CN115279942B - 介电涂层 - Google Patents
介电涂层 Download PDFInfo
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- CN115279942B CN115279942B CN202180020801.2A CN202180020801A CN115279942B CN 115279942 B CN115279942 B CN 115279942B CN 202180020801 A CN202180020801 A CN 202180020801A CN 115279942 B CN115279942 B CN 115279942B
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- 238000000576 coating method Methods 0.000 title claims description 37
- 239000011248 coating agent Substances 0.000 title claims description 34
- 239000000203 mixture Substances 0.000 claims abstract description 133
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000002245 particle Substances 0.000 claims abstract description 65
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 239000002243 precursor Substances 0.000 claims abstract description 46
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 238000009826 distribution Methods 0.000 claims abstract description 20
- 230000002378 acidificating effect Effects 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims description 30
- 239000006185 dispersion Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000001704 evaporation Methods 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 150000002576 ketones Chemical class 0.000 claims description 4
- 238000003980 solgel method Methods 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 14
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical group CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 229910010413 TiO 2 Inorganic materials 0.000 description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 239000011669 selenium Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 229910002808 Si–O–Si Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000010292 electrical insulation Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000010962 carbon steel Substances 0.000 description 3
- 230000015556 catabolic process Effects 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
- 238000005336 cracking Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 3
- KUCGHDUQOVVQED-UHFFFAOYSA-N ethyl(tripropoxy)silane Chemical compound CCCO[Si](CC)(OCCC)OCCC KUCGHDUQOVVQED-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical group OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 2
