JP2017101320A - 酸性銅電気めっき浴から基板上のビア内へ銅を電気めっきする方法 - Google Patents
酸性銅電気めっき浴から基板上のビア内へ銅を電気めっきする方法 Download PDFInfo
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- JP2017101320A JP2017101320A JP2016201666A JP2016201666A JP2017101320A JP 2017101320 A JP2017101320 A JP 2017101320A JP 2016201666 A JP2016201666 A JP 2016201666A JP 2016201666 A JP2016201666 A JP 2016201666A JP 2017101320 A JP2017101320 A JP 2017101320A
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- Prior art keywords
- copper
- copolymer
- electroplating bath
- hlb
- alkoxylate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000010949 copper Substances 0.000 title claims abstract description 133
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 131
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 238000009713 electroplating Methods 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000758 substrate Substances 0.000 title claims abstract description 27
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 15
- 230000007547 defect Effects 0.000 claims abstract description 26
- 150000003138 primary alcohols Chemical class 0.000 claims abstract description 22
- 125000006732 (C1-C15) alkyl group Chemical group 0.000 claims abstract description 10
- 229920001400 block copolymer Polymers 0.000 claims abstract description 10
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 7
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 7
- -1 halide ion Chemical class 0.000 claims description 29
- 239000002253 acid Substances 0.000 claims description 25
- 229920001577 copolymer Polymers 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 229920000428 triblock copolymer Polymers 0.000 claims description 17
- 238000009499 grossing Methods 0.000 claims description 16
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 14
- 229910001431 copper ion Inorganic materials 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229920005604 random copolymer Polymers 0.000 abstract description 2
- 238000007747 plating Methods 0.000 description 29
- 239000003112 inhibitor Substances 0.000 description 20
- 235000012431 wafers Nutrition 0.000 description 16
- 125000000217 alkyl group Chemical group 0.000 description 15
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 15
- 229920000359 diblock copolymer Polymers 0.000 description 12
- 150000001412 amines Chemical class 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 9
- 239000007795 chemical reaction product Substances 0.000 description 9
- 241000724291 Tobacco streak virus Species 0.000 description 8
- 150000001335 aliphatic alkanes Chemical class 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 150000001924 cycloalkanes Chemical class 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 125000003545 alkoxy group Chemical group 0.000 description 4
- 238000005275 alloying Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910000365 copper sulfate Inorganic materials 0.000 description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 4
