CN103492499A - Silica-coating-forming composition for use with inkjets, method for forming silica coating, semiconductor device, and solar-cell system - Google Patents
Silica-coating-forming composition for use with inkjets, method for forming silica coating, semiconductor device, and solar-cell system Download PDFInfo
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- CN103492499A CN103492499A CN201280019477.3A CN201280019477A CN103492499A CN 103492499 A CN103492499 A CN 103492499A CN 201280019477 A CN201280019477 A CN 201280019477A CN 103492499 A CN103492499 A CN 103492499A
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- Prior art keywords
- solvent
- silica
- butyrolactone
- composition
- gamma
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- Pending
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- 239000000203 mixture Substances 0.000 title claims abstract description 97
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 168
- 239000000377 silicon dioxide Substances 0.000 title claims description 83
- 238000000034 method Methods 0.000 title claims description 35
- 239000004065 semiconductor Substances 0.000 title claims description 23
- 238000000576 coating method Methods 0.000 title description 7
- 239000011248 coating agent Substances 0.000 title description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims abstract description 162
- 239000002904 solvent Substances 0.000 claims abstract description 129
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 73
- 238000009835 boiling Methods 0.000 claims abstract description 66
- 150000001875 compounds Chemical class 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 19
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 125000004432 carbon atom Chemical group C* 0.000 claims description 12
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims description 12
- 238000006068 polycondensation reaction Methods 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 10
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 125000000962 organic group Chemical group 0.000 claims description 4
- -1 gamma-butyrolactone Chemical class 0.000 abstract description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 51
- 229920002050 silicone resin Polymers 0.000 description 49
- 239000007787 solid Substances 0.000 description 45
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 41
- 238000003756 stirring Methods 0.000 description 35
- MTHSVFCYNBDYFN-UHFFFAOYSA-N anhydrous diethylene glycol Natural products OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 30
- WGYZMNBUZFHYRX-UHFFFAOYSA-N 1-(1-methoxypropan-2-yloxy)propan-2-ol Chemical compound COCC(C)OCC(C)O WGYZMNBUZFHYRX-UHFFFAOYSA-N 0.000 description 28
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 24
- 238000007639 printing Methods 0.000 description 23
- 239000012046 mixed solvent Substances 0.000 description 20
- 238000007599 discharging Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 18
- ZMYXZXUHYAGGKG-UHFFFAOYSA-N propoxysilane Chemical compound CCCO[SiH3] ZMYXZXUHYAGGKG-UHFFFAOYSA-N 0.000 description 16
- 239000007921 spray Substances 0.000 description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Natural products CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 15
- 229910000077 silane Inorganic materials 0.000 description 15
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 13
- 235000019439 ethyl acetate Nutrition 0.000 description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 13
- 238000009736 wetting Methods 0.000 description 12
- 208000037656 Respiratory Sounds Diseases 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- AUEJBKCWXPYRGZ-UHFFFAOYSA-N 1,1'-biphenyl diethoxysilane Chemical compound C(C)O[SiH2]OCC.C1(=CC=CC=C1)C1=CC=CC=C1 AUEJBKCWXPYRGZ-UHFFFAOYSA-N 0.000 description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 9
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 9
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 8
- 238000004821 distillation Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- LVTJOONKWUXEFR-FZRMHRINSA-N protoneodioscin Natural products O(C[C@@H](CC[C@]1(O)[C@H](C)[C@@H]2[C@]3(C)[C@H]([C@H]4[C@@H]([C@]5(C)C(=CC4)C[C@@H](O[C@@H]4[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@@H](O)[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@H](CO)O4)CC5)CC3)C[C@@H]2O1)C)[C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1 LVTJOONKWUXEFR-FZRMHRINSA-N 0.000 description 8
- BPIUIOXAFBGMNB-UHFFFAOYSA-N 1-hexoxyhexane Chemical compound CCCCCCOCCCCCC BPIUIOXAFBGMNB-UHFFFAOYSA-N 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- 238000013019 agitation Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 7
- 239000006200 vaporizer Substances 0.000 description 7
- 229940126062 Compound A Drugs 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 239000003377 acid catalyst Substances 0.000 description 6
- 125000003545 alkoxy group Chemical group 0.000 description 6
- MNFGEHQPOWJJBH-UHFFFAOYSA-N diethoxy-methyl-phenylsilane Chemical compound CCO[Si](C)(OCC)C1=CC=CC=C1 MNFGEHQPOWJJBH-UHFFFAOYSA-N 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 5
- 238000005336 cracking Methods 0.000 description 5
- HCOKJWUULRTBRS-UHFFFAOYSA-N propan-2-yloxysilane Chemical compound CC(C)O[SiH3] HCOKJWUULRTBRS-UHFFFAOYSA-N 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 238000000059 patterning Methods 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 3
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- 150000002170 ethers Chemical class 0.000 description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
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- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
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- 238000000206 photolithography Methods 0.000 description 3
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- LEEANUDEDHYDTG-UHFFFAOYSA-N 1,2-dimethoxypropane Chemical compound COCC(C)OC LEEANUDEDHYDTG-UHFFFAOYSA-N 0.000 description 2
- QMGJMGFZLXYHCR-UHFFFAOYSA-N 1-(2-butoxypropoxy)butane Chemical compound CCCCOCC(C)OCCCC QMGJMGFZLXYHCR-UHFFFAOYSA-N 0.000 description 2
- KZVBBTZJMSWGTK-UHFFFAOYSA-N 1-[2-(2-butoxyethoxy)ethoxy]butane Chemical compound CCCCOCCOCCOCCCC KZVBBTZJMSWGTK-UHFFFAOYSA-N 0.000 description 2
- CNJRPYFBORAQAU-UHFFFAOYSA-N 1-ethoxy-2-(2-methoxyethoxy)ethane Chemical compound CCOCCOCCOC CNJRPYFBORAQAU-UHFFFAOYSA-N 0.000 description 2
- OJVAMHKKJGICOG-UHFFFAOYSA-N 2,5-hexanedione Chemical compound CC(=O)CCC(C)=O OJVAMHKKJGICOG-UHFFFAOYSA-N 0.000 description 2
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- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
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- 229940011051 isopropyl acetate Drugs 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 229960004232 linoleic acid Drugs 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- IMXBRVLCKXGWSS-UHFFFAOYSA-N methyl 2-cyclohexylacetate Chemical compound COC(=O)CC1CCCCC1 IMXBRVLCKXGWSS-UHFFFAOYSA-N 0.000 description 1
- 229940057867 methyl lactate Drugs 0.000 description 1
- JYVLIDXNZAXMDK-UHFFFAOYSA-N methyl propyl carbinol Natural products CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 description 1
- QAUVQFQRFPDWFD-UHFFFAOYSA-N methyl-phenyl-di(propan-2-yloxy)silane Chemical compound CC(C)O[Si](C)(OC(C)C)C1=CC=CC=C1 QAUVQFQRFPDWFD-UHFFFAOYSA-N 0.000 description 1
- RXTNIJMLAQNTEG-UHFFFAOYSA-N methylamyl acetate Natural products CCCCC(C)OC(C)=O RXTNIJMLAQNTEG-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 229940017144 n-butyl lactate Drugs 0.000 description 1
- PZYDAVFRVJXFHS-UHFFFAOYSA-N n-cyclohexyl-2-pyrrolidone Chemical compound O=C1CCCN1C1CCCCC1 PZYDAVFRVJXFHS-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229960002969 oleic acid Drugs 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 1
- GXOHBWLPQHTYPF-UHFFFAOYSA-N pentyl 2-hydroxypropanoate Chemical compound CCCCCOC(=O)C(C)O GXOHBWLPQHTYPF-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229960004274 stearic acid Drugs 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-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
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1868—Passivation
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
-
- 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
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Manufacturing & Machinery (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
- Paints Or Removers (AREA)
- Photovoltaic Devices (AREA)
- Formation Of Insulating Films (AREA)
Abstract
The present invention relates to a silica-coating-forming composition for use with inkjets, said composition containing the following: a silicon compound; solvent including gamma-butyrolactone, a second solvent having a boiling point of 80 DEG C to 100 DEG C, and a third solvent having a boiling point of 180 DEG C to 230 DEG C; and a surface conditioner. Gamma-butyrolactone constitutes at least 20% of the total mass of the solvents, and the second solvent constitutes 20% to 50% of the total mass of the solvents.