- 238000000224 chemical solution deposition Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000615 nonconductor Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 description 2
- 229910000058 selane Inorganic materials 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 238000007764 slot die coating Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- GIHPVQDFBJMUAO-UHFFFAOYSA-N tributoxy(ethyl)silane Chemical compound CCCCO[Si](CC)(OCCCC)OCCCC GIHPVQDFBJMUAO-UHFFFAOYSA-N 0.000 description 2
- GYZQBXUDWTVJDF-UHFFFAOYSA-N tributoxy(methyl)silane Chemical compound CCCCO[Si](C)(OCCCC)OCCCC GYZQBXUDWTVJDF-UHFFFAOYSA-N 0.000 description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- VUWVDNLZJXLQPT-UHFFFAOYSA-N tripropoxy(propyl)silane Chemical compound CCCO[Si](CCC)(OCCC)OCCC VUWVDNLZJXLQPT-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- LHENQXAPVKABON-UHFFFAOYSA-N 1-methoxypropan-1-ol Chemical compound CCC(O)OC LHENQXAPVKABON-UHFFFAOYSA-N 0.000 description 1
- GSVMCEUQHZAFKG-UHFFFAOYSA-N 2-triethoxysilylaniline Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1N GSVMCEUQHZAFKG-UHFFFAOYSA-N 0.000 description 1
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 description 1
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- UEEBPQBGLVAFMF-UHFFFAOYSA-M [Al+3].[Se-2].[SeH-] Chemical compound [Al+3].[Se-2].[SeH-] UEEBPQBGLVAFMF-UHFFFAOYSA-M 0.000 description 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 1
- VYKYLQRTMKIQFY-UHFFFAOYSA-N [Mo].[K] Chemical compound [Mo].[K] VYKYLQRTMKIQFY-UHFFFAOYSA-N 0.000 description 1
- QMXBEONRRWKBHZ-UHFFFAOYSA-N [Na][Mo] Chemical compound [Na][Mo] QMXBEONRRWKBHZ-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- KNYGDGOJGQXAMH-UHFFFAOYSA-N aluminum copper indium(3+) selenium(2-) Chemical compound [Al+3].[Cu++].[Se--].[Se--].[In+3] KNYGDGOJGQXAMH-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- -1 modified copper indium gallium diselenide Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- GSWAOPJLTADLTN-UHFFFAOYSA-N oxidanimine Chemical compound [O-][NH3+] GSWAOPJLTADLTN-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000012703 sol-gel precursor Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- WAAWAIHPWOJHJJ-UHFFFAOYSA-N tributoxy(propyl)silane Chemical compound