TW201912677A - 介電膜形成性組成物(一) - Google Patents
介電膜形成性組成物(一) Download PDFInfo
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- TW201912677A TW201912677A TW107107683A TW107107683A TW201912677A TW 201912677 A TW201912677 A TW 201912677A TW 107107683 A TW107107683 A TW 107107683A TW 107107683 A TW107107683 A TW 107107683A TW 201912677 A TW201912677 A TW 201912677A
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- Prior art keywords
- dielectric film
- acrylate
- meth
- composition
- weight
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 143
- 238000000034 method Methods 0.000 claims abstract description 101
- 229910052751 metal Inorganic materials 0.000 claims abstract description 75
- 239000002184 metal Substances 0.000 claims abstract description 75
- 229920000642 polymer Polymers 0.000 claims abstract description 62
- 238000000608 laser ablation Methods 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 239000010410 layer Substances 0.000 claims description 102
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 97
- -1 Carboxyethyl Chemical group 0.000 claims description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 54
- 229910052802 copper Inorganic materials 0.000 claims description 50
- 239000010949 copper Substances 0.000 claims description 50
- 239000000758 substrate Substances 0.000 claims description 43
- 238000000151 deposition Methods 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000003431 cross linking reagent Substances 0.000 claims description 24
- 239000000945 filler Substances 0.000 claims description 22
- 150000002466 imines Chemical class 0.000 claims description 22
- 229920002098 polyfluorene Polymers 0.000 claims description 21
- 239000010936 titanium Substances 0.000 claims description 21
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 20
- 230000005855 radiation Effects 0.000 claims description 20
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- 239000004065 semiconductor Substances 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012634 fragment Substances 0.000 claims description 8
- 238000000059 patterning Methods 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 239000011241 protective layer Substances 0.000 claims description 7
- 239000007983 Tris buffer Substances 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 125000003342 alkenyl group Chemical group 0.000 claims description 6
- 125000000304 alkynyl group Chemical group 0.000 claims description 6
- 229910052735 hafnium Inorganic materials 0.000 claims description 6
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 238000001039 wet etching Methods 0.000 claims description 5
- KFDGIFZCOIOUIL-UHFFFAOYSA-N CCCCO[Zr](OCCCC)OCCCC Chemical compound CCCCO[Zr](OCCCC)OCCCC KFDGIFZCOIOUIL-UHFFFAOYSA-N 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- MTKOCRSQUPLVTD-UHFFFAOYSA-N butan-1-olate;titanium(2+) Chemical compound CCCCO[Ti]OCCCC MTKOCRSQUPLVTD-UHFFFAOYSA-N 0.000 claims description 4
- NUFATYMMMZQQCQ-UHFFFAOYSA-N butan-1-olate;titanium(3+) Chemical compound [Ti+3].CCCC[O-].CCCC[O-].CCCC[O-] NUFATYMMMZQQCQ-UHFFFAOYSA-N 0.000 claims description 4
- NIOLTQNBOYMEQK-UHFFFAOYSA-N butan-1-olate;zirconium(2+) Chemical compound [Zr+2].CCCC[O-].CCCC[O-] NIOLTQNBOYMEQK-UHFFFAOYSA-N 0.000 claims description 4
- BSDOQSMQCZQLDV-UHFFFAOYSA-N butan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] BSDOQSMQCZQLDV-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
- 239000010954 inorganic particle Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 229910004613 CdTe Inorganic materials 0.000 claims description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002113 barium titanate Inorganic materials 0.000 claims description 2
- 229910021523 barium zirconate Inorganic materials 0.000 claims description 2
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000008199 coating composition Substances 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 2
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 claims description 2
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- HEMYIEDNNZJZSV-UHFFFAOYSA-N 4-prop-2-enoyloxybutanoic acid Chemical compound OC(=O)CCCOC(=O)C=C HEMYIEDNNZJZSV-UHFFFAOYSA-N 0.000 claims 1
- VHYWAYGBCDGCCQ-UHFFFAOYSA-K C(=O)(O)CCC=C(C(=O)[O-])C.C(=O)(O)CCC=C(C(=O)[O-])C.C(=O)(O)CCC=C(C(=O)[O-])C.[O-]CCCC.[Ti+4] Chemical compound C(=O)(O)CCC=C(C(=O)[O-])C.C(=O)(O)CCC=C(C(=O)[O-])C.C(=O)(O)CCC=C(C(=O)[O-])C.[O-]CCCC.[Ti+4] VHYWAYGBCDGCCQ-UHFFFAOYSA-K 0.000 claims 1
- 229910000484 niobium oxide Inorganic materials 0.000 claims 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 17
- 239000004642 Polyimide Substances 0.000 abstract description 15
- 229920001721 polyimide Polymers 0.000 abstract description 15
- 150000001252 acrylic acid derivatives Chemical class 0.000 abstract description 7
- 239000010408 film Substances 0.000 description 132
- 230000004888 barrier function Effects 0.000 description 28
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 description 20
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 19
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 18