Description
Technical field
The present invention relates to ink-jet and form formation method, semiconductor devices and the solar cell system of composition, silica-based film with silica-based film.
Background technology
Silica-based film, due to excellences such as insulativity, thermotolerance, the transparency and wear resistants, therefore is suitable in various fields.For example,, in semiconductor devices, for the consideration of insulativity, thermotolerance and block; be applicable to the purposes such as insulating film, element isolation film and mask material of wiring closet; in liquid crystal apparatus, for the consideration of insulativity, thermotolerance and the transparency, be applicable to the purposes such as protective membrane of element.
In the past, as the general method that obtains silica-based film, known had vapor growth method and a coating method.At semiconductor applications, vapor growth method extensively adapts to, and has and can obtain the fine and close specialities such as silica-based film.But, the maximization that needs special device, be accompanied by processing base material is in recent years arranged and the problems such as installation cost increase.On the other hand, coating method have can be easier the device film forming, to the film forming of large-scale base material also than the speciality such as being easier to.As coating method, can enumerate spin coating, spraying, pickling process, rolling method and silk screen print method etc.
Yet, as the method for the silica-based film that forms patterning, photolithography becomes main flow.But, adopted photolithographic patterning that complex procedures, the high such shortcoming of cost are arranged.Therefore, in recent years, as can the easy method that forms at an easy rate pattern, have studied ink jet method (patent documentation 1).Ink jet method can form in desired position desired pattern, therefore without as photolithography, on whole of substrate, forming silica-based film, can greatly cut down the quantity of material of use, thus the cost aspect might as well, the environment aspect might as well have great advantage.
As the method that obtains silica-based film corresponding to ink-jet and form composition, known have using the sol-gel method (patent documentation 2,3) of organoalkoxysilane as raw material.
The prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2001-279134 communique
Patent documentation 2: TOHKEMY 2009-239983 communique
Patent documentation 3: TOHKEMY 2009-253127 communique
Summary of the invention
The problem that invention will solve
But, as patent documentation 2 is put down in writing, while as solvent, using ethanol or water, or as patent documentation 3 is put down in writing, account for while forming 70～90 all quality % at the solvent below 100 ℃, repeat the operation of not discharging and discharging that ink-jet is described, easily cause spray nozzle clogging.During volume production, owing to repeating such discharge and not discharging, it is also insufficient as supplying practical product that described silica-based film in the past forms composition.
In addition, the silica-based film corresponding for ink-jet forms composition, while using it to describe pattern, expects that the cross-sectional shape of describing pattern is rectangle or approaches rectangle.For example, while with such silica-based film formation composition, forming insulating film, if the patterned section shape is not rectangle (that is, the thickness of insulating film reduces in the film edge), insulativity can reduce partly, consequently sometimes makes device characteristics reduce.
Further, silica-based film corresponding to ink-jet forms composition sometimes as mask material.Now, the thickness of mask material is thin, can not obtain sufficient mask, therefore need to be by the thickness increase to a certain degree.But, when intention increases thickness, after by spin-coating method or ink jet method etc., to coating silica-based film on substrate, forming composition, make, in its Procuring or curing process, sometimes to crack.Localized cracks in the coating part face makes device characteristics reduce sometimes, and therefore expectation does not produce.
In this wise, the silica-based film corresponding for ink-jet forms composition, require: even repeat the operation of not discharging and discharging, inkjet nozzle also can not produce with stopping up and be discharged, can form in addition the pattern of describing with cross-sectional shape of more approaching rectangle, even further increase the thickness of describing pattern, in Procuring and while solidifying, do not crack yet.Therefore, need to contain silica-based film and form the non-drying property of the printing ink of composition in spray nozzle front end section, and the inhibition of drop wettability during to land, even further increase the resistance to cracking line that thickness does not also crack.Yet it is very difficult all meeting these characteristics.
The object of the invention is to, provide a kind of ink-jet to form composition with silica-based film, even its operation that repeats not discharge and discharge also can not produce the obstruction ground of inkjet nozzle and be discharged, can form in addition the pattern of describing with cross-sectional shape of more approaching rectangle, even and increase the thickness of describing pattern and also can suppress the generation of crackle.The present invention also aims to provide a kind of formation method, semiconductor devices and solar cell system that has used the silica-based film of said composition.
For the scheme of dealing with problems
In order to solve foregoing problems, the invention provides the ink-jet following (1) and (2) put down in writing and form with silica-based film the solar cell system that the formation method of the silica-based film that composition, following (3) put down in writing, semiconductor devices that following (4) are put down in writing and following (5) are put down in writing.
(1) a kind of ink-jet forms composition with silica-based film, and it contains silicon compound, solvent and surface conditioner,
The silicon compound of described silicon compound for following monomer component hydrolysis, polycondensation are obtained, described monomer component contains:
General formula (I): PhSiX
3the compound meaned, in formula, Ph means also can have substituent phenyl, X means hydrolization group, the X of a plurality of existence can be identical also can be different,
General formula (II): R
1 nsiX
4-nthe compound meaned, in formula, R
1mean the alkyl of carbonatoms 1～20, X means hydrolization group, and n means 0 or 1 integer, the X of a plurality of existence can be identical also can be different, and
General formula (III): R
2 2siX
2the compound meaned, in formula, R
2mean the organic group of carbonatoms 1～20, X means hydrolization group, the R of a plurality of existence
2and X separately can be identical also can be different;
Described solvent contains the 3rd solvent that the second solvent that gamma-butyrolactone, boiling point are 80～100 ℃ and boiling point are 180～230 ℃,
With respect to the total mass of solvent, the mass ratio of described gamma-butyrolactone is more than 0.2, and with respect to the total mass of described solvent, the mass ratio of described the second solvent is 0.2～0.5.
(2) composition as described as (1), wherein, described surface conditioner is the silicone-based surface conditioner.
(3) a kind of formation method of silica-based film, it possesses:
Discharge (1) or (2) described composition by ink jet method and carry out pattern plotter, form the operation of describing pattern film, and
Make to describe the curing operation of pattern film.
(4) a kind of semiconductor devices, it possesses:
Substrate, and
The silica-based film formed by (3) described method on this substrate.
(5) a kind of solar cell system, it possesses (4) described semiconductor devices.
The invention effect
According to the present invention, provide a kind of ink-jet to form composition with silica-based film, even its operation that repeats not discharge and discharge also can not produce the obstruction ground of inkjet nozzle and be discharged, can form in addition the pattern of describing with cross-sectional shape of more approaching rectangle, even and increase the thickness of describing pattern also can suppress Procuring and solidify after the generation of crackle.According to the present invention, provide formation method, semiconductor devices and the solar cell system of the silica-based film that has used said composition.
In addition, for realize the reason of above-mentioned effect by the present invention, the inventor etc. are presumed as follows.
; for even the operation that repeats not discharge and discharge does not produce the obstruction of printing ink nozzle yet; patterned section shape in the time of can making to describe in addition approaches rectangle; even and the thickness increase that makes to describe pattern also can suppress Procuring and solidify after the generation of crackle; need to have concurrently and contain ink-jet and form the non-drying property of the printing ink of composition in spray nozzle front end section with silica-based film, even and inhibition and the thicker resistance to cracking line also do not cracked of thick film of the wetting extendability of drop during to land.In order to meet these characteristics, form the solvent of composition with silica-based film as ink-jet, importantly, use and contain as the second solvent of low boiling point component with as the gamma-butyrolactone of high boiling point composition and the mixed solvent of the 3rd solvent.And very importantly, in this mixed solvent, according to the total mass with respect to solvent, the mode that the mass ratio of gamma-butyrolactone and the second solvent is specific numerical range is adjusted content separately.Thus, think main by the effect of gamma-butyrolactone and the 3rd solvent, can reach the non-drying property at spray nozzle front end high-levelly, main by the effect of gamma-butyrolactone and the second solvent in addition, the inhibition of the wetting extendability of the drop in the time of can reaching the printing ink land high-levelly, further, by the Si that contains phenyl and contain two senses in siloxane backbone, can reach the resistance to cracking line high-levelly.In addition, in the present invention, the boiling point of the 2nd solvent is made as to 80～100 ℃, the boiling point of the 3rd solvent is made as to 180～230 ℃, to be made as more than 0.2 with respect to the mass ratio of the gamma-butyrolactone of the total mass of solvent, and will be made as 0.2～0.5 with respect to the mass ratio of the second solvent of the total mass of solvent.This is based on the inventor's etc. following understanding: for the consideration of the inhibition that takes into account the wetting extendability of drop while containing printing ink that ink-jet forms composition with silica-based film in the non-drying property of spray nozzle front end section with to land, these conditions are suitable.
