CN117304719A - Preparation method of low-refractive-index silicon dioxide film - Google Patents
Preparation method of low-refractive-index silicon dioxide film Download PDFInfo
- Publication number
- CN117304719A CN117304719A CN202311259847.7A CN202311259847A CN117304719A CN 117304719 A CN117304719 A CN 117304719A CN 202311259847 A CN202311259847 A CN 202311259847A CN 117304719 A CN117304719 A CN 117304719A
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- Prior art keywords
- acid
- parts
- refractive index
- silicon dioxide
- minutes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 37
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 10
- -1 siloxane compound Chemical class 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000004528 spin coating Methods 0.000 claims abstract description 5
- 229910021426 porous silicon Inorganic materials 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 9
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 9
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 235000019253 formic acid Nutrition 0.000 claims description 8
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 8
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 235000011054 acetic acid Nutrition 0.000 claims description 6
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 6
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 6
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 5
- WLJVXDMOQOGPHL-PPJXEINESA-N 2-phenylacetic acid Chemical compound O[14C](=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-PPJXEINESA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229930182478 glucoside Natural products 0.000 claims description 4
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims description 4
- 229940011051 isopropyl acetate Drugs 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000005711 Benzoic acid Substances 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims description 3
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 3
- UAEPNZWRGJTJPN-UHFFFAOYSA-N Methylcyclohexane Natural products CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 3
- 235000021314 Palmitic acid Nutrition 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000010233 benzoic acid Nutrition 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 3
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 claims description 3
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- 229960002446 octanoic acid Drugs 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000011007 phosphoric acid Nutrition 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- 229940090181 propyl acetate Drugs 0.000 claims description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- 229940005605 valeric acid Drugs 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical group CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 14
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000005456 glyceride group Chemical group 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- HEBRGEBJCIKEKX-UHFFFAOYSA-M sodium;2-hexadecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HEBRGEBJCIKEKX-UHFFFAOYSA-M 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/455—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application the coating or impregnating process including a chemical conversion or reaction
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of semiconductor materials, and particularly relates to a preparation method of a low-refractive-index silicon dioxide film, which comprises the following steps: preparing a low refractive index silica coating solution; the solution is filtered under pressure by using a filter element, and the solution is uniformly coated on a silicon wafer at 3000rpm/min by using a spin coating method; placing the silicon wafer on a baking tray, heating at 80 ℃ for 2 minutes, heating at 150 ℃ for 2 minutes, and heating at 300 ℃ for 10 minutes to form a porous silicon dioxide film; the low-refractive-index silicon dioxide coating solution comprises the following components in parts by weight: 16-20 parts of siloxane compound, 8-12 parts of alkyl quaternary ammonium salt, 1-2 parts of catalyst, 1-2 parts of surfactant with solid content of 1.75%, 100-120 parts of solvent and 10-15 parts of deionized water. The invention can prepare the silicon dioxide film with the refractive index below 1.2, has simple preparation device, and is convenient for economically and efficiently finishing large-area coating and coating of components with complex forms.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a preparation method of a low-refractive-index dioxide film.
Background
Silicon dioxide films have been widely used in the fields of semiconductors, microwaves, optoelectronics, optical devices, film sensors, and the like with their excellent properties. Silicon oxide films are used in microelectronics as diffusion masking layers, insulating gates for MOS devices, insulating spacers for multilayer wiring, passivation protection layers for device surfaces, and the like. For silicon dioxide films used in microelectronics and sensor technology, electrical performance indicators such as dielectric constant, breakdown field strength, insulation resistance, fixed charge and movable charge density of the silicon dioxide film are of interest. The silicon dioxide film applied to the field of optical coating is more focused on the index of optical performance such as refractive index, extinction coefficient and transparent interval of the film layer.