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexyloxide Natural products O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 17
- 235000012431 wafers Nutrition 0.000 description 16
- 239000002318 adhesion promoter Substances 0.000 description 15
- 238000006116 polymerization reaction Methods 0.000 description 15
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 14
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- 239000000243 solution Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 9
- HCLJOFJIQIJXHS-UHFFFAOYSA-N 2-[2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOCCOC(=O)C=C HCLJOFJIQIJXHS-UHFFFAOYSA-N 0.000 description 8
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
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- 239000004094 surface-active agent Substances 0.000 description 8
- 238000011282 treatment Methods 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 7
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
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- 150000004985 diamines Chemical class 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 6
- WXAIEIRYBSKHDP-UHFFFAOYSA-N 4-phenyl-n-(4-phenylphenyl)-n-[4-[4-(4-phenyl-n-(4-phenylphenyl)anilino)phenyl]phenyl]aniline Chemical compound C1=CC=CC=C1C1=CC=C(N(C=2C=CC(=CC=2)C=2C=CC=CC=2)C=2C=CC(=CC=2)C=2C=CC(=CC=2)N(C=2C=CC(=CC=2)C=2C=CC=CC=2)C=2C=CC(=CC=2)C=2C=CC=CC=2)C=C1 WXAIEIRYBSKHDP-UHFFFAOYSA-N 0.000 description 5
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- 239000002243 precursor Substances 0.000 description 5
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- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 4
- CGSKOGYKWHUSLC-UHFFFAOYSA-N 1-(4-aminophenyl)-1,3,3-trimethyl-2h-inden-5-amine Chemical compound C12=CC=C(N)C=C2C(C)(C)CC1(C)C1=CC=C(N)C=C1 CGSKOGYKWHUSLC-UHFFFAOYSA-N 0.000 description 4
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 4
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- 239000001089 [(2R)-oxolan-2-yl]methanol Substances 0.000 description 3
- AMNPXXIGUOKIPP-UHFFFAOYSA-N [4-(carbamothioylamino)phenyl]thiourea Chemical compound NC(=S)NC1=CC=C(NC(N)=S)C=C1 AMNPXXIGUOKIPP-UHFFFAOYSA-N 0.000 description 3
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- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 3
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- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
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- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
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- 150000003335 secondary amines Chemical class 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- LCHWKMAWSZDQRD-UHFFFAOYSA-N silylformonitrile Chemical compound [SiH3]C#N LCHWKMAWSZDQRD-UHFFFAOYSA-N 0.000 description 1
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- MDDUHVRJJAFRAU-YZNNVMRBSA-N tert-butyl-[(1r,3s,5z)-3-[tert-butyl(dimethyl)silyl]oxy-5-(2-diphenylphosphorylethylidene)-4-methylidenecyclohexyl]oxy-dimethylsilane Chemical compound C1[C@@H](O[Si](C)(C)C(C)(C)C)C[C@H](O[Si](C)(C)C(C)(C)C)C(=C)\C1=C/CP(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 MDDUHVRJJAFRAU-YZNNVMRBSA-N 0.000 description 1
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- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- LUVHDTDFZLTVFM-UHFFFAOYSA-M tetramethylazanium;chlorate Chemical compound [O-]Cl(=O)=O.C[N+](C)(C)C LUVHDTDFZLTVFM-UHFFFAOYSA-M 0.000 description 1
- FDXKBUSUNHRUIZ-UHFFFAOYSA-M tetramethylazanium;chlorite Chemical compound [O-]Cl=O.C[N+](C)(C)C FDXKBUSUNHRUIZ-UHFFFAOYSA-M 0.000 description 1
- ZRVXFJFFJZFRLQ-UHFFFAOYSA-M tetramethylazanium;iodate Chemical compound [O-]I(=O)=O.C[N+](C)(C)C ZRVXFJFFJZFRLQ-UHFFFAOYSA-M 0.000 description 1
- ZCWKIFAQRXNZCH-UHFFFAOYSA-M tetramethylazanium;perchlorate Chemical compound C[N+](C)(C)C.[O-]Cl(=O)(=O)=O ZCWKIFAQRXNZCH-UHFFFAOYSA-M 0.000 description 1
- HLQAWDQQEJSALG-UHFFFAOYSA-M tetramethylazanium;periodate Chemical compound C[N+](C)(C)C.[O-]I(=O)(=O)=O HLQAWDQQEJSALG-UHFFFAOYSA-M 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- LUEGQDUCMILDOJ-UHFFFAOYSA-N thiophene-2,3,4,5-tetracarboxylic acid Chemical compound OC(=O)C=1SC(C(O)=O)=C(C(O)=O)C=1C(O)=O LUEGQDUCMILDOJ-UHFFFAOYSA-N 0.000 description 1
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
- MPSUGQWRVNRJEE-UHFFFAOYSA-N triazol-1-amine Chemical compound NN1C=CN=N1 MPSUGQWRVNRJEE-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- FTDRQHXSYGDMNJ-UHFFFAOYSA-N trimethoxy(3-pyrrol-1-ylpropyl)silane Chemical compound CO[Si](OC)(OC)CCCN1C=CC=C1 FTDRQHXSYGDMNJ-UHFFFAOYSA-N 0.000 description 1
- HLOLETUOZGAKMT-UHFFFAOYSA-N trimethoxysilyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)OC(=O)C(C)=C HLOLETUOZGAKMT-UHFFFAOYSA-N 0.000 description 1
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- QKHLTTQNIKDMEE-UHFFFAOYSA-N undecane-1,2,3,4-tetracarboxylic acid Chemical compound CCCCCCCC(C(O)=O)C(C(O)=O)C(C(O)=O)CC(O)=O QKHLTTQNIKDMEE-UHFFFAOYSA-N 0.000 description 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/04—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonamides, polyesteramides or polyimides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