Further, for the fine droplet land at printing ink, to as coating object surperficial the time, realize that this drop is difficult for soak the such effect of expansion, think that it is also a reason that ink-jet contains surface conditioner with silica-based film formation composition.Think and control thus the wettability for applied thing, the mobility of silica-based resin, thus the wetting expansion of the drop while suppressing the printing ink land.More specifically, the wetting expansion of the drop while thinking the printing ink land, the increase of local ink viscosity, the surface tension variations that by printing ink, for the ununiformity of the solvent evaporation of the wetting ununiformity of applied thing (depression etc.), printing ink while discharging, are caused cause.Therefore, the surface conditioner in the present invention as the surface tension homogenizing of filming that is selected from (1) and has the drying process of making, improvement for compound, (2) of the wetting effect of applied thing there is the evaporation homogenizing that makes from the solvent of film coated surface, reduce that local viscosity increases, at least one compound in the compound of the effect of surface tension variations and being defined.
Embodiment
Below, for the preferred embodiment of the present invention, be elaborated.
[ink-jet forms composition with silica-based film]
The ink-jet of present embodiment forms composition with silica-based film and contains following (A)～(C) composition.
(A), by following monomer component hydrolysis, polycondensation and the silicon compound obtained, described monomer component contains:
General formula (I): PhSiX
3represented compound,
[in formula, Ph means also can have substituent phenyl, and X means hydrolization group, the X of a plurality of existence can be identical also can be different.]
General formula (II): R
1 nsiX
4-nrepresented compound,
[in formula, R
1mean the alkyl of carbonatoms 1～20, X means hydrolization group, and n means 0 or 1 integer, the X of a plurality of existence can be identical also can be different.], and
General formula (III): R
2 2siX
2represented compound.
[in formula, R
2mean the organic group of carbonatoms 1～20, X means hydrolization group, the R of a plurality of existence
2and X separately can be identical also can be different.]
(B) contain the 3rd solvent that the second solvent that gamma-butyrolactone, boiling point are 80～100 ℃ and boiling point be 180～230 ℃ (wherein, except gamma-butyrolactone) solvent, total mass with respect to solvent, the mass ratio of gamma-butyrolactone is more than 0.2, and, with respect to the total mass of solvent, the mass ratio of the second solvent is 0.2～0.5.
(C) surface conditioner.
Below, respectively to (A) composition, (B) composition and (C) composition described in detail.
(A) composition: silicon compound
Form composition (below, according to circumstances be called " composition ") for the ink-jet of present embodiment with silica-based film,
Using following monomer component hydrolysis, polycondensation and the silicon compound obtained as essential component, described monomer component contains:
General formula (I): PhSiX
3represented compound,
[in formula, Ph means also can have substituent phenyl, and X means hydrolization group, the X of a plurality of existence can be identical also can be different.]
General formula (II): R
1 nsiX
4-nrepresented compound,
[in formula, R
1mean the alkyl of carbonatoms 1～20, X means hydrolization group, and n means 0 or 1 integer, the X of a plurality of existence can be identical also can be different.], and
General formula (III): R
2 2siX
2represented compound.
[in formula, R
2mean the organic group of carbonatoms 1～20, X means hydrolization group, the R of a plurality of existence
2and X separately can be identical also can be different.Wherein, R
2do not mean hydrolization group.] in addition, in this manual, described " hydrolysis, polycondensation " refer to, will comprise the monomer component hydrolysis of the compound that aforementioned formula means, on one side dehydration (H
2o) one side condensation polymerization.
As described X, for example can enumerate alkoxyl group, halogen atom, acetoxyl group, isocyanate group and hydroxyl, wherein preferably be made as alkoxyl group.By X is made as to alkoxyl group, can realize obtained silicon compound aqueous stability, suppress the halogen concentration in the composition of gained.
When X is alkoxyl group, as the represented compound of general formula (1), can enumerate the represented trialkoxy silane of following general formula (I-1).Trialkoxy silane can be used separately a kind of, also can combine two or more the use.
PhSi(OR
1)
3 …(I-1)
[in formula, Ph means also can have substituent phenyl, R
1can be identical also can be different, mean independently of one another the alkyl of carbonatoms 1～3.]
As the represented trialkoxy silane of general formula (I-1), can enumerate phenyltrimethoxysila,e, phenyl triethoxysilane, phenyl three positive propoxy silane and phenyl three isopropoxy silane etc.Wherein, for consideration reactive, byproduct of reaction, preferably use phenyl triethoxysilane.
When X is alkoxyl group, as the represented compound of general formula (II), can enumerate the represented tetraalkoxysilane of following general formula (II-1) and the represented trialkoxy silane of following general formula (II-2).These organoalkoxysilanes can be used separately a kind of, also can combine two or more the use.
Si(OR
2)
4 …(II-1)
[in formula, R
2can be identical also can be different, mean independently of one another the alkyl of carbonatoms 1～3.]
R
3Si(OR
4)
3 …(II-2)
[in formula, R
3mean alkyl, R
4can be identical also can be different, mean independently of one another the alkyl of carbonatoms 1～3.]
As the represented tetraalkoxysilane of general formula (II-1), can enumerate tetramethoxy-silicane, tetraethoxysilane, four positive propoxy silane and tetraisopropoxysilan etc.Wherein, for processing reactive, byproduct of reaction, easily consider, preferably use tetraethoxysilane.
As the represented trialkoxy silane of general formula (II-2), can enumerate methyltrimethoxy silane, Union carbide A-162, methyl three positive propoxy silane, methyl three isopropoxy silane, ethyl trimethoxy silane, ethyl triethoxysilane, ethyl three positive propoxy silane, ethyl three isopropoxy silane, propyl trimethoxy silicane, propyl-triethoxysilicane, propyl group three positive propoxy silane, propyl group three isopropoxy silane, butyl trimethoxy silane, the butyl triethoxyl silane, butyl three positive propoxy silane and butyl three isopropoxy silane etc.Wherein, for consideration reactive, byproduct of reaction, preferably use Union carbide A-162, ethyl triethoxysilane and propyl-triethoxysilicane.
When X is alkoxyl group, as the represented compound of general formula (III), can enumerate the represented dialkoxy silicane of following general formula (III-1).Dialkoxy silicane can be used separately a kind of, also can combine two or more the use.
R
5 2Si(OR
6)
2 …(III-1)
[in formula, R
5can be identical also can be different, mean independently of one another alkyl or phenyl, R
6can be identical also can be different, mean independently of one another the alkyl of carbonatoms 1～3.]
As the represented dialkoxy silicane of general formula (III-1), can enumerate dimethyldimethoxysil,ne, dimethyldiethoxysilane, dimethyl two positive propoxy silane, dimethyl diisopropoxy silane, diethyl dimethoxy silane, the diethyl diethoxy silane, diethyl two positive propoxy silane, diethyl diisopropoxy silane, diη-propyl dimethoxy silane, the diη-propyl diethoxy silane, diη-propyl two positive propoxy silane, diη-propyl diisopropoxy silane, diisopropyl dimethoxy silane, the di-isopropyl diethoxy silane, di-isopropyl two positive propoxy silane, di-isopropyl diisopropoxy silane, di-n-butyl dimethoxy silane, the di-n-butyl diethoxy silane, di-n-butyl two positive propoxy silane, di-n-butyl diisopropoxy silane, di-sec-butyl dimethoxy silane, the di-sec-butyl diethoxy silane, di-sec-butyl two positive propoxy silane, di-sec-butyl di-isopropyl silane, di-t-butyl dimethoxy silane, the di-t-butyl diethoxy silane, di-t-butyl two positive propoxy silane, di-t-butyl diisopropoxy silane, dimethoxydiphenylsilane, the phenylbenzene diethoxy silane, phenylbenzene two positive propoxy silane, phenylbenzene diisopropoxy silane, phenyl methyl dimethoxy silane, the phenyl methyl diethoxy silane, phenyl methyl two positive propoxy silane, phenyl methyl diisopropoxy silane, ethylphenyl dimethoxy silane, the ethylphenyl diethoxy silane, ethylphenyl two positive propoxy silane and ethylphenyl diisopropoxy silane etc.