CCCCO[Si](CCC)(OCCCC)OCCCC WAAWAIHPWOJHJJ-UHFFFAOYSA-N 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- FHVAUDREWWXPRW-UHFFFAOYSA-N triethoxy(pentyl)silane Chemical compound CCCCC[Si](OCC)(OCC)OCC FHVAUDREWWXPRW-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及用于在金属基底上生产介电层的溶胶组合物，所述溶胶组合物包含：按溶胶组合物的重量计为10％至30％的包含三烷氧基硅烷的前体；按溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm；按溶胶组合物的重量计为4.5％至36％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm；按溶胶组合物的重量计为5％至15％的能够使前体在水中能混溶的溶剂；按溶胶组合物的重量计为0.1％至2％的酸性催化剂，剩余部分为水。
Description
技术领域
本发明涉及用于生产介电涂层，特别地在金属基底上生产介电涂层的溶胶组合物。本发明还涉及介电涂层，涉及所述介电涂层用于制造电子器件、光电子器件特别是太阳能电池的用途。本发明还涉及其方法。
背景技术
太阳能电池通常由数个层构成，其中有基底、背电极、包括吸收层的p-n结和前电极。
当基底为金属的时，其通常必须涂有介电层以将太阳能电池与导电基底隔开。该介电层必须抵抗250V而不产生电弧。其还必须抵抗在太阳能电池的制造期间进行的热循环典型地为了形成CIGS层而在550℃下的退火，而不会分层且不改变特性。
此外，由于要施加在介电层上的层非常薄(微米级)，因此只有介电层非常平滑，其才可以为连续层。因此，介电层的粗糙度(Rz)必须显著低于1μm。
满足先前的要求并具有合适粗糙度的当前解决方案具有应变网络，这导致介电层开裂。减小其内应力会损害粗糙度。
因此，需要在粗糙度、内应力和热稳定性之间具有良好折衷的介电涂层。
发明内容
为此目的，本发明的第一主题包括用于在金属基底上生产介电层的溶胶组合物，所述溶胶组合物包含：
-按溶胶组合物的重量计为10％至30％的包含三烷氧基硅烷的前体，
-按溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
-按溶胶组合物的重量计为4.5％至36％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
-按溶胶组合物的重量计为5％至15％的能够使前体在水中能混溶的溶剂，
-按溶胶组合物的重量计为0.1％至2％的酸性催化剂，
剩余部分为水。
根据本发明的溶胶组合物可以包含：
-按溶胶组合物的重量计为10％至30％的包含三烷氧基硅烷的前体，
-按溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
-按溶胶组合物的重量计为30％至60％的二氧化硅的水分散体，所述二氧化硅的水分散体包含按水分散体的重量计为15％至60％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
-按溶胶组合物的重量计为5％至15％的能够使前体在水中能混溶的溶剂，
-按溶胶组合物的重量计为0.1％至2％的酸性催化剂。
根据本发明的溶胶组合物也可以具有以下列出的单独或组合考虑的任选特征：
-三烷氧基硅烷为通式R'-Si(OR)3的有机官能三烷氧基硅烷，其中R'表示有机官能团以及R表示烷基，
-三烷氧基硅烷为烷基三烷氧基硅烷，
-三烷氧基硅烷选自甲基三烷氧基硅烷、乙基三烷氧基硅烷和丙基三烷氧基硅烷，
-三烷氧基硅烷为甲基三甲氧基硅烷，
-前体为至少一种四烷氧基硅烷和至少一种三烷氧基硅烷的混合物，
-前体的含量为溶胶组合物的15重量％至25重量％，
-溶剂选自醇、酮及其混合物，
-溶剂为丙酮，
-二氧化钛颗粒的尺寸为200nm至1000nm，
-二氧化钛颗粒涂覆有按TiO2颗粒的重量计为2％至6％的氧化铝，
-二氧化硅的水分散体的含量按溶胶组合物的重量计为35％至55％，以及二氧化硅的水分散体包含按水分散体的重量计为40％至55％的二氧化硅颗粒，
-二氧化硅的水分散体包含以下两种不同尺寸范围的二氧化硅颗粒的混合物：50nm至120nm的第一范围和3nm至25nm的第二范围，
-酸性催化剂包括磷酸。
本发明的第二主题包括在其至少一个表面的至少一部分上涂覆有至少10μm的介电层的金属基底，所述至少10μm的介电层包含：
-按介电层的重量计为20％至70％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
-按介电层的重量计为20％至70％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
-按介电层的重量计为5％至18％的聚合的三烷氧基硅烷前体，
-按介电层的重量计为0.1％至2％的酸性催化剂。
本发明的第三主题包括用于生产溶胶组合物的方法，所述方法包括以下步骤：
-提供：
ο10重量份至30重量份的包含三烷氧基硅烷的前体，
ο10重量份至40重量份的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