- C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
-
- C—CHEMISTRY; METALLURGY
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Abstract
本揭示有關介電膜形成性組成物,其含有a)至少一種完全醯亞胺化的聚醯亞胺聚合物;b)至少一種含金屬的(甲基)丙烯酸酯;c)至少一種催化劑;及d)至少一種溶劑,以及相關的方法及相關的產物。該組成物可形成一介電膜,當用雷射剝蝕程序圖案化該介電膜時,其實質上不會產生碎片。
Description
相關申請案之交叉引用 本申請案請求於2017年11月6日提申之美國臨時申請案第62/581,895號及於2017年9月11日提申之美國臨時申請案第62/556,723號之優先權。該等優先申請案之全部在此併入本案以為參考。
本發明係有關於介電膜形成性組成物。
本揭示之背景 行動計算之持續的擴展,需要於更小的元件空間中封裝日益增長的計算能力。半導體元件之設計人員仰賴使用各種新晶片架構以符合新元件的需求。此等新架構不僅對新積體電路之設計人員,亦對將用於此等元件之封裝材料之設計人員帶來極大的挑戰。
本揭示之概要 因為新型先進的元件極度仰賴晶圓與面板級的封裝(WLP及PLP)及3D集成,所以用於封裝應用之介電材料的需求不斷的發展。目前是利用由透過多階通孔結構連結之多個介電堆積層構成之高密度互連(HDI)架構,來將更多的計算能力封裝進更小的空間中。在先進的半導體封裝應用中,生產具極小尺寸及緊密間距(例如2x2微米)之銅跡線之銅互連結構已成為必需。準分子雷射剝蝕介電膜是達成此圖案化位準之便利技術之一。然而,使用普通的介電材料,在剝蝕過程期間會形成大量的碎片。碎片的存在會妨礙均勻晶種層的沈積而干擾銅沈積之過程。因此,必須去除剝蝕碎片。此剝蝕碎片之去除常常需要化學和/或電漿處理之額外的清潔處理步驟,此導致成本的增加。為了減少或排除此必須的清潔處理,開發能夠進行高解析度圖案化,同時亦產生少量或不會產生剝蝕碎片之介電材料將是有利的。本揭示透過使用本發明之新穎介電膜形成性組成物滿足此需求。
本揭示之一實施例之特徵為一種新穎的介電膜形成性組成物,其含有: a)至少一種完全醯亞胺化的聚醯亞胺聚合物; b)至少一種含金屬的(甲基)丙烯酸酯; c)至少一種催化劑;及 d)至少一種溶劑。
在一些實施例中,本揭示之特徵為一種由在此所述之組成物形成之新穎的介電膜(如,自立膜)。在一些實施例中,該介電膜可含有:a)至少一種完全醯亞胺化的聚醯亞胺聚合物;b)至少一種含金屬的(甲基)丙烯酸酯(如,未交聯含金屬的(甲基)丙烯酸酯);及c)至少一種催化劑。在一些實施例中,該介電膜可包括(如,交聯後):a)至少一種完全醯亞胺化的聚醯亞胺聚合物;及b)至少一種交聯含金屬的(甲基)丙烯酸酯。
在一些實施例中,本揭示之特徵為一種沈積一導電金屬層(如,製造一內嵌銅線結構)之方法,其包括下列步驟: a)將在此所述之介電膜形成性組成物塗佈(如,利用旋塗)在一基材上,形成一介電膜; b)使該介電膜曝露於輻射源或熱; c)圖案化該膜,以形成具有開口之一圖案化介電膜;及 d)於該圖案化介電膜上之至少一個開口中沈積一導電金屬。 在一些實施例中,該方法進一步包括在沈積該導電金屬之前,於該圖案化介電膜上沈積一晶種層。
在一些實施例中,本揭示之特徵為一種製備一乾膜結構之方法。該方法包括: (A)用在此所述之介電膜形成性組成物塗佈一載體基材; (B)乾燥該塗佈的組成物,形成該介電膜;及 (C)任擇地於該介電膜上施用一保護層。
本揭示之詳細說明 在此使用之術語“完全醯亞胺化”意指本揭示之聚醯亞胺聚合物至少約90% (如,至少約95%、至少約98%、至少約99%或約100%)為醯亞胺化的。在此使用之含金屬的(甲基)丙烯酸酯(MCA)意指含金屬與(甲基)丙烯酸酯配位基之化合物。MCA之(甲基)丙烯酸酯配位基具有充份的反應性,使得該MCA能參與自由基誘發的含MCA膜之交聯反應。在此使用之術語“(甲基)丙烯酸酯”包括丙烯酸酯與甲基丙烯酸酯二者。在此使用之催化劑(如,引發劑),是當曝露於熱和/或輻射源時能夠誘發聚合反應或交聯反應之化合物。在此使用之交聯劑,是在催化劑之存在下能夠進行交聯或聚合反應之含二或多個烯基或炔基基團之化合物。
在一些實施例中,本揭示之特徵為一種介電膜形成性組成物,其含有: a)至少一種完全醯亞胺化的聚醯亞胺聚合物; b)至少一種含金屬的(甲基)丙烯酸酯; c)至少一種催化劑;及 d)至少一種溶劑。
在一些實施例中,該介電膜形成性組成物之至少一種完全醯亞胺化的聚醯亞胺聚合物,是由至少一個二胺與至少一個二羧酸二酐反應製得的。適合的二胺之例子包括,但不限於,1-(4-胺苯基)-1,3,3-三甲基二氫茚-5-胺(別稱包括4,4'-[1,4-伸苯基-雙(1-甲基亞乙基)]二苯胺)、1-(4-胺苯基)-1,3,3-三甲基-2H-茚-5-胺、1-(4-胺苯基)-1,3,3-三甲基-二氫茚-5-胺、[1-(4-胺苯基)-1,3,3-三甲基-二氫茚-5-基]胺、1-(4-胺苯基)-2,3-二氫-1,3,3-三甲基-1H-茚-5-胺、5-胺基-6-甲基-1-(3'-胺基-4'-甲基苯基)-1,3,3-三甲基二氫茚、4-胺基-6-甲基-1-(3'-胺基-4'-甲基苯基)-1,3,3-三甲基二氫茚、5,7-二胺基-1,1-二甲基二氫茚、4,7-二胺基-1,1-二甲基二氫茚、5,7-二胺基-1,1,4-三甲基二氫茚、5,7-二胺基-1,1,6-三甲基二氫茚、5,7-二胺基-1,1-二甲基-4-乙基二氫茚、對-苯二胺、間-苯二胺、鄰-苯二胺、3-甲基-1,2-苯-二胺、1,2-二胺乙烷、1,3-二胺丙烷、1,4-二胺丁烷、1,5-二胺戊烷、1,6-二胺己烷、1,7-二胺庚烷、1,8-二胺辛烷、1,9-二胺壬烷、1,10-二胺癸烷、1,2-二胺環己烷、1,4-二胺環己烷、1,3-環己烷雙(甲胺)、5-胺基-1,3,3-三甲基環己烷甲胺、2,5-二胺基三氟甲苯、3,5-二胺基三氟甲苯、1,3-二胺基-2,4,5,6-四氟苯、4,4'-二胺基二苯醚、3,4'-二胺基二苯醚、3,3'-二胺基二苯醚、3,3'-二胺聯苯碸、4,4'-二胺聯苯碸、4,4'-異亞丙基二苯胺、4,4'-二胺聯苯甲烷、2,2-雙(4-胺苯基)丙烷、4,4' 二胺聯苯丙烷、4,4'-二胺聯苯硫化物、4,4'- 二胺聯苯碸、4-胺苯基-3-胺基苯甲酸酯、2,2'-二甲基-4,4'-二胺聯苯、3,3'-二甲基-4,4'-二胺聯苯、2,2'-雙(三氟甲基) 聯胺苯、3,3'-雙(三氟甲基)聯胺苯、2,2-雙[4-(4-胺基苯氧基苯基)]六氟丙烷、2,2-雙(3-胺基-4-甲基苯基)-六氟丙烷、2,2-雙(3-胺苯基)-1,1,1,3,3,3-六氟丙烷、1,3-雙-(4-胺基苯氧基)苯、1,3-雙-(3-胺基苯氧基)苯、1,4-雙-(4-胺基苯氧基)苯、1,4-雙-(3-胺基苯氧基)苯、1-(4-胺基苯氧基)-3-(3-胺基苯氧基)苯、2,2'-雙-(4-苯氧基苯胺)異亞丙基、雙(對-b-胺基-叔-丁苯基)醚、對-雙-2-(2-甲基-4-胺戊基)苯、對-雙(1,1-二甲基-5-胺戊基)苯、3,3'-二甲基-4,4'-二胺聯苯、4,4'-二胺基二苯甲酮、3'-二氟聯胺苯、2,2-雙[4-(4-胺基苯氧基)苯基]丙烷、4,4'-[1,3-伸苯基雙(1-甲基-亞乙基)]二苯胺、4,4'-[1,4-伸苯基雙(1-甲基-亞乙基)]二苯胺、2,2-雙[4-(4-胺基苯氧基)苯基]碸、2,2-雙[4-(3-胺基苯氧基)苯]、1,4-雙(4-胺基苯氧基)苯、1,3-雙(4-胺基苯氧基)苯、(1,3'-雙(3-胺基苯氧基)苯及9H-茀-2,6-二胺。任一此等二胺可個別使用或以任一比率合併使用,只要所產的聚醯亞胺聚合物滿足本揭示之要求即可。
四羧酸二酐單體例子包括,但不限於,1-(3',4'-二羧基苯基)-1,3,3-三甲基二氫茚-5,6-二羧酸二酐、1-(3',4'-二羧基苯基)-1,3,3-三甲基二氫茚-6,7-二羧酸二酐、1-(3',4'-二羧基苯基)-3-甲基二氫茚-5,6-二羧酸二酐、1-(3',4'-二羧基苯基)-3-甲基二氫茚-6,7-二羧酸酐、吡嗪-2,3,5,6-四羧酸二酐、噻吩-2,3,4,5-四羧酸二酐、2,3,5,6-吡啶四羧酸二酐、降茨烷-2,3,5,6-四羧酸二酐、二環[2.2.2]辛-7-烯-3,4,8,9-四羧酸二酐、四環[4.4.1.02,5
.07,10
]十一烷-1,2,3,4-四羧酸二酐、3,3',4,4'-二苯基酮四羧酸二酐、3,3',4,4'-二苯基碸四羧酸二酐、3,3',4,4'-二苯醚四羧酸二酐、2,3,3',4'-二苯醚四羧酸二酐、2,2-[雙(3,4-二羧基苯基)]六氟丙烷二酐、乙二醇雙(脫水偏苯三酸酯)及5-(2,5-二氧四氫)-3-甲基-3-環己烯-1,2-二羧酸酐。更佳的四羧酸二酐單體包括2,2-[雙(3,4-二羧基苯基)]六氟丙烷二酐、3,3',4,4'-二苯基酮四羧酸二酐、3,3',4,4'-二苯基碸四羧酸二酐及3,3',4,4'-二苯醚四羧酸二酐。任一此等四羧酸二酐可單獨使用或以任一比率結合使用,只要所產生的聚醯亞胺聚合物符合本揭示之需求即可。
通常,因此形成之聚醯亞胺聚合物可溶於有機溶劑中。在一些實施例中,該聚醯亞胺聚合物在25°C有機溶劑中可具有至少約50mg/mL (如,至少約100mg/mL或至少約200mg/mL)之溶解度。有機溶劑之例子包括,但不限於,內酯類,如g-丁內酯、ε-己內酯、γ-己內酯及δ-戊內酯;環酮類,如環戊酮及環己酮;直鏈酮類,如甲乙酮(MEK);酯類,如醋酸正丁酯;酯醇類,如乳酸乙酯;醚醇類,如四氫糠醇;甘醇酯類,如丙二醇甲醚醋酸酯;及吡咯烷酮類,如正-甲基吡咯烷酮。
在一些實施例中,為合成該完全醯亞胺化的聚醯亞胺(PI)聚合物,首先製備聚醯亞胺前趨物聚合物。在一些實施例中,該PI前趨物聚合物是聚醯胺酸(PAA)聚合物。在一些實施例中,該PI前趨物是聚醯胺酯(PAE)聚合物。在一些實施例中,使一或多個二胺於至少一種(如,二、三或更多種)聚合溶劑中與一或多個四羧酸二酐結合,形成聚醯胺酸(PAA)聚合物。在一些實施例中,將所形成的PAA聚合物以化學或熱醯亞胺化成PI聚合物。在一些實施例中,在該聚合物合成期間或之後,使用適當的試劑封住該PAA聚合物之端基。在一些實施例中,將所形成的PAA聚合物酯化成聚醯胺酯(PAE)聚合物。在一些實施例中,該PAE聚合物是經由在至少一種聚合溶劑中結合四羧酸半酯與一或多個二胺而形成的。在一些實施例中,使用適當的試劑封住該PAE聚合物之端基。在一些實施例中,封端PI聚合物係從含有封端基團之PAA聚合物或PAE聚合物合成而得。在一些實施例中,在醯亞胺化之後,封住此一PI聚合物之端基。
在一些實施例中,於PAA聚合物中添加化學醯亞胺化劑(如,脫水劑),催化該聚醯胺酸基團之閉環脫水過程,形成醯亞胺官能基,從而形成PI聚合物。適合的脫水劑之例子包括,但不限於,三氟甲磺酸、甲磺酸、對-甲苯磺酸、乙磺酸、丁磺酸、全氟丁磺酸、乙酸酐、丙酸酐及丁酸酐。此外,可藉由進一步添加鹼性催化劑來催化此脫水過程。適合的鹼性催化劑之例子包括,但不限於,吡啶、三乙胺、三丙胺、三丁胺、二環己基甲胺、2,6-二甲吡啶、3,5-二甲吡啶、甲吡啶、4-二甲基胺基吡啶(DMAP)等等。
用於合成封端及未封端PI前趨物聚合物及PI聚合物之方法是熟悉此技藝之人士熟知的。此方法之例子揭示於美國專利案號US2,731,447、US3,435,002、US3,856,752、US3,983,092、US4,026,876、US4,040,831、US4,579,809、US4,629,777、US4,656,116、US4,960,860、US4,985,529、US5,006,611、US5,122,436、US5,252,534、US5,4789,15、US5,773,559、US5,783,656、US5,969,055、US9,617,386及美國專利申請案號US20040265731、US20040235992及US2007083016中,其等之全部內容在此併入本案以為參考。