In the present embodiment, described general formula (I), (II) reach (III) represented organoalkoxysilane and can be used in combination.More specifically, described general formula (I-1), (II-1), (II-2) and (III-1) represented organoalkoxysilane can be used in combination (wherein, described general formula (II-1) and (II-2) represented compound may not and with).
The ratio of mixture of these organoalkoxysilanes is not particularly limited.Wherein, for being easy to guarantee the consideration of ink-jet with the resistance to cracking line of the silica-based film obtained after the stability (viscosity stability) under the room temperature of silica-based film formation composition and raising ink-jet, the molar weight M of represented tetraalkoxysilane with respect to described general formula (II-1)
1, the molar weight M of the trialkoxy silane that the trialkoxy silane that general formula (I-1) is represented and general formula (II-2) are represented
2and the molar weight M of the represented dialkoxy silicane of general formula (III-1)
3the ratio (M of total amount
2+ M
3)/M
1be preferably more than 0.1, more preferably, more than 0.3, more preferably, more than 0.5, especially be preferably more than 0.8.In addition, for the wettability with basal substrate, be good viewpoint, (M
2+ M
3)/M
1be preferably below 4.0, more preferably, below 2.5, especially be preferably below 1.5.
When hydrolysis, polycondensation organoalkoxysilane, (B) composition can be used as to solvent, or also can use the solvent beyond (B) composition.The solvent used during as hydrolysis, polycondensation organoalkoxysilane, can enumerate: acetone, methyl ethyl ketone, methyl n-propyl ketone, methyl isopropyl Ketone, methyl n-butyl ketone, methyl iso-butyl ketone (MIBK), methyl-n-amyl ketone, methyl n hexyl ketone, metacetone, butyrone, diisobutyl ketone, trimethylammonium nonanone, pimelinketone, cyclopentanone, methylcyclohexanone, 2, the ketone series solvents such as 4-diacetylmethane, acetonyl-acetone, gamma-butyrolactone and γ-valerolactone;
Anaesthetie Ether, methyl ethyl ether, the positive diη-propyl ether of methyl, Di Iso Propyl Ether, tetrahydrofuran (THF), methyltetrahydrofuran, two
alkane and dimethyl two
the ether series solvents such as alkane;
Ethylene glycol dimethyl ether, the ethylene glycol bisthioglycolate ethyl ether, the ethylene glycol bisthioglycolate n-propyl ether, the ethylene glycol bisthioglycolate butyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol methyl ethyl ether, Diethylene Glycol methyl list n-propyl ether, Diethylene Glycol methyl list n-butyl ether, Diethylene Glycol diη-propyl ether, the Diethylene Glycol di-n-butyl ether, Diethylene Glycol methyl list n-hexyl ether, the triethylene glycol dimethyl ether, the triethylene glycol Anaesthetie Ether, the triethylene glycol methyl ethyl ether, triethylene glycol methyl list n-butyl ether, the triethylene glycol di-n-butyl ether, triethylene glycol methyl list n-hexyl ether, the TEG dimethyl ether, the TEG Anaesthetie Ether, four diethylene glycol methyl ethyl ethers, TEG methyl list n-butyl ether, the Diethylene Glycol di-n-butyl ether, TEG methyl list n-hexyl ether, the TEG di-n-butyl ether, the propylene glycol dimethyl ether, the propylene glycol Anaesthetie Ether, propylene glycol diη-propyl ether, the propylene glycol dibutyl ether, the dipropylene glycol dimethyl ether, the dipropylene glycol Anaesthetie Ether, the dipropylene glycol methyl ethyl ether, dipropylene glycol methyl list n-butyl ether, dipropylene glycol diη-propyl ether, the dipropylene glycol di-n-butyl ether, dipropylene glycol methyl list n-hexyl ether, the tripropylene glycol dimethyl ether, the tripropylene glycol Anaesthetie Ether, the tripropylene glycol methyl ethyl ether, tripropylene glycol methyl list n-butyl ether, the tripropylene glycol di-n-butyl ether, tripropylene glycol methyl list n-hexyl ether, four propylene glycol dimethyl ethers, four propylene glycol Anaesthetie Ethers, four propylene glycol methyl ethyl ethers, four propylene glycol methyl list n-butyl ether, the aklylene glycol dialkyl ether series solvents such as four propylene glycol methyl list n-hexyl ethers and four propylene glycol di-n-butyl ethers,
Methyl acetate, ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, sec-butyl acetate, n-amyl acetate, sec-amyl acetate, acetic acid-3-methoxyl group butyl ester, methyl amyl acetate, acetic acid 2-ethyl butyl ester, acetic acid 2-ethylhexyl, jasmal, hexalin acetate, methylcyclohexyl acetate, nonyl acetate, methyl acetoacetate, methyl aceto acetate, the diethylene glycol monomethyl ether acetic ester, the TC acetic ester, Diethylene Glycol list n-butyl ether acetic ester, the DPGME acetic ester, the dihydroxypropane single-ethyl ether acetic ester, diacetate glycol ester, acetic acid methoxyl group triethyleneglycol ester, ethyl propionate, n-butyl propionate, isoamyl propionate, diethyl oxalate, the oxalic acid di-n-butyl, methyl lactate, ethyl lactate, the ester series solvents such as n-butyl lactate and lactic acid n-pentyl ester,
The aklylene glycol alkyl oxide acetic ester series solvents such as Ethylene Glycol Methyl ether propionic ester, glycol ethyl ether propionic ester, Ethylene Glycol Methyl ether acetic acid ester, Ethylene Glycol Methyl ether acetic acid ester, Diethylene Glycol methyl ether acetic ester, Diethylene Glycol ethyl ether acetic ester, Diethylene Glycol n-butyl ether acetic ester, methyl proxitol acetate, propylene glycol ethyl ether acetic ester, propylene glycol propyl ether acetic ester, dipropylene glycol methyl ether acetic ester and dipropylene glycol ethyl ether acetic ester;
The pyrrolidone series solvents such as N-Methyl pyrrolidone, N-ethyl pyrrolidone, N-propyl pyrrole alkane ketone, N-butyl pyrrolidine ketone, N-hexyl pyrrolidone and N-cyclohexyl pyrrolidone;
Methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, sec-butyl alcohol, the trimethyl carbinol, Pentyl alcohol, primary isoamyl alcohol, the 2-methyl butanol, sec.-amyl alcohol, tertiary amyl alcohol, the 3-methoxybutanol, n-hexyl alcohol, the 2-methyl amyl alcohol, secondary hexyl alcohol, 2-ethyl butanol, secondary enanthol, n-Octanol, 2-Ethylhexyl Alcohol, secondary octanol, nonanol-, nonylcarbinol, secondary hendecanol, Exxal 12, secondary tetradecanol, secondary heptadecanol, phenol, hexalin, the pure series solvent such as methyl-cyclohexanol and benzylalcohol,
The glycol series solvents such as ethylene glycol, 1,2-PD, 1,3 butylene glycol, Diethylene Glycol, dipropylene glycol, triethylene glycol and tripropylene glycol;
The alkylene glycol monoalkyl ethers series solvents such as Ethylene Glycol Methyl ether, glycol ethyl ether, glycol monomethyl phenyl ether, diethylene glycol monomethyl ether, TC, Diethylene Glycol list n-butyl ether, Diethylene Glycol list n-hexyl ether, oxyethyl group triglycol, TEG list n-butyl ether, propylene glycol monomethyl ether, DPGME, dihydroxypropane single-ethyl ether and tripropylene glycol monomethyl ether; And
Acetonitrile, DMF, N,N-dimethylacetamide and N, N-dimethyl sulfoxide (DMSO) etc.They can use separately a kind of, also can be used in combination of two or more.