- 125000004404 heteroalkyl group Chemical group 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000006259 organic additive Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 238000000231 atomic layer deposition Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 150000002118 epoxides Chemical class 0.000 description 3
- 125000001072 heteroaryl group Chemical group 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 125000001624 naphthyl group Chemical group 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- SEULWJSKCVACTH-UHFFFAOYSA-N 1-phenylimidazole Chemical compound C1=NC=CN1C1=CC=CC=C1 SEULWJSKCVACTH-UHFFFAOYSA-N 0.000 description 2
- OBDVFOBWBHMJDG-UHFFFAOYSA-N 3-mercapto-1-propanesulfonic acid Chemical compound OS(=O)(=O)CCCS OBDVFOBWBHMJDG-UHFFFAOYSA-N 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 150000001880 copper compounds Chemical class 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical class C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 2
- 125000002228 disulfide group Chemical group 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000000879 optical micrograph Methods 0.000 description 2
- 238000000399 optical microscopy Methods 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 229920001983 poloxamer Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- AIODYXCONSJORM-UHFFFAOYSA-N sodium;3-(3-sulfopropyldisulfanyl)propane-1-sulfonic acid Chemical compound [Na].OS(=O)(=O)CCCSSCCCS(O)(=O)=O AIODYXCONSJORM-UHFFFAOYSA-N 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 125000000547 substituted alkyl group Chemical group 0.000 description 2
- 125000003107 substituted aryl group Chemical group 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 description 1
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 description 1
- WGJCBBASTRWVJL-UHFFFAOYSA-N 1,3-thiazolidine-2-thione Chemical compound SC1=NCCS1 WGJCBBASTRWVJL-UHFFFAOYSA-N 0.000 description 1
- AFEITPOSEVENMK-UHFFFAOYSA-N 1-(2-hydroxyethyl)imidazolidine-2-thione Chemical compound OCCN1CCNC1=S AFEITPOSEVENMK-UHFFFAOYSA-N 0.000 description 1
- FHTDDANQIMVWKZ-UHFFFAOYSA-N 1h-pyridine-4-thione Chemical compound SC1=CC=NC=C1 FHTDDANQIMVWKZ-UHFFFAOYSA-N 0.000 description 1
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- YXEXMVJHQLWNGG-UHFFFAOYSA-N 3-(3,3-disulfopropyldisulfanyl)propane-1,1-disulfonic acid Chemical compound OS(=O)(=O)C(S(O)(=O)=O)CCSSCCC(S(O)(=O)=O)S(O)(=O)=O YXEXMVJHQLWNGG-UHFFFAOYSA-N 0.000 description 1
- FULCXPQDMXUVSB-UHFFFAOYSA-N 3-(3-sulfanylpropylsulfonyloxy)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCOS(=O)(=O)CCCS FULCXPQDMXUVSB-UHFFFAOYSA-N 0.000 description 1
- WRBSVISDQAINGQ-UHFFFAOYSA-N 3-(dimethylcarbamothioylsulfanyl)propane-1-sulfonic acid Chemical compound CN(C)C(=S)SCCCS(O)(=O)=O WRBSVISDQAINGQ-UHFFFAOYSA-N 0.000 description 1
