JP4888913B2 - マイクロ電子機器における銅電気沈積方法 - Google Patents
マイクロ電子機器における銅電気沈積方法 Download PDFInfo
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- JP4888913B2 JP4888913B2 JP2007541369A JP2007541369A JP4888913B2 JP 4888913 B2 JP4888913 B2 JP 4888913B2 JP 2007541369 A JP2007541369 A JP 2007541369A JP 2007541369 A JP2007541369 A JP 2007541369A JP 4888913 B2 JP4888913 B2 JP 4888913B2
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- 239000010949 copper Substances 0.000 title claims description 172
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 35
- 229910052802 copper Inorganic materials 0.000 title claims description 35
- 238000000151 deposition Methods 0.000 title claims description 28
- 238000004377 microelectronic Methods 0.000 title description 3
- 239000003112 inhibitor Substances 0.000 claims description 92
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 84
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 67
- 238000007747 plating Methods 0.000 claims description 47
- 238000009713 electroplating Methods 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 43
- 150000001875 compounds Chemical class 0.000 claims description 38
- 229920000570 polyether Polymers 0.000 claims description 38
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 33
- 239000000758 substrate Substances 0.000 claims description 31
- 229920001400 block copolymer Polymers 0.000 claims description 28
- 230000008021 deposition Effects 0.000 claims description 24
- 239000004065 semiconductor Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 19
- 238000005868 electrolysis reaction Methods 0.000 claims description 18
- 125000000217 alkyl group Chemical group 0.000 claims description 15
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 11
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 10
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 10
- 150000001412 amines Chemical group 0.000 claims description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 8
- 125000003118 aryl group Chemical group 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 125000003277 amino group Chemical group 0.000 claims description 4
- 125000005842 heteroatom Chemical group 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 4
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 3
- 150000004985 diamines Chemical class 0.000 claims description 2
- 150000002898 organic sulfur compounds Chemical class 0.000 claims 2
- 239000002253 acid Substances 0.000 description 43
- 239000000654 additive Substances 0.000 description 26
- 125000002091 cationic group Chemical group 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 21
- 238000012360 testing method Methods 0.000 description 18
- -1 amine salts Chemical class 0.000 description 15
- 230000007547 defect Effects 0.000 description 15
- 239000000243 solution Substances 0.000 description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- 229920002359 Tetronic® Polymers 0.000 description 11