In addition, when hydrolysis, polycondensation organoalkoxysilane, use in the situation of (B) composition solvent in addition, can be after reaction by distillation, remove etc. and to remove or to replace solvent, by obtained silicone resin or silicone resin solution in modulation ink-jet silica-based film, forming composition.
The quantity of solvent during monomer component that uses the hydrolysis of described solvent, polycondensation to contain the represented compound of described general formula (I)～(III), the consideration for reaction homogeneity etc., preferably be made as SiO
2the scope that conversion concentration is 5～35 quality %, the more preferably scope of 10～30 quality %.
In addition, when hydrolysis, polycondensation organoalkoxysilane, for the homogenizing of Reaction time shorten and reaction, preferably add catalyzer.As catalyzer, can enumerate acid catalyst, basic catalyst and metal complex compounds etc., for guaranteeing that obtained ink-jet forms the consideration of the stability of composition with silica-based film, preferably use acid catalyst.
As acid catalyst, can enumerate for example organic acid and mineral acid.As organic acid, for example can enumerate formic acid, toxilic acid, fumaric acid, phthalic acid, propanedioic acid, succsinic acid, tartrate, oxysuccinic acid, lactic acid, citric acid, acetic acid, propionic acid, butyric acid (acid of Block タ Application), valeric acid, caproic acid, enanthic acid, sad, n-nonanoic acid, capric acid, oxalic acid, hexanodioic acid, sebacic acid, butyric acid (butyric acid), oleic acid, stearic acid, linolic acid, linolenic acid, Whitfield's ointment, Phenylsulfonic acid, phenylformic acid, para-amino benzoic acid, tosic acid, methylsulfonic acid, trifluoromethanesulfonic acid and trifluoro ethyl sulfonic acid.As mineral acid, can enumerate for example hydrochloric acid, phosphoric acid, nitric acid, boric acid, sulfuric acid and hydrofluoric acid.Among these, as organic acid, particularly preferably use toxilic acid, as mineral acid, particularly preferably use nitric acid.They can use separately a kind of, also can be used in combination of two or more.
The usage quantity of catalyzer can be suitable selected according to the kind of the kind of organoalkoxysilane and usage quantity, catalyzer etc.For example, be used in combination the represented tetraalkoxysilane of general formula (II-1), the trialkoxy silane that the trialkoxy silane that general formula (I-1) is represented and general formula (II-2) are represented and the represented dialkoxy silicane of general formula (III-1), and while using acid catalyst as catalyzer, will be with respect to the total mole number of organoalkoxysilane, the molar ratio of the tetraalkoxysilane that general formula (II-1) is represented is made as A, the molar ratio of the trialkoxy silane that the trialkoxy silane that general formula (I-1) is represented and general formula (II-2) are represented is made as B, the molar ratio of the dialkoxy silicane that general formula (III-1) is represented is made as the words of C, the usage quantity of acid catalyst (molar ratio) is preferably the scope of [(4A+3B+2C)/3000]～[(4A+3B+2C)/10], the scope of more preferably [(4A+3B+2C)/3000]～[(4A+3B+2C)/100].Be made as in aforesaid scope by the usage quantity by acid catalyst, can carry out with reacting fully, this external enwergy inhibited reaction carries out excessively and produces the phenomenon of gelation.
In addition, hydrolysis, during the polycondensation organoalkoxysilane, the amount of the water used can be according to the kind of organoalkoxysilane and usage quantity and suitable selected.For example be used in combination the represented tetraalkoxysilane of general formula (II-1), during the represented dialkoxy silicane of the trialkoxy silane that the trialkoxy silane that general formula (I-1) is represented and general formula (II-2) are represented and general formula (III-1), will be with respect to the total mole number of organoalkoxysilane, the molar ratio of the tetraalkoxysilane that general formula (II-1) is represented is made as A, the molar ratio of the trialkoxy silane that the trialkoxy silane that general formula (I-1) is represented and general formula (II-2) are represented is made as B, the molar ratio of the dialkoxy silicane that general formula (III-1) is represented is made as the words of C, the amount of water (molar ratio) is preferably the scope of [(4A+3B+2C)/2]～[(4A+3B+2C) * 2], the scope of more preferably [(4A+3B+2C)/2]～[(4A+3B+2C) * 1].Be made as in aforesaid scope by the amount by water, can carry out with reacting fully, this external enwergy inhibited reaction carries out excessively and produces the phenomenon of gelation.
For the weight-average molecular weight (Mw) as the silicon compound of (A) composition, discharge the viewpoints such as property for the solvability to solvent, ink-jet, be preferably 500～20000, more preferably 500～10000.This weight-average molecular weight, in aforementioned range, can be reached the consistency of film-forming properties and silicon compound and the solvent of silica-based film high-levelly.In addition, in this manual, " weight-average molecular weight " refers to and measures by gel permeation chromatography (below, be called " GPC ") and the typical curve of Application standard polystyrene and the value that converses.
The mensuration of<weight-average molecular weight >
Weight-average molecular weight (Mw) for example can be measured by the GPC that adopts following condition.
(condition)
Sample: ink-jet forms composition 10 μ L with silica-based film
Polystyrene standard: TOSOH Co., Ltd's system, polystyrene standard (molecular weight: 190000,17900,9100,2980,578,474,370,266)
Detector: Hitachi Co., Ltd's system, RI detector, trade(brand)name " L-3000 "
Totalizing instrument: Hitachi Co., Ltd's system, GPC totalizing instrument, trade(brand)name " D-2200 "
Pump: Hitachi Co., Ltd's system, trade(brand)name " L-6000 "
De-gassing vessel: Showa Denko K. K's system, trade(brand)name " Shodex DEGAS(Shodex), registered trademark "
Post: Hitachi Chemical Co., Ltd.'s system, trade(brand)name " GL-R440 ", " GL-R430 ", " GL-R420 " connect use successively
Elutriant: tetrahydrofuran (THF) (THF)
Measure temperature: 23 ℃
Flow velocity: 1.75mL/ minute
Minute: 45 minutes
In the present embodiment, the content that ink-jet forms (A) composition in composition with silica-based film is preferably 5～35 quality %, more preferably 5～30 quality %.(A) content of composition is that 5 quality % are above, and the thickness of the silica-based film of formation can be excessively not thin, become appropriate thickness, therefore can be reduced to the possibility that obtains desired thickness and need to carry out repeatedly replotting.Thus, the wetting extendability of the increase that is easy to suppress the process time of becoming, the ink-jet drop that caused by replotting, and the tendency that also is easy to improve the resistance to cracking line is arranged.On the other hand, if (A) content of composition is that 35 quality % are following, there is the ink-jet of making to form the better tendency of storage stability of composition with silica-based film.
(B) composition: solvent
(B) composition of present embodiment is following solvent: the 3rd solvent that the second solvent that to contain gamma-butyrolactone, boiling point be 80～100 ℃ and boiling point are 180～230 ℃, total mass with respect to solvent, the mass ratio of gamma-butyrolactone is more than 0.2, and, with respect to the total mass of solvent, the mass ratio of the 2nd solvent is 0.2～0.5.In addition in this manual, " boiling point " means the boiling point under normal pressure (1 normal atmosphere).
Gamma-butyrolactone is that boiling point is 204 ℃, the organic solvent that is 43.9dyn/cm the surface tension of 20 ℃.Think and there is such boiling point and capillary gamma-butyrolactone by containing in solvent, can take into account the wetting extendability of drop when containing ink-jet forms composition printing ink with silica-based film in the non-drying property of spray nozzle front end section and suppressing the printing ink land.
The boiling point of the second solvent is 80～100 ℃, is preferably 80～90 ℃.As long as boiling point, in such scope, is not particularly limited.As the second solvent, can enumerate 1-propyl alcohol, 2-propyl alcohol and 2-butanols etc.In these solvents, the consideration for the consistency of the silicone resin with obtained, gamma-butyrolactone and the 3rd solvent, be preferably the 2-propyl alcohol.In addition, in composition, the second contained solvent can be one or more.