The introduction of porosity can effectively reduce the refractive index of the material, so that the mesoporous material is widely applied to the aspects of chemical sensing, novel photoelectric materials and the like. For example, patent CN111253854A, CN101016415B is all laid out around the subject of porous silica films. The technology in the patent has the defects of high equipment precision requirement, high equipment investment and high process difficulty.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method of a low-refractive-index silicon dioxide film.
In order to achieve the above object, the present invention provides a method for preparing a low refractive index silica film, comprising:
preparing a low refractive index silica coating solution;
the solution is filtered under pressure by using a filter element, and the solution is uniformly coated on a silicon wafer at 3000rpm/min by using a spin coating method;
placing the silicon wafer on a baking tray, heating at 80 ℃ for 2 minutes, heating at 150 ℃ for 2 minutes, and heating at 300 ℃ for 10 minutes to form a porous silicon dioxide film;
the low-refractive-index silicon dioxide coating solution comprises the following components in parts by weight: 16-20 parts of siloxane compound, 8-12 parts of alkyl quaternary ammonium salt, 1-2 parts of catalyst, 1-2 parts of surfactant with solid content of 1.75%, 100-120 parts of solvent and 10-15 parts of deionized water.
Further, the siloxane compound is one or more of trimethoxysilane, methyltriethoxysilane and ethyl orthosilicate.
Further, the alkyl quaternary ammonium salt is dodecyl trimethyl ammonium chloride.
Further, the catalyst is one or more of hydrochloric acid, nitric acid, boric acid, hydrofluoric acid, sulfuric acid, carbonic acid, phosphoric acid, formic acid, acetic acid, propionic acid, butyric acid, caprylic acid, oxalic acid, malonic acid, succinic acid, maleic acid, tartaric acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, valeric acid, caproic acid, capric acid, palmitic acid and acrylic acid.
Further, the surfactant is one or more of stearic acid, sodium dodecyl benzene sulfonate, alkyl glucoside and fatty glyceride.
Further, the solvent is one or more of acetone, isopropanol, n-butanol, PGMEA, pentane, hexane, octane, formic acid, acetic acid, diethyl ether, anisole, propanol, 2-propanol, butanol, 2-butanol, amyl alcohol, butyl acetate, tributylmethyl ethyl ether, isopropyl acetate, methyl ethyl ketone, dimethyl sulfoxide, isopropyl benzene, ethyl acetate, ethyl formate, isobutyl acetate, methyl acetate, 3-methyl-1-butanol, methyl isobutyl ketone, 2-methyl-1-propanol, propyl acetate, cyclohexane, and cyclohexanone.
The invention uses the coating containing the hydrolysate of the siloxane compound, the thermal decomposition component, the catalyst, the surfactant and the solvent to coat on the silicon wafer, and the thermal decomposition component volatilizes when heating and solidifying, so that the silicon dioxide film with multiple pores and refractive index below 1.2 can be formed, and the preparation device is simple, thereby being convenient for economically and efficiently completing large-area coating and coating of components with complex forms.
Detailed Description
The present invention will be described in detail with reference to the following specific embodiments, which are not to be construed as being limited thereto.
The invention provides a preparation method of a low-refractive-index silicon dioxide film, which comprises the following steps: preparing a low refractive index silica coating solution; the solution is filtered under pressure by using a filter element, and the solution is uniformly coated on a silicon wafer at 3000rpm/min by using a spin coating method; the silicon wafer is placed on a baking tray and heated at 80 ℃ for 2 minutes, at 150 ℃ for 2 minutes and at 300 ℃ for 10 minutes to form the porous silicon dioxide film.
In the invention, the low refractive index silica coating solution comprises the following components in parts by weight: 16-20 parts of siloxane compound, 8-12 parts of alkyl quaternary ammonium salt, 1-2 parts of catalyst with solid content of 1.75%, 1-2 parts of surfactant, 100-120 parts of solvent and 10-15 parts of deionized water.