- 239000008151 electrolyte solution Substances 0.000 description 11
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 11
- 125000004433 nitrogen atom Chemical group N* 0.000 description 11
- 239000003792 electrolyte Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 238000005240 physical vapour deposition Methods 0.000 description 7
- 230000000996 additive effect Effects 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 125000004430 oxygen atom Chemical group O* 0.000 description 6
- 235000012431 wafers Nutrition 0.000 description 6
- 150000008064 anhydrides Chemical class 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 150000003973 alkyl amines Chemical class 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000012733 comparative method Methods 0.000 description 3
- CGPVLUCOFNAVGV-UHFFFAOYSA-N copper;pentahydrate Chemical compound O.O.O.O.O.[Cu] CGPVLUCOFNAVGV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009499 grossing Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
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- 230000002829 reductive effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 208000012868 Overgrowth Diseases 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N anhydrous diethylene glycol Natural products OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 150000004982 aromatic amines Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- NISGSNTVMOOSJQ-UHFFFAOYSA-N cyclopentanamine Chemical class NC1CCCC1 NISGSNTVMOOSJQ-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
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- 238000001465 metallisation Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 150000002924 oxiranes Chemical class 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000005077 polysulfide Chemical class 0.000 description 2
- 229920001021 polysulfide Chemical class 0.000 description 2
- 150000008117 polysulfides Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- 150000003335 secondary amines Chemical class 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 1
- FPYGTMVTDDBHRP-OWOJBTEDSA-N (e)-but-2-ene-1,4-diamine Chemical compound NC\C=C\CN FPYGTMVTDDBHRP-OWOJBTEDSA-N 0.000 description 1
- KFDVPJUYSDEJTH-UHFFFAOYSA-N 4-ethenylpyridine Chemical compound C=CC1=CC=NC=C1 KFDVPJUYSDEJTH-UHFFFAOYSA-N 0.000 description 1
- 125000001054 5 membered carbocyclic group Chemical group 0.000 description 1
- 125000004008 6 membered carbocyclic group Chemical group 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- KSSJBGNOJJETTC-UHFFFAOYSA-N COC1=C(C=CC=C1)N(C1=CC=2C3(C4=CC(=CC=C4C=2C=C1)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC(=CC=C1C=1C=CC(=CC=13)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC=C(C=C1)OC Chemical compound COC1=C(C=CC=C1)N(C1=CC=2C3(C4=CC(=CC=C4C=2C=C1)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC(=CC=C1C=1C=CC(=CC=13)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)N(C1=CC=C(C=C1)OC)C1=C(C=CC=C1)OC)C1=CC=C(C=C1)OC KSSJBGNOJJETTC-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 229920005682 EO-PO block copolymer Polymers 0.000 description 1