ο30重量份至60重量份的二氧化硅的水分散体，所述二氧化硅的水分散体包含按水分散体的重量计为15％至60％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
ο5重量份至15重量份的能够使前体在水中能混溶的溶剂，
ο0.1重量份至2重量份的酸性催化剂，
-将组分混合。
本发明的第四主题包括用于在金属基底上生产介电层的溶胶-凝胶方法，所述溶胶-凝胶方法包括以下步骤：
-(i)提供金属基底和溶胶组合物，所述溶胶组合物包含：
ο按溶胶组合物的重量计为10％至30％的包含三烷氧基硅烷的前体，
ο按溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
ο按溶胶组合物的重量计为30％至60％的二氧化硅的水分散体，所述二氧化硅的水分散体包含按水分散体的重量计为15％至60％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
ο按溶胶组合物的重量计为5％至15％的能够使前体在水中能混溶的溶剂，
ο按溶胶组合物的重量计为0.1％至2％的酸性催化剂，
-(ii)将溶胶组合物沉积在金属基底的至少一个表面上，
-(iii)使溶剂蒸发以形成介电层。
根据本发明的溶胶-凝胶方法也可以具有以下列出的单独或组合考虑的任选特征：
-沉积至少20μm的溶胶组合物，
-步骤(iii)在于干燥步骤，所述干燥步骤的金属基底的峰值金属温度为120℃至200℃以及所述干燥步骤的干燥时间为30秒至4分钟，
-该方法还包括步骤(iv)：对介电层进行退火，持续30秒至4分钟，其中金属基底的峰值金属温度为300℃至600℃。
本发明的第五主题包括用于制造太阳能电池的方法，所述方法包括：
-(i)提供在其至少一个表面的至少一部分上涂覆有至少10μm的介电层的金属基底，所述至少10μm的介电层包含：
ο按介电层的重量计为20％至70％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
ο按介电层的重量计为20％至70％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
ο按介电层的重量计为5％至18％的聚合的三烷氧基硅烷前体，
ο按介电层的重量计为0.1％至2％的酸性催化剂，
-(ii)向介电层上沉积基于钼的背电极。
具体实施方式
通过阅读以下描述将更好地理解本发明，以下描述仅为了解释目的而提供，并且决不旨在为限制性的。
应注意，如本文所用，术语“在……上方”和“在……上”均包含性地包括“直接在……上”(在其之间没有设置中间材料、元件或空间)和“间接在……上”(在其之间设置有中间材料、元件或空间)。例如，“在基底上”形成元件可以包括直接在基底上形成元件而在其之间没有中间材料/元件，以及间接地在基底上形成元件而在其之间具有一个或更多个中间材料/元件。
金属基底意指具有平坦形状的元件，即其厚度与其其他尺寸相比是低的。一般来说，其厚度是其宽度的1/500至1/4000。基底可以由单一材料或复合组件制成。可以将碳钢、不锈钢、铝、铜和锌引用为金属材料的非限制性实例。优选碳钢和不锈钢。金属基底可以呈卷材或片材的形式。
本发明的介电涂层由于溶胶组合物而获得。溶胶-凝胶方法为由小分子生产固体材料的方法。该方法用于制造金属氧化物，特别是硅(Si)和钛(Ti)的氧化物。该方法涉及将单体转化为胶体溶液(溶胶)，所述胶体溶液(溶胶)充当离散颗粒或网络聚合物的一体化网络(或凝胶)的前体。典型的前体为金属醇盐。
根据本发明的溶胶组合物首先包含前体，所述前体包含三烷氧基硅烷，优选地未氢化的三烷氧基硅烷。
前体可以特别地为通式R'-Si(OR)3的有机官能三烷氧基硅烷，其中R'表示有机官能团以及R表示烷基。
有机官能三烷氧基硅烷可以特别地选自甲基三甲氧基硅烷、甲基三乙氧基硅烷、甲基三丙氧基硅烷、甲基三丁氧基硅烷、乙基三甲氧基硅烷、乙基三乙氧基硅烷、乙基三丙氧基硅烷、乙基三丁氧基硅烷、丙基三甲氧基硅烷、丙基三乙氧基硅烷、丙基三丙氧基硅烷、丙基三丁氧基硅烷、(3-缩水甘油氧基丙基)三甲氧基硅烷、(二丁基-氧基铝氧基)三乙氧基硅烷、3-氨基丙基三乙氧基硅烷、3-异氰酸基丙基三乙氧基硅烷、3-巯基丙基三乙氧基硅烷、氨基苯基三乙氧基硅烷、十三氟1，1，2，2-四氢辛基三乙氧基硅烷、氯丙基三乙氧基硅烷、戊基三乙氧基硅烷、乙烯基三乙氧基硅烷或苯基三乙氧基硅烷或其混合物。
三烷氧基硅烷优选为烷基三烷氧基硅烷，更优选地选自甲基三烷氧基硅烷、乙基三烷氧基硅烷或丙基三烷氧基硅烷。
三烷氧基硅烷更优选地选自甲基三甲氧基硅烷、甲基三乙氧基硅烷、甲基三丙氧基硅烷、乙基三甲氧基硅烷、乙基三乙氧基硅烷、乙基三丙氧基硅烷、丙基三甲氧基硅烷、丙基三乙氧基硅烷或丙基三丙氧基硅烷。这些三烷氧基硅烷进一步改善介电涂层的耐热性。
由于三烷氧基官能，由前体获得的网络为三价网络，其优选地散布有有机官能团。其与二氧化硅网络相比较小应变，因此裂纹是受限的。网络的柔性可以根据具体情况通过有机官能团的选择来进行调节。
这些基团的效果使得前体也可以为至少一种四烷氧基硅烷和至少一种三烷氧基硅烷的混合物。特别地，其可以为四甲氧基硅烷、四乙氧基硅烷、四丙氧基硅烷或四丁氧基硅烷与甲基三甲氧基硅烷、甲基三乙氧基硅烷、甲基三丙氧基硅烷、甲基三丁氧基硅烷、乙基三甲氧基硅烷、乙基三乙氧基硅烷、乙基三丙氧基硅烷或乙基三丁氧基硅烷的组合。在这种情况下，第一前体的四面体网络与第二前体的三价网络平衡，这限制了网络中的应力。