用於製備PI聚合物或其等之前趨物之聚合溶劑通常是一種極性、非質子性溶劑,或二或多種極性、非質子性溶劑之組合。適合的極性、非質子性溶劑包括,但不限於,二甲基甲醯胺(DMF)、二甲基乙醯胺(DMAc)、N-甲醯嗎啉(NFM)、N-甲基吡咯烷酮(NMP)、N-乙基吡咯烷酮(NEP)、二甲基亞碸(DMSO)、g-丁內酯(GBL)、六甲基磷酸三醯胺(HMPT)、四氫呋喃(THF)、甲基四氫呋喃、1,4-二噁烷及其等之混合物。
在一些實施例中,在此所述之聚醯亞胺聚合物之重量平均分子量(Mw)為至少約5,000道爾頓(如,至少約10,000道爾頓、至少約20,000道爾頓、至少約25,000道爾頓、至少約30,000道爾頓、至少約35,000道爾頓、至少約40,000道爾頓或至少約45,000道爾頓)和/或最多約100,000道爾頓(如,最多約90,000道爾頓、最多約80,000道爾頓、最多約70,000道爾頓、最多約65,000道爾頓、最多約60,000道爾頓、最多約55,000道爾頓或最多約50,000道爾頓)。在一些實施例中,該聚醯亞胺聚合物之重量平均分子量(Mw)從約20,000道爾頓至約70,000道爾頓或從約30,000道爾頓至約80,000道爾頓。該重量平均分子量可透過凝膠滲透層析法且使用聚苯乙烯標準品計算而得。
在一些實施例中,該聚醯亞胺(A)之量為該介電膜形成性組成物之總重量(包括任何的溶劑)之至少約3重量% (如,至少約6重量%、至少約9重量%、至少約12重量%或至少約15重量%)和/或最多約40重量% (如,最多約35重量%、最多約30重量%、最多約25重量%或最多約20重量%)。在一些實施例中,該聚醯亞胺(A)之量為該介電膜形成性組成物中固體量之至少約10重量% (如,至少約12.5重量%、至少約15重量%、至少約20重量%或至少約25重量%)和/或最多約60重量% (如,最多約55重量%、最多約50重量%、最多約45重量%、最多約40重量%、最多約35重量%或最多約30重量%)。 在此使用之該介電膜形成性組成物中之固體量,意指該組成物之總重量減去該組成物中之溶劑量,或由該組成物形成之介電膜之總重量。
可用於本揭示之含金屬的(甲基)丙烯酸酯(MCAs),通常與該介電膜形成性組成物中之其它成份具有充分的相容性,且在混合時易於分散或溶於該組成物中。該MCAs可以固體或溶液之形式併入該介電膜形成性組成物中。通常,該含MCA之組成物在25°C下靜置至少24個小時之期間後不會形成相分離(變得看得出非均質)。此外,由該含MCA之組成物形成之介電膜一般看起來是清澈且均質的。
可用於本揭示中之MCAs之適合的金屬原子包括鈦、鋯、鉿及鍺。在一些實施例中,該MCAs包括至少一個金屬原子及至少一個(如,一、二、三或四個) (甲基)丙烯酸酯基團。較佳的MCAs含三或四個連接至各金屬原子之(甲基)丙烯酸酯基團。適合的MCAs之例子包括,但不限於,四(甲基)丙烯酸鈦、四(甲基)丙烯酸鋯、四(甲基)丙烯酸鉿、丁醇鈦三(甲基)丙烯酸酯、二丁醇鈦二(甲基)丙烯酸酯、三丁醇鈦(甲基)丙烯酸酯、丁醇鋯三(甲基)丙烯酸酯、二丁醇鋯二(甲基)丙烯酸酯、三丁醇鋯(甲基)丙烯酸酯、丁醇鉿三(甲基)丙烯酸酯、二丁醇鉿二(甲基)丙烯酸酯、三丁醇鉿(甲基)丙烯酸酯、鈦四(羧乙基(甲基)丙烯酸酯)、鋯四(羧乙基(甲基)丙烯酸酯)、鉿四(羧乙基(甲基)丙烯酸酯)、丁醇鈦三(羧乙基(甲基)丙烯酸酯)、二丁醇鈦二(羧乙基(甲基)丙烯酸酯)、三丁醇鈦(羧乙基(甲基)丙烯酸酯)、丁醇鋯三(羧乙基(甲基)丙烯酸酯)、二丁醇鋯二(羧乙基(甲基)丙烯酸酯)、三丁醇鋯(羧乙基(甲基)丙烯酸酯)、丁醇鉿三(羧乙基(甲基)丙烯酸酯)、二丁醇鉿二(羧乙基(甲基)丙烯酸酯)或三丁醇鉿(羧乙基(甲基)丙烯酸酯)。通常該MCAs之(甲基)丙烯酸酯基團具有充分的反應性,使得該MCA能參與由自由基誘發(可由該介電膜形成性組成物中所存在之一或多種催化劑產生)的含MCA膜之交聯或聚合反應。該交聯或聚合反應可在該介電膜形成性組成物中之至少二個MCAs之間或至少一個MCA與至少一個非MCA交聯劑之間發生。在一些實施例中,MCA是一交聯劑(如,當MCA包括二或多個(甲基)丙烯酸酯基團時)。在一些實施例中,MCA是適合用於聚合反應或作為鏈終止劑之單體(如,當該MCA僅包括一個(甲基)丙烯酸酯基團時)。在一些實施例中,於在此所述之組成物所形成之交聯介電膜中,該MCA是沒有交聯的(如,當該MCA僅包括一個(甲基)丙烯酸酯基團時)。
在一些實施例中,該至少一種MCA之量為該介電膜形成性組成物之總重量之至少約0.5重量% (如,至少約1重量%、至少約2重量%、至少約3重量%、至少約4重量%或至少約5重量%)和/或最多約20重量% (如,最多約18重量%、最多約16重量%、最多約14重量%、最多約12重量%或最多約10重量%)。在一些實施例中,該MCA之量為該介電膜形成性組成物中固體量之至少約1重量% (如,至少約2重量%、至少約4重量%、至少約6重量%、至少約8重量%或至少約10重量%)和/或最多約25重量% (如,最多約20重量%、最多約18重量%、最多約16重量%、最多約14重量%或最多約12重量%)。
出人意料的觀察到,該介電膜形成性組成物中至少一種MCA之存在,可使當使用雷射剝蝕程序圖案化從該組成物形成之介電膜時碎片的產生減至最少。
在一些實施例中,本揭示之介電膜形成性組成物可包括至少一種催化劑(如,引發劑)。當曝露於熱和/或輻射源時,該催化劑能夠誘發交聯或聚合反應。
在一些實施例中,所使用之催化劑是光引發劑,在此該光引發劑是當曝露於高能輻射時能夠產生自由基之化合物。高能輻射之非限制性例子包括電子束、紫外線及X射線。不希望受理論之約束,一般認為光引發劑可誘發涉及MCA化合物之(甲基)丙烯酸酯基團和/或該組成物中能夠進行交聯或聚合反應之其它實體之交聯或聚合反應。此實體之例子包括交聯劑(如,非MCA交聯劑)及帶有烯基及炔基官能基團之聚醯亞胺。
光引發劑之特定例子包括,但不限於,1,8-辛二酮、1,8-雙[9-(2-乙己基)-6-硝基-9H-咔唑-3-基]-1,8-雙(O-乙醯肟)、2-羥基-2-甲基-1-苯基丙-1-酮、1-羥基環己基苯基酮(BASF之Irgacure 184)、1-羥基環己基苯基酮與二苯基酮之摻合物(BASF之Irgacure 500)、2,4,4-三甲基苯基氧化膦(BASF之Irgacure 1800、1850及1700)、2,2-二甲氧基-2-乙醯苯(BASF之Irgacure 651)、雙(2,4,6-三甲基苯甲醯基)苯基氧化膦(BASF之Irgacure 819)、2-甲基-1-[4-(甲硫基)苯基]-2-嗎啉代丙-1-酮(BASF之Irgacure 907)、(2,4,6-三甲基苯甲醯基)二苯基氧化膦(BASF之Lucerin TPO)、乙氧基(2,4,6-三甲基苯甲醯基)苯基氧化膦(BASF之Lucerin TPO-L);氧化膦、羥基酮與二苯基酮衍生物之摻合物(Arkema之ESACURE KTO46);2-羥基-2-甲基-1-苯基丙-1-酮(Merck之Darocur 1173)、NCI-831(ADEKA Corp.)、N-1919 (ADEKA Corp.)、2-(苯甲醯氧基亞胺基)-1-[4-(苯硫基)苯基]-1-辛酮(可得自BASF之OXE-01)、1-(O-乙醯基肟)-1-[9-乙基-6-(2-甲基苯甲醯基)-9H-咔唑-3-基]乙酮(可得自BASF之OXE-02)、二苯基酮、2-氯噻噸酮、2-甲基噻噸酮、2-異丙基噻噸酮、苯並二甲基縮酮、1,1,1-三氯苯乙酮、二乙氧基苯乙酮、間-氯苯乙酮、苯丙酮、蒽醌、二苯並環庚酮等等。
非離子性類光引發劑之特定例子包括:(5-甲苯甲醯基磺醯氧基亞胺基-5H-苯硫-2-亞基)-2-甲基苯基-乙腈(BASF之Irgacure 121)、對-甲基苯磺酸苯甲醯甲酯、對-甲苯磺酸安息香酯、(對-甲苯-磺醯氧基)甲基安息香、3-(對-甲苯磺醯氧基)-2-羥基-2-苯基-1-苯丙基醚、N-(對-十二烷基苯磺醯氧基)-1,8-萘二甲醯亞胺、N-(苯基-磺醯氧基)-1,8-萘二甲醯亞胺、雙(環己基磺醯基)重氮甲烷、1-對-甲苯磺醯基-1-環己基羰基重氮甲烷、對甲苯磺酸2-硝基苯甲酯、對甲苯磺酸2,6-二硝基苯甲酯及對三氟甲基苯磺酸2,4-二硝基苯甲酯等等。
在一些實施例中,可於該介電膜形成性組物中使用一光敏劑,在此該光敏劑可吸收193至405nm波長範圍之光。光敏劑之例子包括,但不限於,9-甲蒽、蒽甲醇、苊、噻噸酮、甲基-2-萘基酮、4-乙醯基聯苯及1,2-苯並茀。
在交聯或聚合反應是通過熱誘發之實施例中,所使用之催化劑是熱引發劑,在此該熱引發劑是當曝露於從約70°C至約250°C之溫度時,能夠產生自由基之化合物。不希望受理論之約束,一般認為熱引發劑會誘發涉及MCA化合物之(甲基)丙烯酸酯基團和/或該組成物中能夠進行交聯或聚合反應之其它實體之交聯或聚合反應。此實體之例子包括交聯劑(如,非MCA交聯劑)及帶有烯基及炔基官能基團之聚醯亞胺。
熱引發劑之特定例子包括,但不限於,過氧化苯甲醯、過氧化環己酮、過氧化月桂醯基、過氧苯甲酸叔戊酯、過氧化氫叔丁基、雙異丙苯過氧化物、異丙苯過氧化氫、過氧化琥珀酸、二(正丙基)過氧二羧酸酯、2,2-偶氮雙(異丁腈)、2,2-偶氮雙(2,4-二甲基戊腈)、二甲基-2,2-偶氮雙異丁酸酯、4,4-偶氮雙(4-氰戊酸)、偶氮雙環己烷甲腈、2,2-偶氮雙(2-甲基丁腈)等等。
在一些實施例中,可於該介電膜形成性組成物中使用二或多種催化劑之組合。該催化劑之組合可全為熱引發劑、全為光引發劑或熱引發劑與光引發劑之組合。
在一些實施例中,該催化劑之量為該介電膜形成性組成物之總重量之至少約0.25重量% (如,至少約0.5重量%、至少約0.75重量%、至少約1.0重量%或至少約1.5重量%)和/或最多約4.0重量% (如,最多約3.5重量%、最多約3.0重量%、最多約2.5重量%或最多約2.0重量%)。在一些實施例中,該催化劑之量為該介電膜形成性組成物中固體量之至少約0.5重量% (如,至少1.0重量%、至少約1.5重量%、至少約2.0重量%或至少約2.5重量%)和/或最多約5.0重量% (如,最多約4.5重量%、最多約4.0重量%、最多約3.5重量%或最多約3.0重量%)。
可用於本揭示之介電膜形成性組成物之有機溶劑之適合的例子包括,但不限於,g
-丁內酯(GBL)、N-甲基-2-吡咯烷酮(NMP)、二甲基咪唑啉酮、N-甲基己內醯胺、N-甲基丙醯胺、N,N-二甲基乙醯胺(DMAc)、二甲基亞碸(DMSO)、N,N-二甲基甲醯胺(DMF)、N,N-二乙基甲醯胺、二乙基乙醯胺、甲乙酮(MEK)、甲基異丁酮(MIBK)、2-庚酮、環戊酮(CP)、環己酮、醋酸正丁酯(nBA)、丙二醇甲醚醋酸酯(PGMEA)、丙二醇甲醚(PGME)、乳酸乙酯(EL)、乳酸丙酯、3-甲基-3-甲氧丁醇、四氫萘、異佛酮、乙二醇單丁醚、二乙二醇單***、二乙二醇單***醋酸酯、二乙二醇二甲醚、二乙二醇甲***、三乙二醇單***、二丙二醇單甲醚、3-甲氧丙酸甲酯、3-乙氧丙酸乙酯、丙二酸二乙酯、乙二醇1,4:3,6-二脫水山梨醇、正丁醇、2,5-二甲醚(2,5-二甲基異山梨糖醇酐)、1,4:3,6-二脫水山梨醇2,5-二***(2,5-二乙基異山梨糖醇酐)及其等之混合物。在一些較佳實施例中,該有機溶劑可為g
-丁內酯(GBL)、環戊酮(CP)、環己酮、正丁醇、N-甲基-2-吡咯烷酮(NMP)、二甲基亞碸(DMSO)或其等之混合物。此等溶劑可個別或合併使用,只要其可完全溶解該組成物中之除不溶性填料外之所有的組份、澆注出良好的膜且不會干擾結合反應即可。