- 240000007817 Olea europaea Species 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 239000005700 Putrescine Substances 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 229940073608 benzyl chloride Drugs 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
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- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- WIYCQLLGDNXIBA-UHFFFAOYSA-L disodium;3-(3-sulfonatopropyldisulfanyl)propane-1-sulfonate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)CCCSSCCCS([O-])(=O)=O WIYCQLLGDNXIBA-UHFFFAOYSA-L 0.000 description 1
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- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-N methyl sulfate Chemical compound COS(O)(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 150000003141 primary amines Chemical class 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical group CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
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- 229910052711 selenium Inorganic materials 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
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- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229920000428 triblock copolymer Polymers 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Classifications
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- 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
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
- H01L21/2885—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition using an external electrical current, i.e. electro-deposition
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
- C25D7/123—Semiconductors first coated with a seed layer or a conductive layer
-
- 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
- H01L21/34—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 not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
- H01L21/44—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/38 - H01L21/428
-
- 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
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76877—Filling of holes, grooves or trenches, e.g. vias, with conductive material
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
- Electrodes Of Semiconductors (AREA)
Description
発明の分野
本発明はマイクロ電子機器の分野における電気分解的Cu金属化のための方法、組成物及び添加剤に関する。
電気分解によるCu金属化の方法は、マイクロ電子機器製造の分野に利用されて、例えば、半導体集積回路(IC)基板の製造などのような幅広い応用における電子内部配線回路を製造する。コンピュータチップのような半導体IC基板を高い配線速度と高い充填密度でもって製造するという要求は超大規模回路(ULSI)や超々大規模回路(VLSI)構造の配線の小径化となる。小径化と高密度化の傾向は内部配線の径をより減少化させる。内部配線の凹凸は、誘電体基板に作成されたビアやトレンチなどの凹凸であり、それらは次いで金属で充填されて、電気導電性の内部配線回路となる。さらに内部配線の減少化は金属充填を問題としている。
