropyl alcohol, aminopropanol, diisopropanolamine (DIPA), quadrol, tetramethylphosphonihydroxide hydroxide base amine, hydroxide tetraethyl-amine, hydroxide tetrapropyl amine, choline, piperidines, piperazine, the polyethylene imines, sodium carbonate, salt of wormwood, sodium phosphate, potassiumphosphate, Sodium phosphate dibasic, the mixture of a kind of or its arbitrary proportion in ammonium hydrogen phosphate etc.One of according to the embodiment of the present invention, pH adjusting agent is inorganic or organic acids and base, and preferably, pH adjusting agent is selected from the group that comprises sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, potassium hydroxide, ammoniacal liquor, thanomin, trolamine and the composition of their arbitrary proportions.
One of according to the embodiment of the present invention, acidic chemical mechanical polishing composition provided by the invention, its pH value is preferably 3-5.
Polishing mechanism and the advantage of the inventive method are as follows:
1, polish abrasive colloid silica used in the present invention has carried out before use that deionization is refining and surface silicon is siloxane modified, this measure can effectively promote the stability of abrasive particle in polishing slurries, make the total composition liquid of polishing slurries still keep excellent polishing effect after placing 7 days, polish removal rate and surfaceness all have optimization to a certain degree.
2. this polishing composition is acid partial neutral, and the pH value between 3-5, keeps nanometer silicon dioxide particle stability and dispersed the time, and the stability of oxidants hydrogen peroxide has also been given guarantee, and less to the corrodibility of equipment.
3. preferred organic film coalescence aid polyalkylene glycol used in the present invention (PAG) can form the self assembly molecule rete with oilness and wettability in the metallic surface of oxidation.In the situation that low downforce pressure polishing, residing polishing environment common mechanical action intensity far is weaker than chemical action intensity, and the molecule rete on this metal oxide top layer can effectively be protected polished depression in the surface zone, and the highly selective of pattern is provided; And when polish pressure increased, the polymer molecule rete was not enough to resist the mechanical grinding effect of increase, and the disengaging of rete drives the disengaging of metal oxide rete, can effectively increase polish removal rate.Can think, the good balance of additive effect that above organic film coalescence aid polyalkylene glycol is exclusive chemical corrosion action intensity and mechanical grinding action intensity, improve polishing and remove the effect of efficiency and overall planarization thereby reach.
4. be low to moderate in the overdraft situation of 0.5～7.0Psi, under experiment condition, the polish removal rate of optimum combination composition formula reaches as high as 1738.0nm/min, and surfaceness is minimum can be to 0.599nm, and polish removal rate is high, surface finish is good, and the shelf-stability of total composition liquid is good.Can be used for the polishing of multilayer copper wire in large scale integrated circuit copper.
The aspect that the present invention adds and advantage part in the following description provide, and part will become obviously from the following description, or by practice of the present invention, recognize.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage will become from the following description of the accompanying drawings of embodiments and obviously and easily understand, wherein:
Fig. 1 is the polishing clearance of the embodiment of the present invention 1～6 and the rule schematic diagram of pressure dependence;
Fig. 2 is the surfaceness of the embodiment of the present invention 1～6 and the rule schematic diagram of pressure dependence;
Fig. 3 is the surface of polished pattern observation figure of the embodiment of the present invention 9.
Embodiment
Below describe embodiments of the invention in detail, the example of described embodiment is shown in the drawings.Be exemplary below by the embodiment that is described with reference to the drawings, only be used for explaining the present invention, and can not be interpreted as limitation of the present invention.
In embodiment, experiment all uses CETR CP4 to be the polishing experiments machine, use the IC1000/SUBA IV of Rodel company microvoid polyurethane polishing pad, the polishing speed of relative movement is fixed as 1m/s, the polishing fluid flow is 100mL/min, and polished is 2 cun electroplating surface copper sheets.It is the precise electronic balance check weighing calculating of 0.01mg that polish removal rate (MRR) adopts precision, uses the three-dimensional white light interference surface topographic apparatus fo of the microXAM of Veeco company to observe surface topography and gauging surface roughness (Sa).
Embodiment 1
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 0.5Psi overdraft, polish removal rate MRR is 421.0nm/min, surfaceness Sa is 4.01nm.
Embodiment 2
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 1.0Psi overdraft, polish removal rate MRR is 569.4nm/min, surfaceness Sa is 3.02nm.
Embodiment 3
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 2.0Psi overdraft, polish removal rate MRR is 692.5nm/min, surfaceness Sa is 1.39nm.
Embodiment 4
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 3.0Psi overdraft, polish removal rate MRR is 857.4nm/min, surfaceness Sa is 1.14nm.