在一些實施例中,該介電膜形成性組成物中該有機溶劑之量為該介電膜形成性組成物之總重量之至少約35重量% (如,至少約40重量%、至少約45重量%、至少約50重量%、至少約55重量%、至少約60重量%或至少約65重量%)和/或最多約98重量% (如,最多約95重量%、最多約90重量%、最多約85重量%、最多約80重量%、最多約75重量%或最多約70重量%)。
在一些實施例中,本揭示之介電膜形成性組成物可進一步包括至少一種交聯劑(如,非-MCA交聯劑)。在一些實施例中,該交聯劑含有二或多個烯基或炔基基團。一般而言,該交聯劑能夠在催化劑之存在下進行交聯或聚合反應。
在一些實施例中,該至少一種交聯劑是至少一種胺基甲酸乙酯丙烯酸酯寡聚物。術語“胺基甲酸乙酯丙烯酸酯寡聚物”意指含有胺基甲酸乙酯鍵聯且具有(甲基)丙烯酸酯(如,丙烯酸酯或甲基丙烯酸酯)官能基之胺基甲酸乙酯(甲基)丙烯酸酯類化合物,諸如胺基甲酸乙酯多(甲基)丙烯酸酯、多胺基甲酸乙酯(甲基)丙烯酸酯及多胺基甲酸乙酯多(甲基)丙烯酸酯。胺基甲酸乙酯(甲基)丙烯酸酯寡聚物之類型述於例如Coady et al.之美國專利案號US4,608,409及Chisholm et al.之美國專利案號US6,844,950中,其等之內容在此併入本案以為參考。可用於本揭示之胺基甲酸乙酯丙烯酸酯寡聚物之特定例子包括,但不限於,CN9165US、CN9167US、CN972、CN9782、CN9783及CN992。此等及其它胺基甲酸乙酯丙烯酸酯寡聚物是可從Arkema (Sartomer)商業購得的。
在一些實施例中,該交聯劑含有至少二個(甲基)丙烯酸酯基團。在一些實施例中,該交聯劑係選自於由下列所構成之群組:1,6-己二醇二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、1,12-十二烷二醇二(甲基)丙烯酸酯、1,3-丁二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、環己烷二甲醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、丙氧基化(3)甘油三(甲基)丙烯酸酯、二乙烯基苯、乙氧基化雙酚-A-二(甲基)丙烯酸酯、二乙二醇雙(烯丙基碳酸酯)、三甲醇丙烷三(甲基)丙烯酸酯、二三甲醇丙烷四(甲基)丙烯酸酯、新戊四醇三(甲基)丙烯酸酯、新戊四醇四(甲基)丙烯酸酯、二季戊四醇戊-/己-(甲基)丙烯酸酯、異氰脲酸酯三(甲基)丙烯酸酯、雙(2-羥乙基)-異氰脲酸酯二(甲基)丙烯酸酯、1,3-丁二醇三(甲基)丙烯酸酯、1,4-丁二醇三(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、(甲基)丙烯酸酯改質的脲-甲醛樹脂、(甲基)丙烯酸酯改質的三聚氰胺-甲醛樹脂及(甲基)丙烯酸酯改質的纖維素。
在一些實施例中,該介電膜形成性組成物中該交聯劑之量為該組成物之總重量之至少約2.5重量% (如,至少約5重量%、至少約7.5重量%、至少約10重量%、至少約12.5重量%或至少約15重量%)和/或最多約30重量% (如,最多約27.5重量%、最多約25重量%、最多約22.5重量%、最多約20重量%或最多約17.5重量%)。在一些實施例中,該介電膜形成性組成物中該交聯劑之量為該組成物中固體量之約5重量% (如,至少約10重量%、至少約15重量%、至少約20重量%、至少約25重量%或至少約30重量%)和/或最多約60重量% (如,最多約55重量%、最多約50重量%、最多約45重量%、最多約40重量%或最多約35重量%)。不希望受理論之約束,一般認為交聯劑可改善由在此所述之組成物形成之介電膜之機械特性及化學抗性。
本揭示之介電膜形成性組成物可任擇地包括其它組份,諸如助黏劑、填料、界面活性劑、塑化劑、銅鈍化劑、著色劑及染料。
在一些實施例中,本揭示之介電膜形成性組成物進一步包括一或多種助黏劑。適合的助黏劑述於“Silane Coupling Agent” Edwin P. Plueddemann, 1982 Plenum Press, New York中。助黏劑之種類包括,但不限於,巰基烷氧基矽烷、胺基烷氧基矽烷、環氧基烷氧基矽烷、環氧丙基氧基烷氧基矽烷、巰基矽烷、氰氧基矽烷及咪唑矽烷。 在一些實施例中,該助黏劑包含烷氧矽基及含碳-碳多鍵之官能基(其選自取代或未取代烯基基團及取代或未取代炔基基團)二者。
若有使用,該介電膜形成性組成物中該任擇的助黏劑之量為該組成物之總重量之至少約0.3重量% (如,至少約0.5重量%、至少約0.7重量%或至少約1重量%)和/或最多約4重量% (如,最多約3重量%、最多約2重量%或最多約1.5重量%)。在一些實施例中,該介電膜形成性組成物中該任擇的助黏劑之量為該組成物中固體量之至少約0.5重量% (如,至少約1重量%、至少約2重量%或至少約2.5重量%)和/或最多約8重量% (如,最多約6重量%、最多約5重量%、最多約4重量%或最多約3重量%)。
在一些實施例中,本揭示之介電膜形成性組成物可進一步包括一或多種填料。在一些實施例中,該填料是無機粒子。在一些實施例中,該無機粒子選自於由下列所構成之群組:二氧化矽、氧化鋁、二氧化鈦、氧化鋯、氧化鉿、CdSe、CdS、CdTe、CuO、氧化鋅、氧化鑭、氧化鈮、氧化鎢、氧化鍶、氧化鈣鈦、鈦酸鈉、硫酸鋇、鈦酸鋇、鋯酸鋇、鈮酸鉀。較佳地,該無機填料呈具平均粒徑約0.1-20微米之顆粒形式。在一些實施例中,該填料是有機粒子,在此該有機粒子不溶於該組成物之溶劑中。有機粒子之例子包括,但不限於,交聯橡膠粒子、交聯或非交聯聚醯亞胺粒子及交聯聚合物粒子。
可在本揭示中使用之二氧化矽填料可為親水性或疏水性的。疏水性二氧化矽填料可通過親水性、氣相二氧化矽之表面改質而產生,或通過直接形成表面改質的二氧化矽填料而產生。直接形成表面改質的二氧化矽填料,通常是由官能性矽烷之水解縮合達成。可在本揭示中使用之表面改質的二氧化矽填料之表面上,可具有反應性和/或無反應性基團。可在本揭示中使用之填料(如,二氧化矽填料)具有最多約2微米(如,最多約1.5微米、最多約1微米、最多約0.75微米、最多約0.5微米、最多約0.25微米或最多約0.2微米)和/或至少約0.1微米(如,至少約0.2微米、至少約0.3微米、至少約0.5微米或至少約1微米)之粒徑(如,平均粒徑)。該填料尺寸分佈可為窄的(如,基本上單分散)或寬的。所需的填料尺寸及分佈可通過熟悉此技藝之人士已知之任一技術達成,包括,但不限於,碾磨、研磨及過濾。在一些實施例中,該二氧化矽填料分散於有機溶劑中。在溶劑中的分散可以通過熟悉此技藝之人士已知的各種方法來完成,包括,但不限於,介質磨及高剪切混合。可用於分散二氧化矽填料之溶劑沒有特別限制。較佳的溶劑包括酯類、醚類、內酯類、酮類、醯胺類及醇類。更佳的溶劑包括GBL、環戊酮、環己酮、乳酸乙酯及正丁醇。
在一些實施例中,若有使用,則本揭示之介電膜形成性組成物中該填料(如,二氧化矽填料)之量為該組成物之總重量之至少約2重量% (如,至少約4重量%、至少約6重量%、至少約8重量%或至少約10重量%)和/或最多約20重量% (如,最多約18重量%、最多約15重量%或最多約12重量%)。在一些實施例中,本揭示之介電膜形成性組成物中該填料(如,二氧化矽填料)之量為該組成物中固體量之至少約5重量% (如,至少約10重量%、至少約14重量%、至少約17重量%或至少約20重量%)和/或最多約40重量% (如,最多約35重量%、最多約30重量%或最多約25重量%)。
本揭示之介電膜形成性組成物亦可任擇地含有一或多種界面活性劑。若有使用界面活性劑,則該界面活性劑之量為該介電膜形成性組成物之總重量之至少約0.001重量% (如,至少約0.01重量%或至少約0.1重量%)和/或最多約2重量% (如,最多約1重量%或最多約0.5重量%)。在一些實施例中,該界面活性劑之量為該介電膜形成性組成物中固體量之至少約0.002重量% (如,至少約0.02重量%或至少約0.2重量%)和/或最多約4重量% (如,最多約1重量%或最多約0.5重量%)。適合的界面活性劑之例子包括,但不限於,JP-A-62-36663、JP-A-61-226746、JP-A-61-226745、JP-A-62-170950、JP-A-63-34540、JP-A-7-230165、JP-A-8-62834、JP-A-9-54432及JP-A-9-5988中所述之界面活性劑。
本揭示之介電膜形成性組成物可任擇地含有一或多種塑化劑。若有使用,則該任擇的塑化劑之量為該介電膜形成性組成物之總重量之至少約1重量% (如,至少約2重量%或至少約3重量%)和/或最多約10重量% (如,最多約7.5重量%或至少約5重量%)。在一些實施例中,該任擇的塑化劑之量為該介電膜形成性組成物中固體量之至少約2重量% (如,至少約4重量%或至少約6重量%)和/或最多約20重量% (如,最多約14重量%或最多約10重量%)。
本揭示之介電膜形成性組成物可任擇地含有一或多種銅鈍化劑。銅鈍化劑之例子包括***化合物、咪唑化合物及四唑化合物。***化合物可包括***、苯並***、取代的***及取代的苯並***。取代基之例子包括C1
-C8
烷基、胺基、硫醇基、巰基、亞胺基、羧基及硝基基團。***化合物之特定例子包括苯並***、1,2,4-***、1,2,3-***、甲苯***、5-甲基-1,2,4-***、5-苯基-苯並***、5-硝基-苯並***、3-胺基-5-巰基-1,2,4-***、1-胺基-1,2,4-***、羥苯並***、2-(5-胺基-苯基)-苯並***、1-胺基-1,2,3-***、1-胺基-5-甲基-1,2,3-***、3-胺基-1,2,4-***、3-巰基-1,2,4-***、3-異丙基-1,2,4-***、5-苯硫醇-苯並***、鹵基-苯並***(鹵基= F、Cl、Br或I)、萘並***等等。咪唑化合物之例子包括,但不限於,2-烷基-4-甲基咪唑、2-苯基-4-烷基咪唑、2-甲基-4(5)-硝基咪唑、5-甲基-4-硝基咪唑、4-羥甲基咪唑鹽酸鹽、2-巰基-1-甲基咪唑。四唑化合物之例子包括,但不限於,1-H-四唑、5-甲基-1H-四唑、5-苯基-1H-四唑、5-胺基-1H-四唑、1-苯基-5-巰基-1H-四唑、5,5'-雙-1H-四唑、1-甲基-5-乙基四唑、1-甲基-5-巰基四唑、1-羧甲基-5-巰基四唑等等。
在一些實施例中,若有使用,則該任擇的銅鈍化劑之量為該介電膜形成性組成物之總重量之至少約0.01重量% (如,至少約0.05重量%、至少約0.1重量%或至少約0.5重量%)和/或最多約2重量% (如,最多約1.5重量%或最多約1重量%)。在一些實施例中,該任擇的銅鈍化劑之量為該介電膜形成性組成物中固體量之至少約0.02重量% (如,至少約0.1重量%、至少約0.2重量%或至少約1重量%)和/或最多約4重量% (如,最多約3重量%或最多約2重量%)。
本揭示之介電膜形成性組成物可任擇地含有一或多種染料和/或一或多種著色劑。
在一些實施例中,該聚醯亞胺可從除了結構(1)之矽氧烷二胺外之二胺製得:結構(I) 其中R1
及R2
各獨立為二價脂族或芳族基團(如,C1-6
二價脂族基團或C6-12
二價芳族基團),R3
、R4
、R5
及R6
各獨立為單價脂族或芳族基團(如,C1-6
單價脂族基團或C6-12
單價芳族基團),及m是1 – 100之整數。
具結構(III)之矽氧烷二胺單體之例子包括,但不限於:。
在一些實施例中,本揭示之介電膜形成性組成物可明確地排除下列溶劑中之一或多種(若超過一種,則為其等之任一組合)。此等溶劑可選自於由下列所構成之群組:直鏈酮類,諸如甲乙酮(MEK);酯類,諸如醋酸乙酯;酯醇類,諸如乳酸乙酯;醚醇類,諸如四氫糠醇;及甘醇酯類,諸如丙二醇甲醚醋酸酯(PGMEA)。
在一些實施例中,本揭示之介電膜形成性組成物可明確地排除下列助黏劑中之一或多種(若超過一種,則為其等之任一組合)。此等助黏劑可選自於由下列所構成之群組:含初級胺之助黏劑(諸如,3-胺丙基三乙氧基矽烷及間-胺苯基三乙氧基矽烷)、含次級胺之助黏劑(諸如N-環己胺基三甲氧基矽烷)、含三級胺之助黏劑(諸如二乙胺基乙基三乙氧基矽烷)、含脲之助黏劑(諸如脲丙基三甲氧基矽烷)、含酐之助黏劑(諸如3-(三乙氧基矽基)丙基琥珀酸酐)、含環氧基之助黏劑(諸如2-(3,4-環氧基環己基)乙基三乙氧基矽烷)、含異氰氧基之助黏劑(諸如3-異氰氧丙基三乙氧基矽烷)及含硫之助黏劑(諸如3-巰基丙基三甲氧基矽烷)。