半導体集積回路基板を電解溶液に浸漬して平面性メッキ表面とサブミクロン径の内部配線凹凸を有する半導体集積回路基板上に電気分解メッキをするための電気メッキ組成物を本発明は指向する。この組成物は、電気分解的にCuを基板上に、そして電子内部配線凹凸内へ沈積させるのに十分な量のCuイオン供給源と、プロピレンオキサイド(PO)繰り返し単位とエチレンオキサイド(EO)繰り返し単位の組み合わせで、PO:EO比が約1:9と約9:1の間にあり、含窒素種に結合しているものからなる抑制剤化合物からなり、ここで、抑制剤化合物の分子量は約1000と約30,000の間にあるものである。
図1は、本発明の抑制剤化合物からなる電解メッキ浴の充填速度(―■―)と市販の抑制剤化合物からなる電解メッキ浴の充填速度(―●―)とを比較したグラフである。本発明の抑制剤を含む電気分解メッキ浴は実施例1に列挙される浴成分を含み、実施例7の方法に従いメッキされた。市販抑制剤からなる電気分解メッキ浴は比較例1に列挙の浴成分を含み、実施例7の方法に従いメッキされた。
本発明に従い困難な充填特性を有する半導体集積回路基板をメッキするに適した組成物が提供され、その特性は不十分に種付けされたまたは実質的に種付けされていない内部配線凹凸、複雑な配置の内部配線凹凸、および大径の内部配線凹凸、ならびに小径の内部配線凹凸(約0.5μm未満)、および高アスペクト比の凹凸(少なくとも約3:1)または低アスペクト比の凹凸(約3:1未満)であり、ここでCuは全ての凹凸へ完全に実質的に欠陥なく充填しなければならない。
ここで、R1は置換または無置換のアルキル基であり、好ましくは炭素数1と8の間の直鎖または分枝アルキル基であり、好ましくは、R1はポリエーテル基が共有結合する他のアミノ基で置換しており、ポリエーテル基はEO繰り返し単位、PO繰り返し単位及びその組み合わせからなり、その配列はランダム、交互またはブロック配列であり、
R2は、水素原子及びアルキル基からなる群から選択され、ここでR2がアルキル基の場合、好ましくはメチル基であり、
R3は、好ましくはEO繰り返し単位、PO繰り返し単位及びその組み合わせからなるポリエーテル基であり、その配列はランダム、交互またはブロック配列であり、そして
R4は、水素原子、置換または無置換アルキル基、アリール基、アラルキル基または複素原子含有アリール基からなる群から選択される。
そしてここでnは1と約30の間にあり、そしてmは1と約30に間にある。それゆえ、構造(5)を有する抑制剤化合物は4個のPO/EOブロック共重合体として合計で約4と約120個の間のPO繰り返し単位と合計で約4と約120個の間のEO繰り返し単位を有する。単一のPO/EOブロック共重合体上のPO(疎水性)ブロックの分子量は約50g/molと約1800g/molに間にあり、単一のPO/EOブロック共重合体上のEO(親水性)ブロックの分子量は約40g/molと約1400g/molの間にある。単一のPO/EOブロック共重合体の分子量は約100g/molと約3600g/molの間にあることができる。構造(5)を有する例示の抑制剤化合物は、登録商標Tetronic 704としてMt.オリーブ、ニュージャージー、BASF社から入手できる。この抑制剤化合物は、PO/EOブロック共重合体の一つあたり約13のPO繰り返し単位を有し、合計では全4個のPO/EOブロック共重合体に対して約52のPO繰り返し単位を有し、PO/EOブロック共重合体に対して約11個のEO繰り返し単位と合計では全4個のPO/EOブロック共重合体に対して約44個のEO繰り返し単位を有する。それ故、登録商標Tetronic 704の合計の分子量は約5000g/molと約5500g/molの間にあり得る。構造(5)の他のブロック共重合体の例は、またBASF者から登録商標Tetronic 504として市販されている。この抑制剤化合物は、PO/EOブロック共重合体の一つあたり約9のPO繰り返し単位を有し、合計では全4個のPO/EOブロック共重合体に対して約36のPO繰り返し単位を有し、PO/EOブロック共重合体に対して約7.5個のEO繰り返し単位と合計では全4個のPO/EOブロック共重合体に対して約30個のEO繰り返し単位を有する。それ故、登録商標Tetronic 504の合計の分子量は約3200g/molと約3600g/molの間にあり得る。浴組成物は構造(5)のブロック共重合体の混合物からなることができる。
ここで、nは1と約30の間にあり、mは1と約30の間である。構造(6)を有する抑制剤化合物の源は、N−メチル化Tetronic 504またはN−メチル化Tetronic 704である。
そして、ここで、nは1と約30の間であり得て、mは1と約30の間であり得る。構造(7)を有する抑制剤化合物の源は、メチル基末端封止Tetronic 504またはメチル基末端封止Tetronic 704である。種々の代替としては末端酸素原子の一つがメチル基に結合され、そして他の3個の末端酸素原子が水素原子に結合する;または末端酸素原子の二つがメチル基に結合し、末端酸素原子の二つが水素原子に結合する;または末端酸素原子の3個がメチル基に結合し、末端酸素原子の一つが水素原子に結合する;または末端酸素原子の全てがメチル基に結合する。
そしてここで、nは1と約30の間であり得て、mは1と約30の間であり、oは約1と約5の間であり得るか、または曇り点が銅溶液と相溶することを示す程度である。好ましくは、oは1または2である。構造(8)を有する抑制剤化合物の源は、PO基末端封止Tetronic 504またはPO基末端封止Tetronic 704である。
そして、ここでnは1と約30の間であり得て、mは1と約30の間であり得る。PO/EOブロック共重合体が共有結合する、トリエチレン グリコール ジアミンは、商品名Jeffamine XTJ-504としてユタ、ソルトレークシティーのハンツマン LLCから市販されている。構造(9)の抑制剤化合物におけるPO/EOブロック共重合体の構造は、Tetronic 504とTetronic 704のPO/EOブロック構造体それと実質的に同じである。それ故、構造(9)を有する抑制剤の分子量は、約5200g/molと約5800g/molの間である。
ここで
Mは、電荷を中和するに必要な水素原子、アルカリ金属またはアンモニウムであり;
XはSまたはPであり;
Rは炭素数1〜8のアルキレンまたは環状アルキレン、炭素数6〜1の芳香族炭化水素、または脂肪族芳香族であり;
nは1〜6であり;
R1は、MO3XRであり、ここでM、XおよびRは上記定義どおりである。
160 g/L CuSO4・5H20(硫酸銅・五水物)
10g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
9 mL/L 商品名 ViaForm 促進剤
200 mg/Lのカチオン性抑制剤(MW5500g/molを有するエチレンジアミンのPO/EOブロック共重合体で、構造式(5)に相当する)。