- LAIUFBWHERIJIH-UHFFFAOYSA-N 3-Methylheptane Chemical group CCCCC(C)CC LAIUFBWHERIJIH-UHFFFAOYSA-N 0.000 description 1
- REEBJQTUIJTGAL-UHFFFAOYSA-N 3-pyridin-1-ium-1-ylpropane-1-sulfonate Chemical compound [O-]S(=O)(=O)CCC[N+]1=CC=CC=C1 REEBJQTUIJTGAL-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229920005682 EO-PO block copolymer Polymers 0.000 description 1
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 description 1
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- RMVFTKYDJQMBRT-UHFFFAOYSA-L [Cu++].[O-]S(=O)(=O)Cc1ccccc1.[O-]S(=O)(=O)Cc1ccccc1 Chemical compound [Cu++].[O-]S(=O)(=O)Cc1ccccc1.[O-]S(=O)(=O)Cc1ccccc1 RMVFTKYDJQMBRT-UHFFFAOYSA-L 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 125000000499 benzofuranyl group Chemical group O1C(=CC2=C1C=CC=C2)* 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000002837 carbocyclic group Chemical group 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- YRNNKGFMTBWUGL-UHFFFAOYSA-L copper(ii) perchlorate Chemical compound [Cu+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O YRNNKGFMTBWUGL-UHFFFAOYSA-L 0.000 description 1
- RIOSFUBRIQHOMS-UHFFFAOYSA-L copper;benzenesulfonate Chemical compound [Cu+2].[O-]S(=O)(=O)C1=CC=CC=C1.[O-]S(=O)(=O)C1=CC=CC=C1 RIOSFUBRIQHOMS-UHFFFAOYSA-L 0.000 description 1
- IJCCOEGCVILSMZ-UHFFFAOYSA-L copper;dichlorate Chemical compound [Cu+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O IJCCOEGCVILSMZ-UHFFFAOYSA-L 0.000 description 1
- SSOVMNXYUYFJBU-UHFFFAOYSA-L copper;ethanesulfonate Chemical compound [Cu+2].CCS([O-])(=O)=O.CCS([O-])(=O)=O SSOVMNXYUYFJBU-UHFFFAOYSA-L 0.000 description 1
- BSXVKCJAIJZTAV-UHFFFAOYSA-L copper;methanesulfonate Chemical compound [Cu+2].CS([O-])(=O)=O.CS([O-])(=O)=O BSXVKCJAIJZTAV-UHFFFAOYSA-L 0.000 description 1
- MNEVGNCIZWZKLR-UHFFFAOYSA-N copper;phenol Chemical compound [Cu].OC1=CC=CC=C1.OC1=CC=CC=C1 MNEVGNCIZWZKLR-UHFFFAOYSA-N 0.000 description 1
- NPSDYIWFLLIHOT-UHFFFAOYSA-L copper;propane-1-sulfonate Chemical compound [Cu+2].CCCS([O-])(=O)=O.CCCS([O-])(=O)=O NPSDYIWFLLIHOT-UHFFFAOYSA-L 0.000 description 1
- 125000000332 coumarinyl group Chemical group O1C(=O)C(=CC2=CC=CC=C12)* 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 125000005265 dialkylamine group Chemical group 0.000 description 1
- 125000005266 diarylamine group Chemical group 0.000 description 1
- FWBOFUGDKHMVPI-UHFFFAOYSA-K dicopper;2-oxidopropane-1,2,3-tricarboxylate Chemical compound [Cu+2].[Cu+2].[O-]C(=O)CC([O-])(C([O-])=O)CC([O-])=O FWBOFUGDKHMVPI-UHFFFAOYSA-K 0.000 description 1
- 238000009792 diffusion process Methods 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
- 239000012153 distilled water Substances 0.000 description 1
- 239000002659 electrodeposit Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002541 furyl group Chemical group 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 125000001041 indolyl group Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 125000002971 oxazolyl group Chemical group 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