在一些實施例中,本揭示之介電膜形成性組成物可明確地排除添加物組份中之一或多種(若超過一種,則為其等之任一組合)。此等組份可選自於由下列所構成之群組:非聚醯亞胺聚合物、非交聯非聚醯亞胺聚合物、界面活性劑、塑化劑、著色劑、染料、水、除氧劑、季銨氫氧化物、胺類、鹼金屬及鹼土金屬鹼基(諸如NaOH、KOH、LiOH、氫氧化鎂及氫氧化鈣)、含氟化物單體化合物、氧化劑(如,過氧化物、過氧化氫、硝酸鐵、碘酸鉀、過錳酸鉀、硝酸、亞氯酸銨、氯酸銨、碘酸銨、過硼酸銨、過氯酸銨、過碘酸銨、過硫酸銨、亞氯酸四甲基銨、氯酸四甲基銨、碘酸四甲基銨、過硼酸四甲基銨、過氯酸四甲基銨、過碘酸四甲基銨、過硫酸四甲基銨、過氧化脲及過醋酸)、研磨劑、矽酸鹽、防蝕劑(如,非唑防蝕劑)、胍、胍鹽、無機酸(如,磺酸、硫酸、亞硫酸、亞硝酸、硝酸、亞磷酸及磷酸)、有機酸(如,羥羧酸及羧酸及聚羧酸)、吡咯烷酮、聚乙烯吡咯烷酮及金屬鹵化物。
不希望受理論之限制,一般認為本揭示之介電膜形成性組成物可使當使用雷射剝蝕程序圖案化由該組成物形成之介電膜時碎片的產生減至最少。如此,當在半導體基材上形成導電金屬層(如,銅層)之製程中使用此一組成物時,在塗佈晶種層(如,包括障壁層及金屬晶種層)之前,該製程不需要碎片清除程序或預處理程序。
在一些實施例中,本揭示之特徵在於一種由在此所述之介電膜形成性組成物形成之介電膜。在一些實施例中,當該介電膜還沒通過曝露輻射源或熱交聯時,該介電膜可包括:a)至少一種完全聚醯亞胺化的聚醯亞胺聚合物;b)至少一種含金屬的(甲基)丙烯酸酯;及c)至少一種催化劑。在一些實施例中,該介電膜可進一步包括至少一種交聯劑(諸如該等以上針對該介電膜形成性組成物描述者)。
在一些實施例中,當該介電膜已通過曝露於輻射源或熱而交聯時,該介電膜可包括a)至少一種完全醯亞胺化的聚醯亞胺聚合物;b)至少一種交聯含金屬的(甲基)丙烯酸酯;及c)任擇地至少一種無機填料。在此實施例中,該至少一種完全醯亞胺化的聚醯亞胺聚合物可為未交聯的,或(如,當該聚合物具有至少一種交聯基團時)可為自身交聯的或與含金屬的(甲基)丙烯酸酯交聯的。
在一些實施例中,本揭示之介電膜在308nm、355nm、365nm或405nm波長下之光吸收為至少約0.1 µm-1
(如,至少約0.5 µm-1
、至少約1 µm-1
、至少約2 µm-1
、至少約3 µm-1
、至少約5 µm-1
、至少約7 µm-1
或至少約9 µm-1
)。
在一些實施例中,本揭示之特徵為一種製備乾膜結構之方法。該方法包括: (A)用在此所述之介電膜形成性組成物塗佈一載體基材,形成一塗佈組成物,該組成物含有:a)至少一種完全醯亞胺化的聚醯亞胺聚合物;b)至少一種含金屬的(甲基)丙烯酸酯;c)至少一種催化劑;d)至少一種溶劑,及e)任擇地至少一種交聯劑; (B)乾燥該塗佈組成物,形成一介電膜;及 (C)任擇地於該介電膜上施用一保護層。在一些實施例中,該載體基材具有極佳的透光性,且其實質上對用於在該聚合物層上形成浮雕圖案之光照射是透明的。該載體基材之厚度較佳地在至少約10µm (如,至少約15µm、至少約20µm、至少約30µm、至少約40µm、至少約50µm或至少約60µm)至最多約150µm (如,最多約140µm、最多約120µm、最多約100µm、最多約90µm、最多約80µm或最多約70µm)之範圍內。
在一些實施例中,該載體基材是一單或多層膜,其可包括一或多種聚合物(如,聚對苯二甲酸乙二酯)。 在一些實施例中,該保護層基材是一單或多層膜,其可包括一或多種聚合物(如,聚乙烯或聚丙烯)。載體基材及保護層之例子述於美國專利申請公開案第2016/0313642號中,其內容在此併入本案以為參考。在一些實施例中,該乾膜結構中之介電膜還未曝露於輻射源或熱中,如,形成一交聯膜。
在一些實施例中,該乾膜之介電膜可與載體層分離成為自立介電膜。自立介電膜是可在不使用任何諸如載體層之支撐層之情況下維持其物理完整性之膜。在一些實施例中,該自立介電膜可包括(如,交聯前):a)至少一種完全醯亞胺化的聚醯亞胺聚合物;b)至少一種含金屬的(甲基)丙烯酸酯(如,未交聯含金屬的(甲基)丙烯酸酯);及c)至少一種催化劑(如,能夠誘發聚合反應之催化劑)。在一些實施例中,該自立介電膜可曝露於輻射源或熱而形成一交聯自立介電膜。在一些實施例中,該交聯自立介電膜可包括:a)至少一種完全醯亞胺化的聚醯亞胺聚合物;及b)至少一種交聯含金屬的(甲基)丙烯酸酯。在一些實施例中,可在用平面壓縮程序或熱輥壓縮程序預層壓該介電膜之後,使用真空層壓機,在約50o
C至約140o
C下,將該自立介電膜(交聯或未交聯的)層壓於一基材(如,半導體基材)上。
在一些實施例中,可在用平面壓縮程序或熱輥壓縮程序預層壓該乾膜之介電膜之後,使用真空層壓機,在約60o
C至約140o
C之溫度下,將該乾膜結構之介電膜層壓於一基材(如,半導體基材)上。當使用熱輥層壓時,可將該乾膜結構置於熱輥層壓機上,可從該介電膜/載體基材上剝除該任擇的保護層,及可使用滾筒伴隨熱及壓力,使該介電膜與一基材接觸並層壓在一起,形成含該基材、該介電膜及該載體基材之一物件。之後使該介電膜曝露於輻射源或熱(如,通過該載體基材),形成一交聯膜。在一些實施例中,可在使該介電膜曝露於輻射源或熱之前,先去除該載體基材。
在一些實施例中,利用含有下列步驟之方法從本揭示之介電膜形成性組成物製備一介電膜: a)將在此所述之介電膜形成性組成物塗佈於一基材上,形成一介電膜; b)任擇地在約50°C至約150°C之溫度下烘烤該膜約20秒至約240秒;及 c)使該介電膜曝露於輻射源或熱。
用於製備該介電膜之塗佈方法包括,但不限於,旋塗、噴塗、輥塗、棒塗佈、旋轉塗佈、狹縫塗佈、壓縮塗佈、簾塗、模具式塗佈、線棒塗佈、刮刀塗佈和乾膜層壓。半導體基材可具有圓形如晶圓,或可為平板。在一些實施例中,半導體基材可為矽基材、銅基材、鋁基材、二氧化矽基材、氮化矽基材、玻璃基材、有機基材、覆銅層壓板或介電材料基材。
不希望受理論之限制,一般認為本揭示之介電膜可具有相對低的CTE。在一些實施例中,本揭示之介電膜可具有最多約100ppm/°C (如,最多約95ppm/°C、最多約90ppm/°C、最多約85ppm/°C、最多約80ppm/°C、最多約75ppm/°C、最多約70ppm/°C、最多約65ppm/°C、最多約60ppm/°C、最多約55ppm/°C或最多約50ppm/°C)及至少約15ppm/°C (如,至少約20ppm/°C、至少約30ppm/°C或至少約40ppm/°C)之在50-150°之溫度範圍內測得之CTE。
本揭示之介電膜之膜厚度沒有特別限定。在一些實施例中,該介電膜具有至少約3微米(如,至少約4微米、至少約5微米、至少約7微米、至少約10微米、至少約15微米、至少約20微米或至少約25微米)和/或最多約100微米(如,最多約80微米、最多約60微米、最多約50微米、最多約40微米或最多約30微米)之膜厚度。
在一些實施例中,該介電膜具有相對薄的膜厚度(如,最多約5微米、最多約4微米或最多約3微米)。
之後可使該介電膜曝露於輻射源或熱(如,形成一交聯膜)。用於輻射曝露之輻射之非限制性例子包括電子束、紫外線及X射線,紫外線是較佳的。典型地,可使用低壓汞燈、高壓汞燈、超高壓汞燈或鹵素燈作為輻射源。曝露劑量沒有特別限定,熟悉此技藝之人士可輕易地決定適量的量。在一些實施例中,該曝露劑量為至少約100mJ/cm2
(如,至少約200mJ/cm2
或至少約500mJ/cm2
)及最多約2,000mJ/cm2
(如,最多約1,500mJ/cm2
或最多約1,000mJ/cm2
)。假如該介電膜曝露於熱,則該加熱溫度為至少約70°C (如,至少約100°C、至少約130°C或至少約160°C)和/或最多約250°C (如,最多約220°C、最多約200°C或最多約180°C)。該加熱時間為至少約10分鐘(如,至少約20分鐘、至少約30分鐘、至少約40分鐘或至少約50分鐘)和/或最多約5個小時(如,最多約4個小時、最多約3個小時、最多約2個小時或最多約1個小時)。
在一些實施例中,本揭示之特徵為一種用於沈積金屬層(如,製造一內嵌銅線結構)之方法,其包括下列步驟: a)於一基材上沈積本揭示之介電膜形成性組成物,形成一介電膜; b)使該介電膜曝露於輻射源或熱; c)圖案化該膜(如,利用雷射剝蝕程序),形成具有開口之一圖案化介電膜;及 d)沈積一金屬(如,一導電金屬)進入該介電膜之至少一個開口中。
步驟a)及b)可與之前所述的相同。
在本揭示中所述之圖案化結構可利用雷射剝蝕程序獲得。使用準分子雷射束之直接雷射剝蝕程序,通常是一種乾式、一步驟的材料去除,在介電膜中形成開口(或圖案)。在一些實施例中,該雷射之波長為351nm或更短(如,351nm、308nm、248nm或193nm)。在一些實施例中,雷射之波長是308nm或更短。適合的雷射剝蝕程序之例子包括,但不限於,美國專利案號US7,598,167、US6,667,551及US6,114,240中所述之方法,其等之內容在此併入本案以為參考。使用習用介電膜之雷射剝蝕程序會製造出大量的碎片。此碎片之去除常需要額外的化學和/或電漿處理之清潔步驟,此會增加方法之複雜度及成本。本揭示之一重要特徵是當使用雷射剝蝕程序圖案化用本揭示之組成物製得之介電膜時,僅產生微量或不會產生碎片,此可導致較少的方法複雜度及較低的成本。一個描述碎片位準之方法是使用1至5之級別,其中1代表雷射剝蝕程序產生之碎片數量最少(無碎片),而5代表產生之碎片數量最多。如以下範例所述,雷射剝蝕處理從本揭示之介電膜形成性組成物製得之介電膜所產生之碎片最多為3 (如,最多為2或最多為1)。
本揭示之一些實施例描述一種在一半導體基材上沈積一金屬層(如,一導電銅層,形成一內嵌銅線結構)之方法。在一些實施例中,為達此目的,首先於該圖案化介電膜(如,該膜中之開口外)上沈積適形於該圖案化介電膜之一晶種層。該晶種層可含一阻障層及一金屬晶種層(如,銅晶種層)。目前揭示之重要態樣是,該阻障層及金屬晶種層可在不需使用預處理之程序(如,施以化學處理、施以電漿處理或使用外部黏合層)之情況下沈積在該圖案化介電膜上(該膜中之開口中或外),以確保該介電膜與該晶種層間良好的黏著。在一些實施例中,該阻障層是使用能夠預防導電金屬(如,銅)擴散通過該介電膜之材料形成。可用於該阻障層之適合的材料包括,但不限於,鉭(Ta)、鈦(Ti)、氮化鉭(TiN)、氮化鎢(WN)及Ta/TaN。適合用於形成該阻障層之方法是濺鍍(如,PVD或物理氣相沈積)。濺鍍沈積作為金屬沈積技術具有一些優點,因為其可用於沈積許多導電材料、具高沈積速率、具良好均一度及低成本。習用濺鍍充填在較深、較窄 (高深寬比)特徵上產生相對差的結果。藉由准直濺鍍的通量,可改善濺鍍沉積之充填因子。典型地,此可藉由於標的與基材之間***具有六角單元格之准直板達成。
該方法之下一步驟是金屬晶種沈積。為了改善在接下來的步驟中形成金屬層(如,銅層)的沈積,於該阻障層上形成一薄金屬(如,導電金屬,如銅)晶種層。
該方法之下一步驟是於該圖案化介電膜之開口中之金屬晶種層上沈積一導電金屬層(如,銅層),其中該金屬層夠厚,能夠充填該圖案化介電膜中之開口。用於充填該圖案化介電層中之開口之金屬層,可利用電鍍(諸如,無電式或電解電鍍)、濺鍍、電漿氣相沈積(PVD)及化學氣相沈積(CVD)進行沈積。電化學沈積通常是施用銅之較佳的方法,因為其比其它沈積方法經濟且可完美地將銅充填進入互連特徵中。銅沈積方法一般應可符合半導體產業嚴苛的要求。例如,銅沈積應該是均一的且能夠完美地充填元件之小型互連特徵,例如,100nm或更小之開口。此技術已述於如美國專利案號US5,891,804 (Havemann et al.)、US6,399,486 (Tsai et al.)、US7,303,992 (Paneccasio et al.)中,其等之內容在此併入本案以為參考。