Embodiment 5
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 4.0Psi overdraft, polish removal rate MRR is 897.0nm/min, surfaceness Sa is 0.965nm.
Embodiment 6
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 5.0Psi overdraft, polish removal rate MRR is 991.6nm/min, surfaceness Sa is 0.833nm.
Embodiment 7
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 7.0Psi overdraft, polish removal rate MRR is 1597.6nm/min, surfaceness Sa is 0.835nm.
Embodiment 8
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water and supply 1000 grams and stir.Place after 3 days and carry out the copper polishing of 7.0Psi overdraft, polish removal rate MRR is 1643.9nm/min, and surfaceness Sa is 0.668nm.
Embodiment 9
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water and supply 1000 grams and stir.Place after 7 days and carry out the copper polishing of 7.0Psi overdraft, polish removal rate MRR is 1738.0nm/min, and surfaceness Sa is 0.599nm.
Comparative experimental example 1 silicon-dioxide is made with extra care and the impact of modification on polishing effect
1. divide into groups and treatment process:
Experimental group 1-3, adopt respectively the chemical-mechanical polishing compositions of embodiment 7-9.
Comparative group 1-3, adopt respectively following methods to prepare chemical-mechanical polishing compositions and polished finish.
Comparative group 1
10 gram glycine, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir the 50nm silica hydrosol of the not refining and modification that adds 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 7.0Psi overdraft.
Comparative group 2
10 gram glycine, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir the 50nm silica hydrosol of the not refining and modification that adds 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add finally water and supply 1000 grams and stir.Place after 3 days and carry out the copper polishing of 7.0Psi overdraft.
Comparative group 3
10 gram glycine, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir the 50nm silica hydrosol of the not refining and modification that adds 100 grams 30%, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add finally water and supply 1000 grams and stir.Place after 7 days and carry out the copper polishing of 7.0Psi overdraft.
2. result and analysis:
Detailed results is in Table 1.
Table 1 abrasive particle is made with extra care and the impact of modification front and back on the polishing slurries shelf-stability
| Test | The abrasive particle disposition | Storage period (my god) | Overdraft (Psi) | MRR(nm/min) | Sa(nm) |
| Comparative group 1 | Be untreated | 0 | 7.0 | 1457.7 | 1.12 |
| Comparative group 2 | Be untreated | 3 | 7.0 | 1171.8 | 2.10 |
| Comparative group 3 | Be untreated | 7 | 7.0 | 1066.0 | 3.29 |
| Experimental group 1 | Make with extra care and modification | 0 | 7.0 | 1597.6 | 0.835 |
| Experimental group 2 | Make with extra care and modification | 3 | 7.0 | 1643.9 | 0.668 |
| Experimental group 3 | Make with extra care and modification | 7 | 7.0 | 1738.0 | 0.599 |
As shown in table 1, abrasive particle is without the increase with storage period of the polishing slurries of refining and modification, the MRR continuous decrease, and the glazed surface quality also significantly worsens.And use through refining and abrasive particle modification, increase with storage period, the polishing performance of polishing slurries has optimization to a certain degree on the contrary, can find out from the surface of polished pattern schematic diagram of Fig. 3, with the copper sheet that the polishing slurries polishing of placing 7 days goes out, surface roughness has been low to moderate 0.599nm.
As can be seen from the above embodiments, the polishing composition that process is optimized provides beyond thought effect of optimization to polishing speed and the glazed surface quality of copper-connection, has also effectively promoted the shelf-stability of polishing slurries.
The impact of the interpolation of comparative experimental example 2 organic membrane-forming agents on polishing effect
1. divide into groups and treatment process:
Experimental group 1-6, adopt respectively the chemical-mechanical polishing compositions of embodiment 1-6.
Comparative group 1-2, adopt respectively following methods to prepare chemical-mechanical polishing compositions and polished finish.
Comparative group 1:
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram glycine and 0.1 gram benzotriazole are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 0.5Psi overdraft.
Comparative group 2
Raw silicon colloidal sol is flow through cation exchange resin column and anion-exchange resin column through having regenerated with flow velocity 1-10 m/h successively, obtain the silicon dioxide gel of deionization, after adopting Tetramethylammonium hydroxide to regulate pH value to 10.0, be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% 50nm silica hydrosol.
10 gram glycine and 0.1 gram benzotriazole are added in 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add the silica hydrosol of 100 grams through refining and modification.
Add the oxidants hydrogen peroxide solution of 100 grams 30% before polishing is carried out, use H
2SO
4Calibration pH value to 4.0, add finally water supply 1000 grams and stir after carry out immediately the copper polishing of 5.0Psi overdraft.