- 229940044652 phenolsulfonate Drugs 0.000 description 1
- 229940044654 phenolsulfonic acid Drugs 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 125000003373 pyrazinyl group Chemical group 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 125000000714 pyrimidinyl group Chemical group 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- NPAWNPCNZAPTKA-UHFFFAOYSA-M sodium;propane-1-sulfonate Chemical compound [Na+].CCCS([O-])(=O)=O NPAWNPCNZAPTKA-UHFFFAOYSA-M 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 150000003536 tetrazoles Chemical class 0.000 description 1
- 125000000335 thiazolyl group Chemical group 0.000 description 1
- 125000001544 thienyl group Chemical group 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
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- 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
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- C—CHEMISTRY; METALLURGY
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- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
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- 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
- H01L21/76841—Barrier, adhesion or liner layers
- H01L21/76871—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
- H01L21/76873—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers for electroplating
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Abstract
Description
a)銅イオン源と、酸電解液と、ハロゲン化物イオン源と、促進剤と、平滑化剤と、以下の構造を有する第1級アルコールアルコキシレートジブロック共重合体であって、
b)銅で充填される、導電性表面を有する1つ以上のビアを有する電子デバイス基板を、陰極として提供することと、
c)電子デバイス基板と銅電気めっき浴とを接触させることと、
d)銅析出物でビアを充填するために十分な期間の間、電位を印加することと、を含み、ビア内の銅析出物は実質的に空隙がなく、実質的に表面欠陥がない、方法。
R1O−[(EO)a(PO)b]−R2(II)
この共重合体中、ジブロックもしくはトリブロック配列などのブロックで、親水性のEO部分が互いに結合し、疎水性のPO部分が互いに結合するか、または代替として親水性のEO部分及び疎水性のPO部分が共重合体全体を通してランダムに分散され、R1及びR2は同じかもしくは異なり得、水素及び直鎖もしくは分岐(C1−C15)アルキ部分から選択され、a及びbは同じかもしくは異なり得、各部分のモルであり、ランダムまたはブロックアルコキシレート共重合体は16〜35のHLBを有する。好ましくは、R1及びR2は同じかまたは異なり得、水素及び直鎖または分岐(C1−C5)アルキルから選択される。より好ましくは、R1及びR2は水素である。好ましくは、HLBは17〜25であり、より好ましくは、HLBは18〜25である。
式中、R4は、必要に応じて置換されるアルキル、必要に応じて置換されるヘテロアルキル、または必要に応じて置換されるアリール基であり、Xは、水素もしくはナトリウムまたはカリウムなどの対イオンであり、R3は、水素または以下の式の基などの有機残渣であり、
式中、R4は、好ましくはアルキル、より好ましくはC1−16アルキル、及び最も好ましくは未置換のC1−8アルキルである。ヘテロアルキル基は、アルキル鎖内に1つ以上のヘテロ(N、O、またはS)原子を有し、1〜16の炭素及び好ましくは1〜8の炭素を有する。アリール基は、好ましくはフェニルまたはナフチルなどの炭素環式である。複素芳香族基は、1〜3の、N、O、及びS原子のうちの1つ以上、ならびに1〜3の分離または縮合環を含有し、例えばクマリニル、キノリニル、ピリジル、ピラジニル、ピリミジル、フリル、ピロリル、チエニル、チアゾリル、オキサゾリル、オキサジゾリル(oxidizolyl)、トリアゾール、イミダゾリル、インドリル、ベンゾフラニル、及びベンゾチアゾールを含む。ヘテロアルキル基は、1〜3の、N、O、及びS原子のうちの1つ以上、ならびに1〜3の分離または縮合環を有する基などのヘテロ脂環式基を含む。置換アルキル、ヘテロアルキル、アリール基の置換基は、例えば、C1−8アルコキシ、C1−8アルキル、F、Cl、及びBrなどのハロゲン、シアノ、ならびにニトロを含む。1つ以上の促進剤が本組成物において使用され得、好ましくは1つの促進剤が使用される。好適な二硫化物含有促進剤は、Raschigからなど、一般的に市販されており、さらに精製することなく使用され得る。好ましい二硫化物含有促進剤は、以下の式を有するものであり、