前体特别地为具有式CH3Si(OCH3)3的有机硅化合物甲基三甲氧基硅烷(MTMOS)。由这种前体形成的膜非常耐温度。在惰性气体下，其在约500℃至600℃开始缓慢降解。
甲基三甲氧基硅烷易于水解并且其缩合在酸性条件下容易控制。因此，其适用时间为至少24小时，这在制造介电涂层的过程中实现一定灵活性。
该前体的聚合步骤如下：
CH3Si(OCH3)3+H2O→OH-Si(CH3)(OCH3)2+CH3-OH
(OCH3)2(CH3)Si-OH+OH-Si(CH3)(OCH3)2→[(OCH3)2(CH3)Si-O-Si(CH3)(OCH3)2]+H-O-H
或者
(OCH3)2(CH3)Si-OCH3+OH-Si(CH3)(OCH3)2→[(OCH3)2(CH3)Si-O-Si(CH3)(OCH3)2]+CH3-O-H
因此，聚合与硅氧烷[Si-O-Si]键的3维网络的形成有关，伴随着H-O-H和R-O-H物质的产生。
前体的含量为溶胶组合物的10重量％至30重量％。观察到低于10重量％，含量不足以获得良好的涂层内聚性。大于30重量％，趋于出现影响电绝缘的微裂纹。优选地，该含量为15重量％至25重量％，这给出了内应力与热稳定性之间的最佳折衷。
在溶胶组合物中，前体可以呈水解形式。说明书中给出的含量范围没有考虑这种水解。特别地，前体的含量范围为未水解前体的含量范围。对于给定的溶胶组合物，可以容易地计算水解前体的含量范围。
溶胶组合物还包含能够使前体在水中能混溶的溶剂，使得要发生的水解是均匀的。
溶剂可以选自醇、酮及其混合物。醇优选地选自在水溶性与沸点之间呈现最佳折衷的一元醇。可能的一元醇为乙醇、丁醇、异丙醇、甲氧基丙醇及其混合物。酮优选地选自丙酮和甲基乙基酮。丙酮是优选的，因为其有利于颗粒的分散，其能与水100％混溶。其也在低温(56℃)但不是太低的温度下蒸发，使得如果将溶胶组合物喷洒在基底上，其不会在喷雾中蒸发。
使用溶剂的混合物，可以有利于溶胶组合物在金属基底上的润湿性并且更好地控制蒸发。
溶剂的含量为溶胶组合物的5重量％至50重量％。低于5重量％，组合物太粘。大于50重量％，稀释太严重并且无法获得具有良好电绝缘的厚层。优选地，该含量为5重量％至15重量％，这代表粘度与稀释度之间的最佳折衷。
溶胶组合物还包含按溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm。TiO2非常稳定，耐高温并且容易分散在水中。优选地，二氧化钛颗粒的含量为20重量％至30重量％。
由于颗粒的中值尺寸，防止了在介电涂层的表面处突出的大颗粒，从而将粗糙度保持在低水平。更优选地，颗粒尺寸为200nm至1000nm。
优选地，对TiO2颗粒的表面进行涂覆以阻止TiO2成光活性的，否则从长远来看，其可能使介电涂层和相应的太阳能电池劣化。表面涂层可以为氧化铝或二氧化硅。优选氧化铝，因为其被认为有助于介电层在热膨胀期间保持其完整性。当用氧化铝涂覆TiO2时，其典型地包含按涂覆有氧化铝的TiO2颗粒的重量计为2％至6％的氧化铝。
TiO2颗粒的表面优选不被羟基、氢聚硅氧烷或二氢聚硅氧烷官能化。
由于TiO2本身无法为介电涂层带来足够的内聚性，因此溶胶组合物还包含按溶胶组合物的重量计为4.5％至36％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm。二氧化硅也为电绝缘体，是化学惰性的并且耐高温。
溶胶组合物优选地包含按水分散体的重量计为14％至30％的二氧化硅颗粒。
由于二氧化硅颗粒比TiO2颗粒显著更小且更不致密，因此介电涂层的表面主要由二氧化硅构成，这降低了涂层的粗糙度。二氧化硅颗粒优选具有3nm至120nm的尺寸。
二氧化硅颗粒的表面优选地不被羟基、氢聚硅氧烷或二氢聚硅氧烷官能化。
任选地，溶胶组合物包含以下两种不同尺寸范围的二氧化硅颗粒的混合物：50nm至120nm的第一范围和3nm至25nm的第二范围。在这种情况下，第二种颗粒尺寸分布的颗粒可以表示二氧化硅颗粒总重量的高至30重量％，优选地10重量％至30重量％。这进一步改善介电涂层的粗糙度。
根据一个优选实施方案，二氧化硅以二氧化硅的水分散体的形式添加至溶胶组合物。在这种情况下，按溶胶组合物的重量计为4.5％至36％的二氧化硅颗粒连同作为溶胶组合物的剩余部分而添加的水一起对应于按溶胶组合物的重量计为30％至60％的二氧化硅的水分散体，所述二氧化硅的水分散体包含按水分散体的重量计为15％至60％的二氧化硅颗粒。二氧化硅的水分散体是为电绝缘体，化学惰性的且耐高温的纯二氧化硅的来源。其也是用于溶胶-凝胶前体的水解的水源。
溶胶组合物优选包含按溶胶组合物的重量计为35％至55％的二氧化硅的水分散体，所述二氧化硅的水分散体包含按水分散体的重量计为40％至55％的二氧化硅颗粒。由于这种浓度，通过溶胶组合物的聚合获得的凝胶更容易干燥并且介电涂层更干燥，这防止其开裂。由于以这种比例存在水，前体的水解在良好的条件下进行。
根据一种变型，在将溶胶组合物的组分混合之前，将二氧化硅的水分散体的pH保持为9至10以限制硅酸盐的出现。可以通过在溶液中添加碱例如氢氧化钠、氧化钠、氢氧化铵或氧化铵来控制pH。
根据另一种变型，二氧化硅在4至5的pH下分散在去离子水中。