在一些實施例中,該圖案化介電膜包括至少一種單元,其具有最大約10微米(如,最大約9微米、最大約8微米、最大約7微米、最大約6微米、最大約5微米、最大約4微米、最大約3微米、最大約2微米或最大約1微米)之特徵尺寸(如,寬度)。本揭示之一重要態樣是,由在此所述之介電膜形成性組成物製得之介電膜,在經雷射剝蝕程序處理後能夠產生特徵尺寸最大約3微米(如,最大約2微米或最大約1微米)之圖案。
在一些實施例中,本揭示之圖案化介電膜之特徵(如,最小特徵)之高寬比(高度對寬度之比)為至少約1/3 (如,至少約1/2、至少約1/1、至少約2/1、至少約3/1、至少約4/1或至少約5/1)。
在一些實施例中,沈積一導電金屬層之方法進一步包括去除超載的導電金屬或去除該晶種層(如,該阻障層及該金屬晶種層)。本發明之獨特的態樣是,該導電金屬層或該晶種層之超載最少,且可用相對簡單的方法如濕式蝕刻去除。在一些實施例中,該導電金屬層(如,銅層)之超載最多約3微米(如,最多約2.8微米、最多約2.6微米、最多約2.4微米、最多約2.2微米、最多約2.0微米或最多約1.8微米)及至少約0.4微米(如,至少約0.6微米、至少約0.8微米、至少約1微米、至少約1.2微米、至少約1.4微米或至少約1.6微米)。用於去除銅超載之銅蝕刻劑之例子,包括含氯化銅與鹽酸之水溶液或硝酸鐵與鹽酸之混合水溶液。其它適合的銅蝕刻劑之例子包括,但不限於,在美國專利案號US4,784,785、US3,361,674、US3,816,306, US5,524,780、US5,650,249、US5,431,776及US5,248,398及美國專利申請案號US2017175274中所述之銅蝕刻劑,其等之內容在此併入本案以為參考。
額外地,該晶種層(如,該阻障層及該金屬晶種層)亦可用濕式蝕刻法去除。適合用於去除鈦阻障層之鈦蝕刻劑之例子包括,但不限於,氫氟酸及硝酸與氫氟酸之組合。其它適合的鈦蝕刻劑之例子包括,但不限於,在美國專利案號US4,540,465及US8,801,958中所述之鈦蝕刻劑,其等之內容在此併入本案以為參考。用於去除鉭阻障層之鉭蝕刻劑之例子包括,但不限於,氫氧化鈉/過氧化氫之水溶液及氫氧化鉀/過氧化氫之水溶液。
圖1是顯示在圖案化介電膜上沈積導電金屬(如,銅)之習知方法之說明圖。在步驟100中,在一半導體基材上沈積一習知介電膜組成物。在步驟110中,使用雷射剝蝕程序圖案化該介電膜。在步驟120中,去除在步驟110期間所產生之碎片(如,利用使用清潔劑之化學處理或碎片去除機)。用於改善一般的介電膜與晶種層(如,包括阻障層及晶種層)間之黏著之預處理方法示於步驟130中。為了確保該介電膜與晶種層間良好的黏著,涉及化學處理或電漿處理或施用外部助黏劑之預處理方法是必需的。例如,通常是使用加熱該介電膜和過錳酸鉀與氫氧化鈉溶液之去膠渣處理,來改善該介電膜與該晶種層之黏著力。下一步,在步驟140中沈積晶種層,接著在步驟150中沈積一導電金屬。在步驟160中進行化學機械拋光(CMP)以去除任何超載的導電金屬。最後在步驟170中進行後CMP清潔,以獲得具有內嵌導電金屬線之半導體結構。
圖2是顯示本揭示之例示性發明方法之說明圖。如圖2所示,於步驟200中,可藉由於一半導體基材上沈積在此所述之介電膜形成性組成物而形成本揭示之發明介電膜。在步驟210中,可使用雷射剝蝕程序圖案化此塗佈的介電膜,其產生微量或不會產生碎片。在步驟220中,可在無任何碎片去除程序或任何預處理程序之情況下,直接在該介電膜上沈積一晶種層(如,包括一阻障層及一晶種層),接著在步驟230中沈積一導電金屬(如,銅)沈積。最後,在步驟240中,可進行一濕式蝕刻處理去除任何超載的導電金屬或該晶種層,完成該方法,獲得具有內嵌導電金屬線之一半導體基材。
在一些實施例中,本揭示之特徵為一種三維物件,其含有至少一種通過在此所述之方法形成之圖案化膜。在一些實施例中,該三維物件可包括至少二個疊層(如,至少三個疊層)之圖案化膜。此物件之例子包括半導體基材、電子產品之可撓性膜、導線絕緣層、導線塗層、導線漆或著墨基材。在一些實施例中,本揭示之特徵為一半導體元件,其包括此等三維物件中之一或多種。此半導體元件之例子包括積體電路、發光二極體、太陽能電池及電晶體。
在此所引述之所有的公開文獻(如,專利、專利申請公開案及文件)之全部在此併入本案以為參考。
將參考下列範例更詳細地說明本揭示,其等為例示性目的,不應被解釋成本揭示之範疇限制。範例
除非有特別說明,否則列出之任何的百分比均為重量百分比(重量%)。合成範例1 (P-1) 6FDA/DAPI 聚醯亞胺 之製備
將固態4,4'-(六氟異亞丙基)雙(鄰苯二甲酸酐) (6FDA) (2.370kg,5.33莫耳)裝入配製於25°C NMP (9.86kg)中之1-(4-胺苯基)-1,3,3-三甲基二氫茚-5-胺(亦稱作4,4'-[1,4-伸苯基-雙(1-甲基亞乙基)]二苯胺(DAPI)) (1.473kg,5.51莫耳)溶液中。將反應溫度提高至40°C,令混合物反應6個小時。接著加入醋酸酐(1.125kg)及吡啶(0.219kg),且將反應溫度提高至100°C,並使其反應12個小時。
使以上之反應混合物冷卻至室溫,然後將其轉移至設有機械攪拌器之較大容器中。用醋酸乙酯稀釋該反應溶液,然後用水清洗1個小時。攪拌停止後,使該混合物靜置不受干擾。一旦發生相分離,則去除水相。用醋酸乙酯與丙酮之組合稀釋該有機相,然後用水清洗二次。在所有的清洗中所使用之有機溶劑(醋酸乙酯與丙酮)與水之量示於表1中。表1
於該經清洗的有機相中加入環戊酮(10.5kg),然後利用真空蒸餾濃縮該溶液,得到聚合物溶液P-1。最後聚合物之固體%為32.96%,經GPC測得之重量平均分子量(Mw)為49,200道爾頓。製備介電形成性組成物之一般程序
利用機械攪拌聚合物(P-1)、適量的甲基丙烯醯氧基三甲氧基矽烷、NCI-831 (商品名,可得自ADEKA公司)、鈦四(丙烯酸羧乙酯) (MCA,60重量%配製於正丁醇中)、二氧化矽、環己酮與交聯劑之混合物,製備範例1–6及比較例1之介電膜形成性組成物。機械攪拌24個小時之後,在沒有過濾之情況下使用該溶液。此等範例之組成示於表2中。表2
*聚醯亞胺聚合物、MCA及二氧化矽之量作為100%固體。 **交聯劑1 (CL-1)為CN 992 (商品名,可得自Arkema – Sartomer)、交聯劑2 (CL-2)是四乙二醇二丙烯酸酯,而交聯劑3 (CL-3)為三甲醇丙烷三丙烯酸酯雷射剝蝕程序之一般程序
將各介電膜形成性組成物旋塗在矽晶圓上,然後使用熱板在95°C下烘烤10分鐘,形成一塗層。然後使用寬帶UV曝光工具(Carl Süss MA-56),以500mJ/cm2
對該膜進行整面曝光,且在170°C下烘烤2個小時,形成厚度約6至9微米之膜。使用XeCl雷射之雷射剝蝕程序,在波長308nm、頻率100Hz下圖案化該膜。各案例之雷射剝蝕過程所產生之碎片示於表3之範例7-12及比較例2中。表3
在範例7–12中,範例1至6之組成物(其等全部具有完全醯亞胺化的聚醯亞胺聚合物及MCA),在雷射剝蝕處理後,產生微量或沒有產生碎片(即,具3或更低之碎片評級)。相反的,在比較例2中,比較例1之組成物(其是不含MCA之習知介電膜形成性組成物),在雷射剝蝕處理後,產生大量的碎片(即,碎片級別5)。
在表3中,根據聚醯亞胺聚合物及MCA於總固體中之百分比,計算此等二種化合物之量。該總固體之重量定義為,介電膜形成性組成物之總重量減去此組成物溶劑之總重量。範例13 :雷射剝蝕及阻障層之沈積
雷射剝蝕範例2之介電膜形成性組成物,在6.2微米膜上產生2x2微米(線寬/線距)之解析度(如,高寬比= 6.2/2或3.1)。因為在雷射剝蝕處理期間形成微量或沒有形成碎片,所以在沈積阻障層之前,不需要碎片去除步驟或預處理程序。
使用濺鍍技術在該圖案化膜上沈積阻障層(鈦)。該沈積係使用Denton Vacuum Desktop設備,以56mA之電流進行。16分鐘內形成具有26nm厚之鈦阻障層。範例14 :銅晶種層之沈積
使用相同的濺鍍工具,在以上阻障層上沈積銅晶種層。在50mA之電流下,60分鐘內形成420nm厚之銅晶種層。範例15 :銅層之沈積
在設計供不同尺寸之晶圓用之電鍍設備中進行電鍍。整流器形式之電源(其會將交流電轉換成固定的低壓DC電流)提供必須的電流。電鍍前,用10% H2
SO4
清洗以上獲得之工作件(晶圓),接著用去離子水潤洗。將浸在電鍍浴(主成份:3%甲磺酸及5% CuSO4
.5H2
O,配製於去離子水中作為電解質)中之電極連接至DC電流源之輸出。待電鍍的晶圓作為帶負電之陰極。帶正電的陽極接通電路。使電鍍浴維持在25°C下,同時以每分鐘6加侖之速率再循環電解質。為維持銅沈積之均一度,該單元設計成具有適當***物之擋板。當電流維持在4.4安培,電壓維持在8.8伏特時,銅以每分鐘1微米之速率沈積。銅超載為2微米。範例16 :銅超載與鈦阻障層之去除
銅蝕刻劑之製備,首先製備90%去離子水與10%氯化銅之混合物,接著藉由添加鹽酸將pH調整至1。將以上獲得之晶圓浸入銅蝕刻劑中,以致在室溫下20分鐘後去除2微米的銅超載。鈦蝕刻劑之製備是藉由摻合98.994%去離子水、1%氫氟酸及0.006%聚乙烯亞胺(MW為200道爾頓)而製得。將以上所獲得之晶圓浸入鈦蝕刻劑中,以致在室溫下1分鐘內去除該阻障層(26nm)。獲得具有內嵌銅線結構之晶圓。比較例3 :碎片之去除
雷射剝蝕從比較例1之組成物形成之介電膜,在11微米膜上產生8x8微米(線寬/線距)之解析度(如,高寬比=11/8或1.4)。產生大量的碎片。因此,在阻障層沈積之前需先去除碎片。使用由2.5重量%之四甲基氫氧化銨(TMAH)、7.5重量%之去離子水、0.5重量%之硫酸胲、4.3重量%之單甲醇胺、85重量%之四氫糠醇及0.2重量%之5-甲基-1H-苯並***之碎片去除組成物。將此碎片去除組成物加熱至60°C,然後將該晶圓浸入該碎片去除組成物中歷時5分鐘處理該晶圓。用水清洗該晶圓然後乾燥。此處理後,碎片完成去除。比較例4 :阻障層之沈積
使用濺鍍技術在比較例3之圖案化膜上形成阻障層(鈦)。該沈積係使用Denton Vacuum Desktop設備,以56mA之電流進行。16分鐘內形成具有26nm厚之鈦阻障層。比較例5 :銅晶種層之沈積
使用相同的濺鍍工具,在以上之阻障層上沈積銅晶種層。在50mA之電流下,60分鐘內形成420nm厚之銅晶種層。比較例6 :銅層之沈積
以在範例15中所述相同之方法進行電鍍,但進行較長的時間。銅超載為20微米。比較例7 :利用CMP 及後CMP 清潔程序去除銅超載及鈦阻障層
使用CMP程序去除銅超載。在Mirra AMAT拋光器上使用銅粗漿料,漿料流速為175mL/min。CMP處理之總時間為10分鐘。此拋光步驟完成時,在酸性清潔液中清洗晶圓,其可去除有機殘留物以及卡在晶圓表面上之粒子。
接著,用比該粗漿料更能機械驅動之銅阻障漿料去除鈦阻障層,使能有效去除此層。在第二酸性清潔液中清潔該晶圓,其去除有機殘留物及卡在晶圓表面上之粒子。範例17 :範例1 之介電膜形成性組成物之吸光度測量
將範例1之介電膜形成性組成物旋塗在3.0微米厚的透明4“玻璃晶圓上,並在95℃下軟烘180秒。使用CARY 400 Conc. UV-可見光分光光度計,在範圍從300至405nm之波長下測量此自立乾膜之吸光度。此膜在308nm下之吸光度為0.383µm-1
,在355nm下為0.125µm-1
,在365nm下為0.127µm-1
及在405nm下為0.058µm-1
。範例18 :介電膜形成性組成物
使用339.00g之聚合物(P-1)、18.00g之甲基丙烯醯氧基丙基三甲氧基矽烷、10.80g之OXE-01 (商品名,可得自BASF SE)、114.00g之鈦四(丙烯酸羧乙酯) (60重量%,配製於正丁醇中)、340.11g之環己酮、126.00g之可得自Arkema – Sartomer之四乙二醇二丙烯酸酯及252.0g之胺基甲酸乙酯丙烯酸酯(商品名CN 992,可得自Arkema – Sartomer),製備範例18之介電膜形成性組成物。機械攪拌24個小時之後,使用0.2微米之濾器過濾該組成物。範例19 :乾膜範例1 (DF-1)