2. result and analysis:
Detailed results is in Table 2.
Table 2 polyalkylene glycol (PAG) add impact on polishing effect
| Test | The abrasive particle disposition | PAG(％) | Overdraft (Psi) | MRR(nm/min) | Sa(nm) |
| Comparative group 1 | Make with extra care and modification | 0 | 0.5 | 390.6 | 4.33 |
| Comparative group 2 | Make with extra care and modification | 0 | 5.0 | 842.7 | 1.26 |
| Experimental group 1 | Make with extra care and modification | 0.01 | 0.5 | 421.0 | 4.01 |
| Experimental group 2 | Make with extra care and modification | 0.01 | 1.0 | 569.4 | 3.02 |
| Experimental group 3 | Make with extra care and modification | 0.01 | 2.0 | 692.5 | 1.39 |
| Experimental group 4 | Make with extra care and modification | 0.01 | 3.0 | 857.4 | 1.14 |
| Experimental group 5 | Make with extra care and modification | 0.01 | 4.0 | 897.0 | 0.965 |
| Experimental group 6 | Make with extra care and modification | 0.01 | 5.0 | 991.6 | 0.833 |
As shown in table 2, no matter be in low pressure or the situation of high pressure, the interpolation of organic film coalescence aid polyalkylene glycol (PAG) can improve polish removal rate and the optimizing surface quality of copper.Can find out from Fig. 1-2, in the situation that PAG content is fixing, with the increase of polish pressure, MRR presents power exponent and increases progressively, and just breaks through rapidly 600nm/min after polish pressure 1.0Psi; Sa presents power exponent with the increase of polish pressure and successively decreases, and starts lower than 1.0nm after 4.0Psi.
Can find out from above-mentioned contrast experiment, acidic chemical mechanical polishing composition of the present invention and preparation method thereof utilizes the refining and modification of raw silicon colloidal sol, and add organic film coalescence aid that can promote polishing effect, can effectively promote polishing speed and the surface quality of the polishing of wafer copper-connection in wider pressure range, avoid to greatest extent the generation of polishing defect.Specifically, under the polishing experiments condition of embodiment, in the overdraft scope of 0.5～7.0Psi, the polish removal rate of optimum combination composition formula reaches as high as 1738.0nm/min, and surfaceness can reach 0.599nm.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (6)
1. acidic chemical mechanical polishing composition, its pH value is 2-7, its composition comprises
Abrasive material 1-20wt%, oxygenant 0.9-3wt%, complexing agent 0.5-3wt%, inhibiter 0.001-0.05wt%, organic film coalescence aid 0.01-1wt%, pH adjusting agent and deionized water or distilled water, wherein
Described oxygenant is hydrogen peroxide,
Described complexing agent is Padil,
Described inhibiter is benzotriazole,
Described organic film coalescence aid is polyalkylene glycol,
Described abrasive material is the colloidal silica sol of modification, and mean particle size is 10-200 nanometers, and its preparation method is as follows:
(1) deionization: the strong acid type styrene type cation exchange resin post of having regenerated and strong base styrene series anion exchange resin post are washed till with deionized water to flow out water pH value be neutrality, again raw silicon colloidal sol is flow through successively cation exchange resin column and anion-exchange resin column through having regenerated, flow rate control is at 1-10 m/hs, namely obtain the silicon dioxide gel of deionization, adopt organic bases to regulate pH value to 9.0-10.0;
(2) modification: after described deionization silicon dioxide gel is heated to 50-60 ℃, under agitation slowly splash into organosilicon liquid, insulated and stirred is diluted with water to effective solid content after 6 hours be 30% water silica sol solution,
Described organosilicon liquid is gamma-methyl allyl acyloxypropyl trimethoxysilane, and its add-on is 0.01-10wt%.
2. acidic chemical mechanical polishing composition as claimed in claim 1, wherein said organic bases is thanomin, Tetramethylammonium hydroxide, trolamine.
3. acidic chemical mechanical polishing composition as claimed in claim 1, the add-on of wherein said gamma-methyl allyl acyloxypropyl trimethoxysilane is 0.1-1wt%.
4. acidic chemical mechanical polishing composition as claimed in claim 1, the content of the colloidal silica sol of wherein said modification is 3-5wt%, mean particle size is 50-80 nanometers.
5. acidic chemical mechanical polishing composition as claimed in claim 1, wherein said pH adjusting agent is inorganic or organic acids and base, is selected from least a of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, potassium hydroxide, ammoniacal liquor, thanomin and trolamine.
6. acidic chemical mechanical polishing composition as claimed in claim 1, its pH value is 3-5.
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