溶胶组合物还包含按溶胶组合物的重量计为0.1％至2％的酸性催化剂，优选地0.2％至0.8％。由于其酸性性质，可以获得致密的涂层。该催化剂也控制聚合速度。因此将根据应用过程基于所需的速度来选择催化剂。如果优选快的聚合速度，则将考虑强酸例如盐酸或硫酸。如果溶胶组合物的适用时间必须延长至一天或两天使得组合物可以在其应用之前制备并同时储存，则优选弱酸。弱酸可以选自磷酸、亚磷酸、甲酸、乙酸、乳酸、草酸、柠檬酸、酒石酸、苯甲酸。无机酸由于其热稳定性而是优选的，使得涂层网络不会被碳残留物污染。特别优选磷酸，其三价性质使其非常刚性。
溶胶组合物还包含水作为剩余部分。表述“剩余部分为水”意指即使在前体水解之后仍有水留在溶胶组合物中。由于水的存在，前体的水解在良好的条件下进行，颗粒二氧化硅和TiO2得到很好的稳定和分散，并且溶剂的蒸发得到更好的控制。优选去离子水。
当二氧化硅以水分散体的形式添加时，优选仅通过水分散体提供水。
由于该溶胶组合物，可以在金属基底上获得具有非常低的粗糙度(Ra低于100nm，以及Rz为200纳米至600纳米)而没有针孔的厚于20μm的介电层。这些层可以在加热和冷却期间被加热高至600℃持续数小时而没有裂纹。此外，这些层是防止铁从钢基底扩散的有效屏障，这消除了对钢基底与PV电池之间的屏障层的需求。
溶胶组合物通过将不同组分全部混合在一起来制备。
或者，溶胶组合物为双组分产品。在这种情况下，优选通过混合二氧化钛颗粒、二氧化硅的水分散体和溶剂来制备第一组分。优选通过混合前体和酸性催化剂来制备第二组分。然后在使用溶胶组合物之前将两种组分混合在一起。
任选地，最终将溶胶组合物在1μm下过滤以去除可能的团聚物。
就工艺而言，一旦提供金属基底和溶胶组合物，就将该组合物沉积在基底的至少一个表面的至少一部分上。这可以例如通过浸涂、旋涂、辊涂、狭缝模涂覆、喷洒、喷墨印刷来进行。狭缝模因其提供的表面均匀性而是优选的。
优选以足以获得至少10μm厚的干燥介电层的量施加溶胶组合物。低于此，涂层可能没有足够的介电性。施加的湿溶胶组合物为至少20μm厚。
在接下来的步骤中，溶胶朝着形成包含液相和固相二者的凝胶状网络逐渐演变。最简单的方法为允许时间来发生沉降和溶剂的蒸发，从而获得介电层。优选地，也发生水的蒸发。优选进行干燥步骤以使所施加的膜快速干燥并获得介电层。干燥可以在烘箱中以连续过程或间歇过程通过对流、感应、红外线或任何其他合适的方法进行。更优选地，覆盖有膜的金属基底的峰值金属温度为120℃至200℃，并且干燥时间为30秒至4分钟。
任选地，为了最佳的介电性能，将介电层进一步在惰性气体下退火，以从该层中完全去除任何被捕获在涂层中的水。这样的退火防止水在制造太阳能电池的过程的后续步骤中脱气并因此防止使后续层劣化。退火可以在烘箱中以连续过程或间歇过程通过对流、感应或任何其他合适的方法进行。更优选地，覆盖有介电层的金属基底的峰值金属温度为300℃至600℃，更优选为500℃至600℃，甚至更优选为540℃至560℃，并且干燥时间为30秒至4分钟。
溶胶-凝胶涂层包含20重量％至70重量％的二氧化硅颗粒、20重量％至70重量％的二氧化钛颗粒，涂层的剩余部分包含聚合的前体，即硅氧烷(Si-O-Si)键的三维网络，优选地包含与有机官能团连接的Si原子，以及酸性催化剂。特别地，溶胶-凝胶涂层包含按介电层的重量计为5％至18％的网络和按介电层的重量计为0.1％至2％的酸性催化剂。不同要素的含量之和等于100％。
溶胶-凝胶涂层的特性可以通过SEM(对于颗粒尺寸和性质)、通过X射线荧光(对于Si和Ti含量)和通过IR光谱法(对于SiO2和网络含量)获得。
获得的溶胶-凝胶涂层为至少10μm厚以具有良好的介电特性。其粗糙度Ra低于100nm以及粗糙度Rz低于600nm。其对金属基底的附着性为至少3，如根据ASTM D3359通过胶带测试测量的。其电绝缘性使得持续至少3分钟在250V下用千兆欧姆表在金属基底与沉积在溶胶-凝胶涂层表面上的饱和盐水液滴之间测量的电阻为至少272千兆欧姆。其击穿电压为至少1000V。
将溶胶组合物施加在基底上、干燥以及任选地进行热处理之后，可以沉积构成太阳能电池的不同层。
根据本发明的一种变型，太阳能电池为CIGS太阳能电池。CIGS在此是指具有对于用作薄膜太阳能电池中的吸收层所期望的特性的材料组。铜铟联硒化物(CuInSe2或CIS)及其更高带隙变型铜铟镓联硒化物(Cu(In/Ga)Se2或CIGS)、铜铟铝联硒化物(Cu(In/Al)Se2)、铜铟镓铝联硒化物(Cu(In/Ga/Al)Se2)和这些化合物的具有取代一些硒的硫的任一者都是该组的成员。
CIGS薄膜太阳能电池通常通过首先将基于钼的背电极沉积至诸如玻璃、不锈钢箔、碳钢箔或其他功能性基底材料的基底上来生产。这可以通过RF或DC磁控溅射来进行。基于钼的背电极可以由钼(Mo)的层或钼-钠(Mo/Na)的层或钼-钾(Mo/K)的层制成，或者由复数个Mo和/或Mo/Na和/或Mo/K的子层制成。或者，可以在背电极上添加氮化锆屏障层使得阻止扩散，从而允许用其他金属例如银、铝、铜代替钼。
然后通过已知技术在钼层上沉积相对厚的CIGS层。在先驱技术中，首先使用物理气相沉积(PVD)法(即蒸镀或溅射)、化学浴或电镀法将金属(Cu/In/Ga)沉积至基底上。随后，在扩散炉中在高至约600℃的温度下使携带硒的气体与金属层反应以形成最终的CIGS组合物。最常用的携带硒的气体是硒化氢，其对人毒性极大，在使用其时需要非常注意。第二种技术通过从单独的热蒸镀源将所有CIGS成分共蒸镀到热基底上来避免使用硒化氢气体。在第三种技术中，CIGS层通过使用平面和/或旋转磁控管的DC磁控溅射来沉积。