浴(1L)は次のようにして準備された。CuSO4・5H20(160g)を脱イオン水中に十分溶解させる。濃硫酸(10g)を加えて、次に溶液中に塩素イオンで50mgと成る量の塩酸を加える。脱イオン水をさらに加えて全量を1リットルとする。最終的な浴は、さらに9 mL/L の商品名 ViaForm 抑制剤と200 mg/Lのカチオン性抑制剤(MW5500g/molを有するエチレンジアミンのPO/EOブロック共重合体で、構造式(5)に相当する)を加えて調製された。
160 g/L CuSO4・5H20(硫酸銅・五水物)
10g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
9 mL/L 商品名 ViaForm 促進剤
200 mg/Lの以下の構造式を有する比較の市販抑制剤:
ここで、e+f+gの合計は21でh+i+jの合計は27であり、これはViaformの商品名でエンソン社から入手可能である。
70 g/L CuSO4・5H20(硫酸銅・五水物)
180g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
3 mL/L 商品名 ViaForm 促進剤
400 mg/Lのカチオン性抑制剤(MW5500g/molを有するエチレンジアミンのPO/EOブロック共重合体で、構造式(5)に相当する)。
200g/L CuSO4・5H20(硫酸銅・五水物)
80g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
8mL/L 商品名 ViaForm 促進剤
200mg/Lのカチオン性抑制剤(MW5500g/molを有するエチレンジアミンのPO/EOブロック共重合体で、構造式(5)に相当する)
4mL/L のViaForm L700。
160 g/L CuSO4・5H20(硫酸銅・五水物)
10g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
18mL/L 1−プロパンスルフォン酸、3,3’−ジチオビス、ジナトリウム塩
200 mg/Lのカチオン性抑制剤(MW5700g/molを有するトリエチレン グリコール ジアミンのPO/EOブロック共重合体で、構造式(9)に相当する)
2mL/L 商品名 ViaForm。
160g/L CuSO4・5H20(硫酸銅・五水物)
10g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
9mL/L 商品名 ViaForm 促進剤
200mg/Lのカチオン性抑制剤(MW3400g/molを有するエチレンジアミンのPO/EOブロック共重合体で、構造式(5)に相当する)。
160g/L CuSO4・5H20(硫酸銅・五水物)
10g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
9mL/L 商品名 ViaForm 促進剤
200mg/L 実施例1の市販の抑制剤。
160g/L CuSO4・5H20(硫酸銅・五水物)
10g/L H2SO4 (濃硫酸)
50mg/L 塩素イオン
9mL/L 商品名 ViaForm 促進剤
200mg/Lのカチオン性抑制剤(MW5600g/molを有するトリエチレン グリコール ジアミンのPO/EO/POブロック共重合体で、構造式(8)に相当する)。
図の2Aと2Bを見ると、それは実施例1(図2A)の浴と比較例1(図2B)の浴でメッキされた試験ビアのSEM写真である。電解メッキは電流密度10mA/cm2で行った。比較例1の浴を使用した電解メッキと比較して実施例1の浴を使用した電解メッキは有意に底部と側壁のボイドが少ないことが観察されることができる。
Claims (12)
- 底、側壁および上部開口を有する直径0.5μm以下のサブミクロン径の電気内部配線凹凸を備える半導体集積回路機器基板上に電気分解メッキで銅沈積をする方法であって、該方法は以下からなる:
基板上でかつ電気内部配線凹凸上へ電気分解でメッキするに十分な4〜70g/Lの銅の供給源である硫酸銅、浴可溶性の二価の有機硫黄化合物を0.5〜1000mg/L含んでなる促進剤およびポリエーテル抑制剤化合物を含み、該化合物はプロピレンオキサイド(PO)繰り返し単位とエチレンオキサイド(EO)繰り返し単位とをPO:EO比で1:9と9:1の間の割合による組み合わせからなり、含窒素基に結合しており、該抑制剤の分子量は1000と30,000g/molの間にあるものである電気分解メッキ組成物に、底、側壁および上部開口を有するサブミクロン径の電気内部配線凹凸を備える半導体集積回路機器基板を浸漬し、ここで、前記サブミクロン径の凹凸が少なくとも3:1のアスペクト比を有する高アスペクト比凹凸を有するような次元の高アスペクト比凹凸を含むものであり;および
電気分解メッキ組成物に通電して基板上にCuを沈積して、水平方向の成長速度よりも大なる垂直方向の成長速度で急速ボトムアップ沈積することによりサブミクロン径の凹凸を超充填する。 - プロピレンオキサイド(PO)繰り返し単位とエチレンオキサイド(EO)繰り返し単位とがPO:EO比で2:3と3:2の間の割合で存在する請求項1の方法。
- 窒素含有基が二つと五つの間のアミン官能基を含む請求項1または2の方法。
- 窒素含有基がジアミンからなる請求項1または2の方法。
- 窒素含有基がエチレンジアミンとトリエチレングリコールジアミンからなる群から選ばれる基である請求項1または2の方法。
- R1は炭素数1と8の間のアルキル基であり、そしてR1はポリエーテル基が共有結合する他のアミノ基で置換されており、ポリエーテル基はEO繰り返し単位、PO繰り返し単位及びその組み合わせからなり、その配列はランダム、交互またはブロック配列である請求項6の方法。
- EPとPO繰り返し単位が、ブロック共重合体で配列している請求項1乃至9のいずれかの方法。
- ポリエーテル抑制剤が、50mg/Lと200mg/Lの間の濃度で存在する請求項1乃至10のいずれかの方法。
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JP2008519908A (ja) | 2008-06-12 |
TW200632147A (ja) | 2006-09-16 |
KR20070086082A (ko) | 2007-08-27 |
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WO2006053242A2 (en) | 2006-05-18 |
KR101138588B1 (ko) | 2012-06-27 |
CN101099231B (zh) | 2011-06-29 |
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