The 3rd solvent is the solvent except gamma-butyrolactone, and boiling point is 180～230 ℃, is preferably 180～200 ℃.The wetting extendability of drop when taking into account printing ink in the non-drying property of spray nozzle front end section and suppressing land, as previously mentioned, must be used gamma-butyrolactone.On the other hand, in order to seek to improve consistency, the raising printing ink stability at room temperature of ink-jet with the silicone resin in the silica-based film composition and solvent, preferably also with the solvent beyond gamma-butyrolactone and gamma-butyrolactone.
As the 3rd solvent, can enumerate ether series solvent, glycol series solvent, alkylene glycol monoalkyl ethers series solvent, aklylene glycol dialkyl ether series solvent and aklylene glycol alkyl oxide acetic ester series solvent, for the consideration of the consistency excellence with gamma-butyrolactone and the second solvent, preferably use alkylene glycol monoalkyl ethers series solvent and glycol series solvent.In addition, in composition, the 3rd contained solvent can be one or more.
In present embodiment, total mass with respect to the solvent that contains the 3rd solvent that the second solvent that gamma-butyrolactone, boiling point are 80～100 ℃ and boiling point be 180～230 ℃, the mass ratio of gamma-butyrolactone is more than 0.2, is preferably 0.2～0.7, more preferably 0.2～0.6.In addition, with respect to the total mass of this solvent, the mass ratio of the second solvent is 0.2～0.5, more preferably 0.3～0.5.Mass ratio by will be separately is made as in this scope, can take into account while discharging the printing ink that contains composition the non-drying property at the printing ink of spray nozzle front end section, and the wetting extendability of drop while suppressing land.Therefore, even repeat the operation of not discharging and discharging, the obstruction that does not also produce inkjet nozzle, and the cross section that can make the depiction case is for more approaching the shape of rectangle.
(C) composition: surface conditioner
The composition of present embodiment contains surface conditioner as (C) composition.Contain surface conditioner by composition, can realize controlling printing ink to the wettability of substrate surface and prevent that the drop of printing ink from soaking expansion, can describe the cross-sectional shape of pattern and control as more approaching the shape of rectangle.As (C) composition, can be used as without particular limitation the commercially available compound of surface conditioner, particularly, can use fluorine is that surface conditioner, silicone-based surface conditioner and nonionic are surface conditioner etc.Wherein, it is effective particularly using aspect the wetting expansion of the drop of silicone-based surface conditioner when suppressing the printing ink land.
For the content of (C) composition, with respect to (A) composition, be preferably the scope of 0.1～1.0 quality %, more preferably the scope of 0.2～0.8 quality %.In addition, (C) composition can use separately a kind of, also two or more use the capable of being combined.
[the formation method of silica-based film]
The formation method of the silica-based film of present embodiment possesses: discharge described composition by ink jet method and carry out pattern plotter, form the operation of describing pattern film; Make to describe the operation of pattern film precuring; And make to describe the curing operation of pattern film.
(operation of pattern film is described in formation)
Adopt the pattern plotter of ink jet method to carry out with ink discharge device.Ink discharge device is roughly divided into successive type (continuously discharge type) and two types, type as required usually, preferably uses type as required in present embodiment.Even successive type is the mode of printing ink of also always discharging continuously while on substrate, not describing pattern.On the other hand, type is described the mode of pattern for the amount only discharge needed when needed on substrate as required.
The ink discharge device that has used the ink discharge device of executing the piezoelectric element that alive words can deform and utilized the hot mode that the bubble that generates by heating discharged is arranged in type as required.The ink-jet of present embodiment with silica-based film form composition be basically with which device can, but the consideration changed for the composition that suppresses printing ink preferably adopts the ink discharge device that has used piezoelectric element.
While by ink jet method, carrying out pattern plotter, Yi Bian can in the scope of 50～100 ℃, heat and be described the substrate that will describe pattern on one side.By base plate heating, can further improve the rapid drying of printing ink on substrate, can prevent from describing the confusion of pattern.
(making to describe the operation of pattern film precuring)
In present embodiment, can, before making to describe the curing operation of pattern film, possess the operation that makes to describe the pattern film precuring.Can be when carrying out Procuring, utilization is set as the first paragraph storing temperature 80～140 ℃, the second segment storing temperature is set as to hot plate of 180～250 ℃ etc., by describing the polycondensation promotion of the silicone resin in pattern film and the drying of organic solvent, carries out stage by stage.In addition, above-mentioned first paragraph and/or second segment can be toasted to further refinement.By multistage, toast, silicone resin is solidified equably, the confusion of describing pattern of the thermal convection in the time of can preventing from following solvent to remove.
(making to describe the curing operation of pattern film)
In this operation, final solidifying for example burns till and carries out describing pattern film (also can not carrying out Procuring) the Heating temperature of 350～1000 ℃.In addition, final curing Heating temperature is more than 350 ℃, easily reach fully and solidify, and be below 1000 ℃, can be difficult to produce the impact on substrate caused by high temperature.
Be preferably 2～60 minutes, more preferably 2～30 minutes heat-up time during final solidifying.Be below 60 minutes this heat-up time, owing to not inputting the excessively situation of increase of heat, therefore can suppress substrate and gradually produce deteriorated.In addition, as heating unit, preferably use quartz tube furnace, other stove, hot plate, rapid thermal annealing (RTA), UV to irradiate the heat treatment apparatus etc. that annealing and EB irradiate annealing etc.
The atmosphere of the gas during for final solidifying, only otherwise substrate is caused to undesirable impact, can be the non-active gas atmosphere such as nitrogen, argon gas and helium, also can be any of atmosphere of oxygen, ozone isoreactivity gas.
The purposes of the silica-based epithelium that the formation method of the silica-based film by present embodiment forms is not particularly limited, such as enumerating the equipment that possesses insulating film for semiconductor devices (element), multi-layer wiring board etc.Particularly, in semiconductor devices, can be used as that surface protection film (passive film), buffering are filmed, interlayer dielectric and nonproliferation film etc.On the other hand, in multi-layer wiring board, can be used as aptly interlayer dielectric.
[semiconductor devices]
The semiconductor devices of present embodiment possesses: the silica-based film of substrate and the pattern with regulation that the formation method by described silica-based film forms on substrate.As such semiconductor devices, for example can enumerate: diode, transistor, compound semiconductor, thermistor, voltage dependent resistor and thyristor etc. be semi-conductor separately, the DRAM(dynamic RAM), the SRAM(static RAM), the EPROM(Erarable Programmable Read only Memory), mask rom (mask ROM), the EEPROM(EEPROM) and the storage element such as flash memory, microprocessor, the logic circuit component such as DSP and ASIC, take the MMIC(monolithic integrated microwave circuit) be the integrated circuit components such as compound semiconductor of representative, hybrid integrated circuit (mixing IC), and the photo-electric conversion elements such as photodiode and charge coupled cell etc.
In addition, as multi-layer wiring board, can enumerate such as high-density wiring boards such as MCM.
[solar cell system]
The solar cell system of present embodiment possesses above-mentioned semiconductor devices is arranged.In above-mentioned semiconductor devices, photo-electric conversion element is the semiconductor devices for solar cell system, also, due to the impact of recent environmental problem, actively develops.As representational photo-electric conversion element, can enumerate and make the diffusion of contaminants that is called as doping agent in semi-conductive Si wafer, form the photo-electric conversion element that p-n engages.In such photo-electric conversion element, for the high efficiency of solar cell, sometimes be produced on a slice Si wafer and mix non-diffusion zone and the such element of diffusion zone that has doping agent.Under these circumstances, produced at non-diffusion zone and formed the needs that diffusion prevents mask.Up to now, diffusion prevents that mask from carrying out patterning by the silica-based film that will be formed by CVD etc. by photolithography and obtaining.But, use the ink-jet of present embodiment to form composition with silica-based film, can obtain having been undertaken by ink-jet the silica-based film of patterning, can cut down process number, cut down necessary material, be therefore useful.
The silica-based epithelium of present embodiment also can be used as the purposes such as parts for liquid crystal, optical waveguides and photo-resist in addition, but use is not limited to this.
Embodiment
Below, be described more specifically the present invention based on embodiment and comparative example, but the present invention is not subject to any restriction of following embodiment.