CIGS层可以由复数个子层制成。在某些实施方案中，各子层具有相同的组成。在另一些实施方案中，子层的组成不同，使得CIGS层具有从至少一个子层到另一个子层的至少一种元素浓度渐变的组成。在一些实施方案中，各子层具有相同的厚度，而在另一些实施方案中，至少两个子层具有不同的厚度。
最常与CIGS吸收体一起使用以形成薄“窗”或“缓冲”层的n型材料为硫化镉(CdS)。其比CIGS层薄得多，并且可以通过化学浴沉积(CBD)或通过DC溅射施加。由于与镉相关的毒性和废物处理问题，可以使用ZnS作为替代物。其可以通过元素锌靶材的AC反应性溅射和硫化氢的注射来制成。
最后，窗或缓冲层用相对厚的透明导电氧化物(其也为n型半导体)覆盖。在过去，使用氧化锌(ZnO)作为传统但更昂贵的氧化铟锡(ITO)的替代物。近来，掺铝的ZnO(AZO)表现出差不多与ITO一样好的性能，并且其已成为行业中的首选材料。其可以通过磁控溅射来制成。
任选地，可以在缓冲层上沉积另外的导电层例如顶部金属化层或钝化层。也可以进行图案化和互连步骤以提供单片集成器件。
或者，由溶胶组合物获得的介电涂层可以用于制造其他电子器件或光电子器件，例如光电晶体管、光电倍增管、发光二极管(LED)。
第一种溶胶组合物通过混合以下来制备：
-在一方面，40g涂覆有4重量％的氧化铝的二氧化钛颗粒(由Chemours TM(DuPontTM)提供的Ti-PureTM R900，中值颗粒尺寸为410nm)、70g包含50重量％的二氧化硅(颗粒尺寸分布D90低于100nm)的二氧化硅的水分散体(由提供的LevasilCT3PL)和15g丙酮，
-在另一方面，30g三甲氧基甲基硅烷和0.5mL作为85％水溶液的磷酸。
然后将这两种组分混合在一起。
第二种溶胶组合物通过混合以下来制备：
-在一方面，40g涂覆有4重量％的氧化铝的二氧化钛颗粒(由Chemours TM(DuPontTM)提供的Ti-PureTM R900，中值颗粒尺寸为410nm)、60g包含50重量％的二氧化硅(颗粒尺寸分布D90低于100nm)的二氧化硅的水分散体(由提供的LevasilCT3PL)和25g工业乙醇，
-在另一方面，30g三甲氧基甲基硅烷和0.5mL作为85％水溶液的磷酸。
然后将这两种组分与25g包含50重量％的二氧化硅(具有基本上单分散(d＝22nm)粒径分布)的二氧化硅的水分散体(由Sigma Aldrich提供的Ludox TM-50)混合在一起。
第三种溶胶组合物通过混合以下来制备：
-在一方面，36g滑石/云母颗粒(由Ymeris Performances Additives提供的 Super，颗粒尺寸D50为3.7μm)、70g包含50重量％的二氧化硅(颗粒尺寸分布D90低于100nm)的二氧化硅的水分散体(由/>提供的Levasil CT3PL)和10g丙酮，
-在另一方面，25g三甲氧基甲基硅烷和1mL作为85％水溶液的磷酸。
然后将这两种组分混合在一起。
第四种溶胶组合物通过混合以下来制备：
-在一方面，40g涂覆有4重量％的氧化铝的二氧化钛颗粒(由Chemours TM(DuPontTM)提供的Ti-PureTM R900，中值颗粒尺寸为410nm)、70g包含50重量％的二氧化硅(颗粒尺寸分布D90低于100nm)的二氧化硅的水分散体(由提供的LevasilCT3PL)和15g丙酮，
-在另一方面，60g三甲氧基甲基硅烷和0.5mL作为85％水溶液的磷酸。
然后将两种组分混合在一起。
第五种溶胶组合物通过混合以下来制备：
-在一方面，40g涂覆有4重量％的氧化铝的二氧化钛颗粒(由Chemours TM(DuPontTM)提供的Ti-PureTM R900，中值颗粒尺寸为410nm)、70g包含50重量％的二氧化硅(颗粒尺寸分布D90低于100nm)的二氧化硅的水分散体(由提供的LevasilCT3PL)和15g丙酮，
-在另一方面，30g三甲氧基甲基硅烷和1mL 30％的氨(碱性催化剂)。
然后将两种组分混合在一起。
溶胶组合物(湿重量％)和用溶胶组合物获得的介电层(干重量％)二者的各要素的含量总结在表1中。
除第五种组合物之外，将所有组合物通过狭缝模涂覆以约50μm的湿厚度施加在钢基底上。将它们干燥，持续1分钟，其中峰值金属温度为170℃。然后将它们退火，持续10分钟，其中峰值金属温度为550℃。第五种溶胶组合物由于碱性催化剂的存在而分层并沉淀，并且无法施加在钢基底上。
从由前四种溶胶组合物获得的前四种介电涂层获得的结果详述于表2中。
根据标准ISO1997(0.5mm/秒，λc＝0.8，行程＝0.5cm)测量粗糙度。
介电性能通过对介电涂层施加250V来评估，所述介电涂层具有饱和盐水液滴(约1cm宽)作为介电涂层与千兆欧姆表的顶电极之间的接触，并且千兆欧姆表的底电极连接至钢基底。电阻必须在3分钟期间保持在272千兆欧姆以上。
击穿电压通过在千兆欧姆表的与具有饱和盐水液滴(约1cm宽)的介电层接触的顶电极与千兆欧姆表的连接至钢基底的底电极之间施加电压来测量。击穿电压必须为至少1000V。
介电涂层在金属基底上的附着性根据ASTM D3359通过胶带测试测量。
从结果明显的是，根据本发明的溶胶组合物在粗糙度、内应力(通过电阻测试评估)、介电性能和热稳定性(在退火期间评估)之间具有良好的折衷。另一方面：