Wherein the siloxane compound is one or more of trimethoxy silane, methyltriethoxy silane and ethyl orthosilicate. The alkyl quaternary ammonium salt is dodecyl trimethyl ammonium chloride. The catalyst is one or more of hydrochloric acid, nitric acid, boric acid, hydrofluoric acid, sulfuric acid, carbonic acid, phosphoric acid, formic acid, acetic acid, propionic acid, butyric acid, caprylic acid, oxalic acid, malonic acid, succinic acid, maleic acid, tartaric acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, valeric acid, caproic acid, capric acid, palmitic acid and acrylic acid. The surfactant is one or more of stearic acid, sodium dodecyl benzene sulfonate, alkyl glucoside and fatty glyceride. The solvent is one or more of acetone, isopropanol, n-butanol, PGMEA, pentane, hexane, octane, formic acid, acetic acid, diethyl ether, anisole, propanol, 2-propanol, butanol, 2-butanol, amyl alcohol, butyl acetate, tributylmethyl ethyl ether, isopropyl acetate, methyl ethyl ketone, dimethyl sulfoxide, isopropyl benzene, ethyl acetate, ethyl formate, isobutyl acetate, methyl acetate, 3-methyl-1-butanol, methyl isobutyl ketone, 2-methyl-1-propanol, propyl acetate, cyclohexane and cyclohexanone.
The invention uses the coating containing the hydrolysate of the siloxane compound, the thermal decomposition component, the catalyst, the surfactant and the solvent to coat on the silicon wafer, and the thermal decomposition component volatilizes when heating and solidifying, so that the silicon dioxide film with multiple pores and refractive index below 1.2 can be formed, and the preparation device is simple, thereby being convenient for economically and efficiently completing large-area coating and coating of components with complex forms.
The following is a description of the method for preparing a silica film according to the present invention by way of specific examples:
example 1:
9.5g of ethyl orthosilicate, 8.5g of methyltriethoxysilane, 10g of dodecyl trimethyl ammonium chloride, 1.5g of nitric acid, 105g of n-butanol and 15g of deionized water are added into a 250m l flask, mixed and stirred for 48 hours at normal temperature, and 1g of stearic acid with 1.75% of solid content is added to form a low-refractive-index silica coating solution; the low refractive index silica solution was pressure filtered using a 0.2 micron filter cartridge, uniformly coated onto an 8 inch silicon wafer using spin coating at 3000rpm/min, and the wafer was placed on a baking pan and heated at 80 c for 2 minutes, 150 c for 2 minutes, and 300 c for 10 minutes.
Example 2:
the siloxane compound was 16g trimethoxysilane, the alkyl quaternary ammonium salt was 8g dodecyltrimethylammonium chloride, the catalyst was 0.5g hydrochloric acid, 0.5g formic acid, the solvent was 30g acetone, 70g acetone, 10g deionized water, the surfactant was 1g sodium dodecylbenzenesulfonate, 1g alkyl glucoside, and the other conditions were the same as in the example.
Example 3:
the conditions were the same as in example 1 except that the siloxane compound was selected from 4g trimethoxysilane, 8g methyltriethoxysilane, 8g ethylorthosilicate, the alkyl quaternary ammonium salt was selected from 12g dodecyltrimethylammonium chloride, the catalyst was selected from 1g nitric acid, 0.5g formic acid, 0.5 phenylacetic acid, the solvent was selected from 60g ethyl acetate, 40g 3-methyl-1-butanol, 20g isopropyl acetate, 12g deionized water, the surfactant was selected from 1.5g fatty acid glyceride.
Example 4:
the siloxane compound was selected from 9.5g of ethyl orthosilicate and 8.5g of trimethoxysilane, and the other conditions were the same as in example 1.
Comparative example 1:
the other conditions were the same as in example 1 without adding a surfactant.
Comparative example 2:
the surfactant was sodium hexadecyl benzene sulfonate, and the other conditions were the same as in example 1.
Comparative example 3:
the surfactant solids content was 3% and the rest of the conditions were the same as in example 1.