使用Fujifilm USA (Greenwood, SC)之狹縫模頭塗佈器,以2呎/分(每分鐘60cm)之直線速度,用30微米微型條棒間隔,將範例18之經過濾的介電膜形成性組成物施塗於20.2吋寬、35微米厚作為載體基材之聚對苯二甲酸乙二酯(PET)膜(Hostaphan 3915,Mitsubishi Polyester Film, Inc.製)上,然後在197°F下乾燥,獲得厚度大約為10.0微米之介電層。在此介電層上,利用輥壓覆蓋一具有20.2吋寬、20微米厚之雙軸取向聚丙烯膜(BOPP,Mirwec Film Inc., Bloomington, IN製,商品名BOPLON),作為保護層。範例20 :介電膜形成性組成物
使用470.98g之聚合物(P-1)、15.00g之甲基丙烯醯氧基丙基三甲氧基矽烷、9.00g之NCI-831 (商品名,可得自ADEKA公司)、175.00g之鈦四(丙烯酸羧乙酯) (60重量%,配製於正丁醇中)、289.04g之環己酮、141.00g之可得自Arkema–Sartomer之四乙二醇二丙烯酸酯、750g之分散於環己酮中之20%二氧化矽及150.00g之胺基甲酸乙酯丙烯酸酯(商品名CN 992,可得自Arkema–Sartomer),製備範例20之介電膜形成性組成物。機械攪拌24個小時之後,在沒有過濾之情況下使用該溶液。範例21 :乾膜範例2 (DF-2)
使用Fujifilm USA (Greenwood, SC)之狹縫模頭塗佈器,以2呎/分(每分鐘60cm)之直線速度,用30微米微型條棒間隔,將範例20之未經過濾的介電膜形成性組成物施塗於20.2吋寬、35微米厚作為載體基材之聚對苯二甲酸乙二酯(PET)膜(Hostaphan 3915,Mitsubishi Polyester Film, Inc.製)上,然後在197°F下乾燥,獲得厚度大約為10.0微米之介電層。在此介電層上,利用輥壓覆蓋一具有20.2吋寬、20微米厚之雙軸取向聚丙烯膜(BOPP,Mirwec Film Inc., Bloomington, IN製,商品名BOPLON),作為一保護層。預測範例22 :介電膜形成性組成物
使用28.00g之聚合物(聚-1)、46.88g之環戊酮、80.00g之環己酮、0.84g之N-(3-三甲氧矽基丙基)吡咯、1.40g之1-(O-乙醯肟)-1-[9-乙基-6-(2-甲基苯甲醯基)-9H-咔唑-3-基]乙酮(OXE-02,可得自BASF)、6.20g之鉿四羧乙基丙烯酸酯、11.00g之平均粒徑0.45微米之二氧化鈦、14g之三乙二醇二甲基丙烯酸酯、17.50g之CN992 (可得自Sartomer)、0.84g之配置於環戊酮中之0.05% Polyfox 6320溶液及0.07g之對苯醌,製備配方範例22。機械攪拌24個小時之後,在沒有過濾之情況下使用該配方。預測範例23 :介電膜形成性組成物
使用26.00g之聚合物(聚-1)、47.00g之環戊酮、75.00g之環己酮、0.80g之N-(3-三乙氧基矽基丙基)-4,5-二氫咪唑、01.50g之過氧化苯甲醯、7.50g之丁醇鋯三(甲基)丙烯酸酯、17.0g之四乙二醇二丙烯酸酯(SR-209,可得自Sartomer)、14.00g之新戊四醇三丙烯酸酯、0.72g之配製於環戊酮中之0.05% Polyfox 6320溶液及0.05g之對-苯醌,製備配方範例23。機械攪拌30個小時後,在沒有過濾之情況下使用該配方。
100、110、120、130、140、150、160、170、200、210、220、230、240‧‧‧步驟
圖1是在圖案化介電膜上沈積銅之習用方法之說明圖。
圖2是本揭示之例示性發明方法之說明圖。
Claims (44)
- 一種介電膜形成性組成物,其包含: a)至少一種完全醯亞胺化的聚醯亞胺聚合物; b)至少一種含金屬的(甲基)丙烯酸酯; c)至少一種催化劑;及 d)至少一種溶劑。
- 如請求項1之組成物,其中該至少一種含金屬的(甲基)丙烯酸酯之金屬原子係選自於由鈦、鋯、鉿及鍺所構成之群組。
- 如請求項1之組成物,其中該至少一種含金屬的(甲基)丙烯酸酯包含至少一個金屬原子及至少一個(甲基)丙烯酸酯基團。
- 如請求項1之組成物,其中該至少一種含金屬的(甲基)丙烯酸酯包含四(甲基)丙烯酸鈦、四(甲基)丙烯酸鋯、四(甲基)丙烯酸鉿、丁醇鈦三(甲基)丙烯酸酯、二丁醇鈦二(甲基)丙烯酸酯、三丁醇鈦(甲基)丙烯酸酯、丁醇鋯三(甲基)丙烯酸酯、二丁醇鋯二(甲基)丙烯酸酯、三丁醇鋯(甲基)丙烯酸酯、丁醇鉿三(甲基)丙烯酸酯、二丁醇鉿二(甲基)丙烯酸酯、三丁醇鉿(甲基)丙烯酸酯、鈦四(羧乙基(甲基)丙烯酸酯)、鋯四(羧乙基(甲基)丙烯酸酯)、鉿四(羧乙基(甲基)丙烯酸酯)、丁醇鈦三(羧乙基(甲基)丙烯酸酯)、二丁醇鈦二(羧乙基(甲基)丙烯酸酯)、三丁醇鈦(羧乙基(甲基)丙烯酸酯)、丁醇鋯三(羧乙基(甲基)丙烯酸酯)、二丁醇鋯二(羧乙基(甲基)丙烯酸酯)、三丁醇鋯(羧乙基(甲基)丙烯酸酯)、丁醇鉿三(羧乙基(甲基)丙烯酸酯)、二丁醇鉿二(羧乙基(甲基)丙烯酸酯)或三丁醇鉿(羧乙基(甲基)丙烯酸酯)。
- 如請求項1之組成物,其中該至少一種含金屬的(甲基)丙烯酸酯之量為該組成物之約0.5重量%至約20重量%。
- 如請求項1之組成物,其中該至少一種完全醯亞胺化的聚醯亞胺聚合物之量為該組成物之約3重量%至約40重量%。
- 如請求項1之組成物,其中該至少一種催化劑包含一光引發劑或一熱引發劑。
- 如請求項1之組成物,其中該至少一種催化劑之量為該組成物之約0.25重量%至約4重量%。
- 如請求項1之組成物,其中該至少一種溶劑之量為該組成物之約35重量%至約98重量%。
- 如請求項1之組成物,其進一步包含至少一種交聯劑。
- 如請求項10之組成物,其中該交聯劑包含二或多個烯基或炔基基團。
- 如請求項1之組成物,其進一步包含至少一種填料。
- 如請求項12之組成物,其中該至少一種填料包含選自於由下列所構成之群組之一無機粒子:二氧化矽、氧化鋁、二氧化鈦、氧化鋯、氧化鉿、CdSe、CdS、CdTe、CuO、氧化鋅、氧化鑭、氧化鈮、氧化鎢、氧化鍶、氧化鈣鈦、鈦酸鈉、硫酸鋇、鈦酸鋇、鋯酸鋇及鈮酸鉀。
- 如請求項1之組成物,其中該組成物形成一介電膜,當藉由雷射剝蝕程序圖案化該介電膜時,其實質上不產生碎片。
- 一種由請求項1之組成物形成之介電膜。
- 一種介電膜,其包含: a)至少一種完全醯亞胺化的聚醯亞胺聚合物; b)至少一種含金屬的(甲基)丙烯酸酯;及 c)至少一種催化劑。
- 如請求項16之介電膜,其中該介電膜是一自立介電膜。
- 一種用於沈積一導電金屬層之方法,其包含: a) 於一基材上沈積如請求項1之組成物,以形成一介電膜; b)使該介電膜曝露於輻射源或熱; c) 圖案化該介電膜,以形成具有開口之一圖案化介電膜;及 d)於該圖案化介電膜上沈積一晶種層;及 e) 於該圖案化介電膜之至少一個開口中沈積一導電金屬層。
- 如請求項18之方法,其進一步包含去除超載的導電金屬或去除該晶種層。
- 如請求項18之方法,其中該去除超載的導電金屬或去除該晶種層係藉由濕式蝕刻進行。
- 如請求項18之方法,其中使該介電膜曝露於輻射源或熱,包含在約70°C至約250°C之溫度下加熱該介電膜。
- 如請求項18之方法,其中該圖案化該介電膜係藉由雷射剝蝕程序進行。
- 如請求項22之方法,其中該雷射剝蝕程序實質上不產生碎片。
- 如請求項18之方法,其中該圖案化介電膜包含至少一種單元,其具有最大約3微米之特徵尺寸。
- 如請求項18之方法,其中該導電金屬層包含銅。
- 如請求項19之方法,其中該超載具最多約2微米的厚度。
- 如請求項18之方法,其中在沒有使用碎片去除程序或預處理程序之情況下,沈積該晶種層。
- 如請求項18之方法,其中該方法不包括用於處理一導電金屬超載之化學機械平坦化程序或後化學機械平坦化清潔程序。
- 一種三維物件,其是由請求項18之方法形成。
- 一種半導體元件,其包含請求項29之三維物件。
- 如請求項30之半導體元件,其中該半導體元件是積體電路、發光二極體、太陽能電池或電晶體。
- 一種用於製備一乾膜結構之方法,其包含: (A)用請求項1之介電膜形成性組成物塗佈一載體基材,以形成一塗佈組成物; (B)乾燥該塗佈組成物,以形成一介電膜;及 (C)任擇地於該介電膜上施用一保護層。
- 一種用於沈積一導電金屬層之方法,其包含: a)在一基材上形成一感光介電膜; b)使該介電膜曝露於輻射源或熱; c)圖案化該介電膜,以形成具有開口之一圖案化介電膜; d)在該圖案化介電膜上沈積一晶種層;及 e)在該圖案化介電膜之至少一個開口中沈積一導電金屬層,其中沈積一導電金屬層形成具有厚度最多約2微米之導電金屬超載。
- 如請求項33之方法,其進一步包含去除該導電金屬超載或去除該晶種層。
- 如請求項34之方法,其中去除該導電金屬超載或去除該晶種層係利用濕式蝕刻進行。
- 如請求項33之方法,其中該使該介電膜曝露於輻射源或熱,包含在約70°C至約250°C之溫度下加熱該介電膜。
- 如請求項33之方法,其中該圖案化該介電膜是藉由雷射剝蝕程序進行。
- 如請求項37之方法,其中該雷射剝蝕程序實質上不產生碎片。
- 如請求項33之方法,其中該圖案化介電膜包含至少一種單元,其具有最大約3微米之特徵尺寸。
- 如請求項33之方法,其中該導電金屬層包含銅。
- 如請求項33之方法,其中在沒有使用碎片去除程序或預處理程序之情況下,沈積該晶種層。
- 如請求項33之方法,其中該方法不包括用於處理任一導電金屬超載之化學機械平坦化程序或後化學機械平坦化程序。
- 一種介電膜,其包含: a)至少一種完全醯亞胺化的聚醯亞胺聚合物;及 b) 至少一種經交聯之含金屬的(甲基)丙烯酸酯。
- 如請求項43之介電膜,其中該介電膜為一自立介電膜。
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TWI753657B (zh) * | 2020-11-17 | 2022-01-21 | 位速科技股份有限公司 | 鈣鈦礦光電元件 |
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WO2019050565A1 (en) | 2019-03-14 |
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TW201912717A (zh) | 2019-04-01 |
EP3478482A1 (en) | 2019-05-08 |
EP3478482A4 (en) | 2019-07-17 |
CN109790405A (zh) | 2019-05-21 |
US10563014B2 (en) | 2020-02-18 |
PH12018550157A1 (en) | 2019-09-09 |
EP3478777B1 (en) | 2020-11-18 |
PH12018550158A1 (en) | 2019-09-09 |
EP3478777A1 (en) | 2019-05-08 |
JP7140687B2 (ja) | 2022-09-21 |
TWI766959B (zh) | 2022-06-11 |
JP7140686B2 (ja) | 2022-09-21 |
US20190077913A1 (en) | 2019-03-14 |
CN109790405B (zh) | 2022-07-15 |
EP3478482B1 (en) | 2020-12-16 |
KR102456361B1 (ko) | 2022-10-19 |
CN109789644B (zh) | 2023-01-31 |
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