-具有除中值尺寸低于500nm的二氧化钛颗粒之外的颗粒的溶胶组合物未达到与电子应用相容的粗糙度(溶胶组合物3)，
-前体水平高于30％的溶胶组合物由于微裂纹和多孔性而未达到合适的电绝缘(溶胶组合物4)，
-具有碱性催化剂的溶胶组合物不稳定并分层。
表1：
*根据本发明
表2：
N/A：无法获得
Claims (15)
1.一种用于在金属基底上生产介电层的溶胶组合物，所述溶胶组合物包含：
-按所述溶胶组合物的重量计为10％至30％的包含三烷氧基硅烷的前体，
-按所述溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
-按所述溶胶组合物的重量计为4.5％至36％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
-按所述溶胶组合物的重量计为5％至15％的能够使所述前体在水中能混溶的溶剂，
-按所述溶胶组合物的重量计为0.1％至2％的酸性催化剂，
剩余部分为水。
2.根据权利要求1所述的溶胶组合物，其中所述三烷氧基硅烷选自甲基三烷氧基硅烷、乙基三烷氧基硅烷和丙基三烷氧基硅烷。
3.根据权利要求1或2所述的溶胶组合物，其中所述前体为至少一种四烷氧基硅烷和至少一种三烷氧基硅烷的混合物。
4.根据权利要求1所述的溶胶组合物，其中前体的含量为所述溶胶组合物的15重量％至25重量％。
5.根据权利要求1所述的溶胶组合物，其中所述溶剂选自醇、酮及其混合物。
6.根据权利要求1所述的溶胶组合物，其中所述二氧化钛颗粒的尺寸为200nm至1000nm。
7.根据权利要求1所述的溶胶组合物，其中所述二氧化钛颗粒涂覆有按TiO2颗粒的重量计为2％至6％的氧化铝。
8.根据权利要求1所述的溶胶组合物，其中所述二氧化硅颗粒呈以下两种不同尺寸范围的二氧化硅颗粒的混合物形式：50nm至120nm的第一范围和3nm至25nm的第二范围。
9.一种在其至少一个表面的至少一部分上涂覆有包含权利要求1所述的溶胶组合物的至少10μm的介电层的金属基底，所述介电层包含：
-按所述介电层的重量计为20％至70％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
-按所述介电层的重量计为20％至70％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
-按所述介电层的重量计为5％至18％的硅氧烷键的三维网络，
-按所述介电层的重量计为0.1％至2％的酸性催化剂。
10.一种用于生产溶胶组合物的方法，包括以下步骤：
-提供：
○10重量份至30重量份的包含三烷氧基硅烷的前体，
○10重量份至40重量份的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
○30重量份至60重量份的二氧化硅的水分散体，所述二氧化硅的水分散体包含按水分散体的重量计为15％至60％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
○5重量份至15重量份的能够使所述前体在水中能混溶的溶剂，○0.1重量份至2重量份的酸性催化剂，
剩余部分为水，
-将组分混合。
11.一种用于在金属基底上生产介电层的溶胶-凝胶方法，包括以下步骤：
-(i)提供所述金属基底和溶胶组合物，所述溶胶组合物包含：
○按所述溶胶组合物的重量计为10％至30％的包含三烷氧基硅烷的前体，
○按所述溶胶组合物的重量计为10％至40％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
○按所述溶胶组合物的重量计为4.5％至36％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
○按所述溶胶组合物的重量计为5％至15％的能够使所述前体在水中能混溶的溶剂，
○按所述溶胶组合物的重量计为0.1％至2％的酸性催化剂，
剩余部分为水，
-(ii)将所述溶胶组合物沉积在所述金属基底的至少一个表面上，
-(iii)使所述溶剂蒸发以形成介电层。
12.根据权利要求11所述的方法，其中沉积至少20μm的溶胶组合物。
13.根据权利要求11或12所述的方法，其中步骤(iii)为干燥步骤，所述干燥步骤的所述金属基底的峰值金属温度为120℃至200℃以及所述干燥步骤的干燥时间为30秒至4分钟。
14.根据权利要求11所述的方法，还包括步骤(iv)：对所述介电层进行退火，持续30秒至4分钟，其中所述金属基底的峰值金属温度为300℃至600℃。
15.一种用于制造太阳能电池的方法，包括：
-(i)提供在其至少一个表面的至少一部分上涂覆有包含权利要求1所述的溶胶组合物的至少10μm的介电层的金属基底，所述介电层包含：
○按所述介电层的重量计为20％至70％的二氧化钛颗粒，所述二氧化钛颗粒的中值尺寸低于500nm，
○按所述介电层的重量计为20％至70％的二氧化硅颗粒，所述二氧化硅颗粒的颗粒尺寸分布D90低于100nm，
○按所述介电层的重量计为5％至18％的硅氧烷键的三维网络，
○按所述介电层的重量计为0.1％至2％的酸性催化剂，
-(ii)向所述介电层上沉积基于钼的背电极。
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