式中、R4は必要に応じて置換されるC1−6アルキルであり、Arは必要に応じて置換されるアリール基であり、Xは水素または好適な対イオンである。好ましくは、R4は必要に応じて置換されるC1−4アルキルであり、より好ましくはC1−4アルキルである。Arが必要に応じて置換されるフェニル及び必要に応じて置換されるナフチルから選択され、より好ましくはフェニル及びナフチルから選択されることが好ましい。Xのための好ましい対イオンは、ナトリウム及びカリウムである。好適な、好ましい二硫化物含有促進剤は、ビス−スルホプロピル二硫化物及びビス−ナトリウム−スルホプロピル二硫化物である。
XO3S−R”−SH(IX)
式中、R”は必要に応じて置換されるC1−6アルキル基、好ましくは未置換のC1−4アルキルであり、Xは水素もしくはナトリウムまたはカリウムなどの好適な対イオンである。例示的な追加の促進剤は当業界で周知であり、N、N−ジメチル−ジチオカルバミン酸(3−スルホプロピル)エステル、3−メルカプト−プロピルスルホン酸−(3−スルホプロピル)エステル、3−メルカプト−プロピルスルホン酸(ナトリウム塩)、3−メルカプト−1−プロパンスルホン酸(カリウム塩)を有する炭酸−ジチオ−o−エチルエステル−s−エステル、3−(ベンズチアゾリル−s−チオ)プロピルスルホン酸(ナトリウム塩)、ピリジニウムプロピルスルホベタイン、1−ナトリウム−3−メルカプトプロパン−1−スルホン酸、及び上記の組み合わせを含むが、これらに限定されない。好適な追加の促進剤が、米国特許第3,770,598号、同第3,778,357号、同第4,374,709号、同第4,376,685号、4,555,315号、及び同第4,673,469号にまた記載されている。かかる追加の促進剤は、単体で、または2つ以上の混合物として使用され得る。本組成物が、かかる追加の促進剤を有さないことが好ましい。
銅電気めっき浴を、CuSO4・5H2Oからの60g/LのCu2+と、60g/LのH2SO4と、1N HClからの50mg/LのCl−とを最初に合わせ、次いで保存溶液からの6mg/Lの促進剤ナトリウムビス(スルホプロピル)二硫化物と、ブチルジグリシジルエーテルの反応生成物である17.5mg/Lの平滑化剤と、保存溶液からの75%の4−フェニルイミダゾール及び25%のイミダゾールとを添加することによって調製した。各浴は、以下の表1に示される量で抑制剤1及び2を含む。
ビアフィル試験を、直径5μmX深さ55μmのTSVを有する様々な試験ウェハの試験片上で行った。試験片をセグメントプレータのめっきヘッドに導電性銅テープで取り付け、それを次いで3M(Minneapolis、Minnesota)からのプレータテープによって覆った。全ての試験片を、めっきする前に5分、脱イオン水噴霧に供した。各ウェハ試験片は陰極としてふるまい、それをPine Instruments製のMSRXロテータによって50rpmで回転させ、実施例1からの電気めっき浴と接触させた。電気めっき浴の温度は25℃であった。監視表面(スワール)欠陥に使用しためっき波形を表3で報告し、表中、CDは電流密度である。めっき浴の各々の動的表面張力を、25℃で、30秒の表面年齢で、Kruss BP100泡圧式表面張力計を使用して計測し、36.7mN/mになるように決定した。
実施例2で開示される方法を、抑制剤結合が表4の構成成分を有したことを除いて繰り返した。
実施例2で開示される方法を、抑制剤結合が表6の構成成分を有したことを除いて繰り返した。
銅電気めっき浴を、CuSO4・5H2Oからの60g/LのCu2+と、60g/LのH2SO4と、1N HClからの50mg/LのCl−とを最初に合わせ、次いで保存溶液からの6mg/Lの促進剤ナトリウムビス(スルホプロピル)二硫化物と、ブチル−ジグリシジルエーテルの反応生成物である15.5mg/Lの平滑化剤と、保存溶液からの75%の4−フェニルイミダゾール及び25%のイミダゾールとを添加することによって調製した。各浴は、表8に示される抑制剤を含む。
実施例6の方法を、銅めっき浴に含まれる抑制剤が以下の表10のものであることを除いて繰り返した。
Claims (12)
- 電子デバイス内のビアを銅で充填する方法であって、
a)銅イオン源と、酸電解液と、ハロゲン化物イオン源と、促進剤と、平滑化剤と、以下の式を有する第1級アルコールアルコキシレートブロック共重合体であって、
b)銅で充填される、導電性表面を有する1つ以上のビアを有する電子デバイス基板を、陰極として提供することと、
c)前記電子デバイス基板と前記銅電気めっき浴とを接触させることと、
d)銅析出物で前記ビアを充填するために十分な期間の間、電位を印加することと、を含み、前記ビア内の前記銅析出物は実質的に空隙がなく、実質的に表面欠陥がない、方法。 - 前記ランダムまたはブロックアルコキシレート共重合体の前記HLBが17〜25である、請求項1に記載の方法。
- 前記ランダムまたはブロックアルコキシレート共重合体の前記HLBが18〜25である、請求項4に記載の方法。
- 前記導電性表面がシード層である、請求項1に記載の方法。
- 前記シード層が銅シード層である、請求項6に記載の方法。
- 前記電子デバイスがウェハまたはダイである、請求項1に記載の方法。
- 銅イオン源と、酸電解液と、ハロゲン化物イオン源と、促進剤と、平滑化剤と、以下の式を有する第1級アルコールアルコキシレートブロック共重合体であって、
- 前記ランダムまたはブロックアルコキシレート共重合体の前記HLBが17〜25である、請求項9に記載の酸性銅電気めっき浴組成物。
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JP2021181586A (ja) * | 2020-05-18 | 2021-11-25 | 深▲せん▼市創智成功科技有限公司 | Icボードのスルーホールを充填するための電気銅めっき液およびその電気めっき方法 |
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JP6276363B2 (ja) | 2018-02-07 |
EP3162921B1 (en) | 2018-11-28 |
US10988852B2 (en) | 2021-04-27 |
US20170114469A1 (en) | 2017-04-27 |
TWI619853B (zh) | 2018-04-01 |
CN106609384A (zh) | 2017-05-03 |
EP3162921A1 (en) | 2017-05-03 |
KR101805642B1 (ko) | 2017-12-07 |
KR20170054234A (ko) | 2017-05-17 |
TW201715089A (zh) | 2017-05-01 |
CN106609384B (zh) | 2018-11-06 |
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