(modulation of silicon compound A)
Tetraethoxysilane (TEOS) 66.0g and phenyl triethoxysilane (PhTES) 76.2g are dissolved in DPGME (boiling point: 188 ℃) 21.4g, under agitation through 10 minutes, drip the water 36.0g that is dissolved with toxilic acid 0.4g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of tetraethoxysilane
1, the molar weight M of phenyl triethoxysilane
2ratio M
2/ M
1be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add DPGME until the silicon compound solution total amount is 100g, obtain silicon compound A.The silicone resin solid component concentration of silicon compound A now is 60 quality %.In addition, solids component refers to the solid part of the material volatilized except anhydrate, solvent etc., means nonvolatile component.Be below same.
(modulation of silicon compound B)
Tetraethoxysilane 64.6g, phenyl triethoxysilane 29.8g and phenyl methyl diethoxy silane (PhMeDES) 39.1g are dissolved in DPGME (boiling point: 188 ℃) 33.9g, under agitation through 10 minutes, drip the water 32.2g that is dissolved with toxilic acid 0.4g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of tetraethoxysilane
1, the molar weight M of phenyl triethoxysilane
2and the molar weight M of phenyl methyl diethoxy silane
3and ratio (M
2+ M
3)/M
1be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add DPGME until the silicon compound solution total amount is 100g, obtain silicon compound B.The silicone resin solid component concentration of silicon compound B now is 60 quality %.
(modulation of silicon compound C)
Tetraethoxysilane 54.2g, phenyl triethoxysilane 25.0g and phenylbenzene diethoxy silane (DPhDES) 42.5g are dissolved in DPGME (boiling point: 188 ℃) 51.0g, under agitation through 10 minutes, drip the water 27.0g that is dissolved with toxilic acid 0.3g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of tetraethoxysilane
1, the molar weight M of phenyl triethoxysilane
2and the molar weight M of phenylbenzene diethoxy silane
4and ratio (M
2+ M
4)/M
1be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add DPGME until the silicon compound solution total amount is 100g, obtain silicon compound C.The silicone resin solid component concentration of silicon compound C now is 60 quality %.
(modulation of silicon compound D)
Tetraethoxysilane 54.2g, phenyl triethoxysilane 25.0g and phenylbenzene diethoxy silane 42.5g are dissolved in Diethylene Glycol single-butyl ether (boiling point: 230 ℃) 51.0g, under agitation through 10 minutes, drip the water 27.0g that is dissolved with toxilic acid 0.3g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of tetraethoxysilane
1, the molar weight M of phenyl triethoxysilane
2and the molar weight M of phenylbenzene diethoxy silane
4and ratio (M
2+ M
4)/M
1be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add the Diethylene Glycol single-butyl ether until the silicon compound solution total amount is 100g, obtain silicon compound D.The silicone resin solid component concentration of silicon compound D now is 60 quality %.
(modulation of silicon compound E)
Phenyl triethoxysilane 54.3g and phenyl methyl diethoxy silane 47.6g are dissolved in DPGME (boiling point: 188 ℃) 79.6g, under agitation through 10 minutes, drip the water 18.3g that is dissolved with toxilic acid 0.2g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of phenyl triethoxysilane
2, the molar weight M of phenyl methyl diethoxy silane
3ratio M
3/ M
2be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add DPGME until the silicon compound solution total amount is 100g, obtain silicon compound E.The silicone resin solid component concentration of silicon compound E now is 60 quality %.
(modulation of silicon compound F)
Tetraethoxysilane 48.4g and phenylbenzene diethoxy silane 63.3g are dissolved in DPGME (boiling point: 188 ℃) 65.5g, under agitation through 10 minutes, drip the water 22.6g that is dissolved with toxilic acid 0.3g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of tetraethoxysilane
1, the molar weight M of phenylbenzene diethoxy silane
4ratio M
4/ M
1be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add DPGME until the silicon compound solution total amount is 100g, obtain silicon compound F.The silicone resin solid component concentration of silicon compound F now is 60 quality %.
(modulation of silicon compound G)
Tetraethoxysilane 54.2g, phenyl triethoxysilane 25.0g and phenylbenzene diethoxy silane 42.5g are dissolved in propylene glycol monomethyl ether (boiling point: 146 ℃) 51.0g, under agitation through 10 minutes, drip the water 27.0g that is dissolved with toxilic acid 0.3g in the solution of gained, react 10 hours, obtain the silicon compound solution of 200g.Now, with respect to the molar weight M of tetraethoxysilane
1, the molar weight M of phenyl triethoxysilane
2and the molar weight M of phenylbenzene diethoxy silane
4and ratio (M
2+ M
4)/M
1be 1.0.Afterwards, use vaporizer to carry out underpressure distillation and remove, until above-mentioned silicon compound solution total amount is below 95g.Afterwards, add propylene glycol monomethyl ether until the silicon compound solution total amount is 100g, obtain silicon compound G.The silicone resin solid component concentration of silicon compound G now is 60 quality %.
[embodiment 1]
Add silicone-based surface conditioner, the trade(brand)name that nanmu originally changes into Co., Ltd.'s system: Disparlon1711(" Disparlon " for registered trademark in above-mentioned silicon compound B.Below omit statement.) 0.3g stirring, add 2-propyl alcohol (boiling point: 82 ℃) the stirring of gamma-butyrolactone (boiling point: 204 ℃) and the 13.3g of 13.3g.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.2, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 47.4%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.2/0.2/0.6, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[embodiment 2]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound B, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[embodiment 3]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound C, adding the gamma-butyrolactone (boiling point: 204 ℃) of 13.3g and the 2-propyl alcohol (boiling point: 82 ℃) of 13.3g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.2, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 47.4%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.2/0.2/0.6, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[embodiment 4]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound C, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[embodiment 5]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound C, adding the gamma-butyrolactone (boiling point: 204 ℃) of 20.0g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.0g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.2, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.4.In addition, silicone resin solid component concentration now is 37.5%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.2/0.4/0.4, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[embodiment 6]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound B, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-butanols (boiling point: 100 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-butanols is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-butanols/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[embodiment 7]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound D, add gamma-butyrolactone (boiling point: 204 ℃) and the 2-propyl alcohol (boiling point: 82 ℃) of 53.4g and stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/Diethylene Glycol single-butyl ether is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 1]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound A, adding the gamma-butyrolactone (boiling point: 204 ℃) of 13.3g and the 2-propyl alcohol (boiling point: 82 ℃) of 13.3g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.2, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 47.4%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.2/0.2/0.6, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 2]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound A, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 3]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound A, adding the gamma-butyrolactone (boiling point: 204 ℃) of 5.7g and the 2-propyl alcohol (boiling point: 82 ℃) of 11.4g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.1, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 51.2%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.1/0.2/0.7, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 4]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound B, adding the gamma-butyrolactone (boiling point: 204 ℃) of 5.7g and the 2-propyl alcohol (boiling point: 82 ℃) of 11.4g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.1, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 51.2%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.1/0.2/0.7, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 5]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound C, adding the gamma-butyrolactone (boiling point: 204 ℃) of 5.7g and the 2-propyl alcohol (boiling point: 82 ℃) of 11.4g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.1, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 51.2%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.1/0.2/0.7, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 6]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound E, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 7]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound F, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 8]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound C, adding the gamma-butyrolactone (boiling point: 204 ℃) of 40.0g and the 2-propyl alcohol (boiling point: 82 ℃) of 120.0g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.2, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.6.In addition, silicone resin solid component concentration now is 23.1%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.2/0.6/0.2, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 9]
2-propyl alcohol (boiling point: 82 ℃) stirring to the gamma-butyrolactone (boiling point: 204 ℃) that adds 13.3g in above-mentioned silicon compound B and 13.3g.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.2, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.2.In addition, silicone resin solid component concentration now is 47.4%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/DPGME is 0.2/0.2/0.6, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 10]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound B, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the propylene glycol monomethyl ether (boiling point: 146 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of propylene glycol monomethyl ether is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/propylene glycol monomethyl ether/DPGME is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
[comparative example 11]
Add the Disparlon 1711 of 0.3g and stir in above-mentioned silicon compound G, adding the gamma-butyrolactone (boiling point: 204 ℃) of 53.4g and the 2-propyl alcohol (boiling point: 82 ℃) of 40.1g and also stir.Now, with respect to the total mass of solvent, the mass ratio of gamma-butyrolactone is 0.4, and with respect to the total mass of solvent, the mass ratio of 2-propyl alcohol is 0.3.In addition, silicone resin solid component concentration now is 31.0%.Then, the mixed solvent that the quality ratio of components that adds gamma-butyrolactone/2-propyl alcohol/propylene glycol monomethyl ether is 0.4/0.3/0.3, until the silicone resin solid component concentration is 13.0%, makes ink-jet and form composition with silica-based film.
Ink-jet for the embodiment 1～7 so obtained and comparative example 1～11 forms composition with silica-based film, implements following evaluation.
[the spray nozzle clogging evaluation while discharging again]
During spray nozzle clogging when discharging is again estimated, having used ink-jet discharge machine, trade(brand)name: the NanoPrinter-1100 Standard(" NanoPrinter " of the icrojet of M Co., Ltd. system is registered trademark).Then, with room temperature (23 ℃) lower discharge (3 minutes), discharge (5 minutes), discharge (30 seconds), discharge (5 minutes), the order of discharging (30 seconds) repeats the discharge of printing ink (each ink-jet forms composition with silica-based film) and while not discharging, determines whether discharge printing ink in spray nozzle clogging ground does not occur.
[describing the evaluation of pattern cross-sectional shape]
For the cross-sectional shape of describing pattern, estimate as follows.At first, use NanoPrinter-1100 Standard, discharge printing ink (each ink-jet forms composition with silica-based film), at the pattern that is heated to describe on the minute surface Si wafer of 70 ℃ regulation.Now, the condition of describing of device is set as to " width: 800 μ m, length: 20000 μ m, average film thickness: 1.2 μ m ".Then, the patterned section shape of surely describing with the poor instrumentation of section.The poor meter of section uses the trade(brand)name of Veeco company system: Dektak 150(" Dektak " is registered trademark).Now, will be with respect to thickness 0 μ m(base) ratio (%) of the cross-sectional width of describing pattern at the thickness of the describing the pattern cross-sectional width 1.0 μ m places that locate calculates as rectangular degree.Then, for rectangular degree, be the situation more than 85%, be evaluated as A: cross-sectional shape is rectangle; Situation for being less than 85% is evaluated as B: cross-sectional shape is not rectangle.
[having or not of crackle]
For having or not of crackle, estimated as follows.At first, use NanoPrinter-1100 Standard, discharge printing ink (each ink-jet forms composition with silica-based film), at the pattern film that is heated to describe on Si unit (セ Le) substrate (concave-convex surface is 4 μ m) of 70 ℃ regulation.Now, the condition of describing of device is set as to " width: 800 μ m, length: 20000 μ m, average film thickness: 1.0 μ m ".This cell substrate is inserted to the quartz boat of vertical heater, use large Japanese Screen to manufacture vertical heater, the trade(brand)name of Co., Ltd.'s system: AVF-801, at oxygen atmosphere (nitrogen flow: 4.0ml/ minute and oxygen flow: 0.2ml/ minute), heat-treat under the condition of 600 ℃/60 minutes, carry out solidifying of pattern film.Then, use Olympus Co., Ltd's opticmicroscope processed, trade(brand)name: the pattern film after the MX61 visual observation is solidified, confirm having or not of crackle.
The ink-jet of embodiment 1～7 and comparative example 1～11 is shown in to table 1 and table 2 with the composition of silica-based film formation composition and above-mentioned evaluation result.
Table 1
Table 2
As shown in table 1, in embodiment 1～7, the spray nozzle clogging while not discharging again, for the patterned section shape, the cross-sectional width at thickness 1.0 μ m places is also more than 85% with respect to the base width of describing patterned section, is rectangle.In addition, the also generation to crackle unconfirmed.
On the other hand, as shown in table 2, in comparative example 1,2 and 7, the spray nozzle clogging while not discharging again, for the patterned section shape, the cross-sectional width at thickness 1.0 μ m places is also more than 85% with respect to the base width of describing patterned section, is rectangle.But, confirm the generation of crackle.
In comparative example 3, although the spray nozzle clogging while not discharging again, for the patterned section shape, the cross-sectional width at thickness 1.0 μ m places is below 75% with respect to the base width of describing patterned section, is not rectangle.In addition, confirm the generation of crackle.
In comparative example 4,5,6,9 and 10, although the spray nozzle clogging while not discharging again, the generation to crackle unconfirmed, the cross-sectional width at thickness 1.0 μ m places is below 75% with respect to the base width of describing patterned section, is not rectangle.
In comparative example 8,11, have the spray nozzle clogging while discharging again.Therefore, for having or not of cross-sectional shape and crackle, estimated.
Claims (5)
1. an ink-jet forms composition with silica-based film, it is characterized in that, it contains silicon compound, solvent and surface conditioner,
The silicon compound of described silicon compound for following monomer component hydrolysis, polycondensation are obtained, described monomer component contains:
General formula (I): PhSiX
3represented compound, in formula, Ph means also can have substituent phenyl, X means hydrolization group, the X of a plurality of existence can be identical also can be different,
General formula (II): R
1 nsiX
4-nrepresented compound, in formula, R
1mean the alkyl of carbonatoms 1～20, X means hydrolization group, and n means 0 or 1 integer, the X of a plurality of existence can be identical also can be different, and
General formula (III): R
2 2siX
2represented compound, in formula, R
2mean the organic group of carbonatoms 1～20, X means hydrolization group, the R of a plurality of existence
2and X separately can be identical also can be different;
Described solvent contains the 3rd solvent that the second solvent that gamma-butyrolactone, boiling point are 80～100 ℃ and boiling point are 180～230 ℃,
With respect to the total mass of described solvent, the mass ratio of described gamma-butyrolactone is more than 0.2, and with respect to the total mass of described solvent, the mass ratio of described the second solvent is 0.2～0.5.
2. composition as claimed in claim 1, wherein, described surface conditioner is the silicone-based surface conditioner.
3. the formation method of a silica-based film, is characterized in that, it possesses:
Discharge the described composition of claim 1 or 2 by ink jet method and carry out pattern plotter, form the operation of describing pattern film, and
Make the described curing operation of pattern film of describing.
4. a semiconductor devices, is characterized in that, it possesses:
Substrate, and
The silica-based film formed by method claimed in claim 3 on this substrate.
5. a solar cell system, is characterized in that, it possesses semiconductor devices claimed in claim 4.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
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| JP2011095971 | 2011-04-22 | ||
| JP2011-095971 | 2011-04-22 | ||
| JP2011175080 | 2011-08-10 | ||
| JP2011-175080 | 2011-08-10 | ||
| PCT/JP2012/057556 WO2012144292A1 (en) | 2011-04-22 | 2012-03-23 | Silica-coating-forming composition for use with inkjets, method for forming silica coating, semiconductor device, and solar-cell system |
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| JP (1) | JPWO2012144292A1 (en) |
| CN (1) | CN103492499A (en) |
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| CN109963915A (en) * | 2016-12-09 | 2019-07-02 | 阪田油墨股份有限公司 | Nonaqueous inkjet ink composition |
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| EP3264446B1 (en) * | 2015-02-25 | 2019-11-27 | Toray Industries, Inc. | P-type impurity diffusion composition, method for manufacturing semiconductor element using said composition, and method for manufacturing a solar cell |
| JP6893438B2 (en) * | 2016-04-12 | 2021-06-23 | 京セラ株式会社 | Insulating paste used to form a protective layer in the manufacture of solar cell elements |
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| JP2001279134A (en) * | 2000-03-31 | 2001-10-10 | Seiko Epson Corp | Delivery composition and method for manufacturing functional membrane |
| JP2003253203A (en) * | 2002-02-27 | 2003-09-10 | Hitachi Chem Co Ltd | Siliceous film-forming composition, method for producing siliceous film and electronic part |
| JP5015412B2 (en) * | 2004-01-13 | 2012-08-29 | 株式会社Ｄｎｐファインケミカル | Oil-based ink for inkjet printer |
| JP2007211081A (en) * | 2006-02-08 | 2007-08-23 | Konica Minolta Holdings Inc | Inkjet ink and method for inkjet recording |
| JP4216886B2 (en) * | 2006-10-19 | 2009-01-28 | 日立マクセル株式会社 | Pigment ink composition |
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