Comparative example 4:
heating was performed at 300℃for 7 minutes, and the other conditions were the same as in example 1.
Comparative example 5:
heating was performed at 300℃for 20 minutes, and the other conditions were the same as in example 1.
Comparative example 6:
the coating speed was 1000rpm/min and the heating was carried out at 300℃for 20 minutes, the other conditions being the same as in example 1.
Comparative example 7:
the coating speed was 2000rpm/min and the heating was carried out at 300℃for 20 minutes, the other conditions being the same as in example 1.
The results of the above experiments are shown in the following table:
uniformity of film surface% | Film thickness/nm | Refractive index | Extinction coefficient | |
Example 1 | 5.04 | 181.73 | 1.17 | 0.0019 |
Example 2 | 5.01 | 182.35 | 1.19 | 0.0017 |
Example 3 | 5.01 | 181.65 | 1.18 | 0.0018 |
Example 4 | 5.10 | 178.49 | 1.20 | 0.0015 |
Comparative example 1 | Film formation prevention | / | / | / |
Comparative example 2 | 4.77 | 194.30 | 1.31 | 0.00021 |
Comparative example 3 | Poor film surface | / | / | / |
Comparative example 4 | 6.47 | 177.28 | 1.29 | 0.0017 |
Comparative example 5 | 6.96 | 180.30 | 1.21 | 0.0014 |
Comparative example 6 | 2.58 | 308.90 | 1.19 | 0.00028 |
Comparative example 7 | 2.0 | 226.20 | 1.19 | 0.00024 |
From the above experimental data, the refractive index of the silica thin film prepared by the low refractive index silica thin film preparation method of the present invention can be 1.2 or less.
The above description is only one embodiment of the present invention and is not intended to limit the present invention, and various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing a low refractive index silica film, comprising:
preparing a low refractive index silica coating solution;
the solution is filtered under pressure by using a filter element, and the solution is uniformly coated on a silicon wafer at 3000rpm/min by using a spin coating method;
placing the silicon wafer on a baking tray, heating at 80 ℃ for 2 minutes, heating at 150 ℃ for 2 minutes, and heating at 300 ℃ for 10 minutes to form a porous silicon dioxide film;
the low-refractive-index silicon dioxide coating solution comprises the following components in parts by weight: 16-20 parts of siloxane compound, 8-12 parts of alkyl quaternary ammonium salt, 1-2 parts of catalyst, 1-2 parts of surfactant with solid content of 1.75%, 100-120 parts of solvent and 10-15 parts of deionized water.
2. The method for producing a low refractive index silica film according to claim 1, wherein the siloxane compound is one or more of trimethoxysilane, methyltriethoxysilane, and ethyl orthosilicate.
3. The method for producing a low refractive index silica film according to claim 1, wherein the alkyl quaternary ammonium salt is dodecyl trimethyl ammonium chloride.
4. The method for preparing a low refractive index silica film according to claim 1, wherein the catalyst is one or more of hydrochloric acid, nitric acid, boric acid, hydrofluoric acid, sulfuric acid, carbonic acid, phosphoric acid, formic acid, acetic acid, propionic acid, butyric acid, caprylic acid, oxalic acid, malonic acid, succinic acid, maleic acid, tartaric acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, valeric acid, caproic acid, capric acid, palmitic acid, and acrylic acid.
5. The method for producing a low refractive index silica film according to claim 1, wherein the surfactant is one or more of stearic acid, sodium dodecylbenzenesulfonate, alkyl glucoside, and fatty acid glyceride.
6. The method for producing a low refractive index silica film according to claim 1, wherein the solvent is one or more of acetone, isopropyl alcohol, n-butanol, PGMEA, pentane, hexane, octane, formic acid, acetic acid, diethyl ether, anisole, propanol, 2-propanol, butanol, 2-butanol, pentanol, butyl acetate, tributylmethylethyl ether, isopropyl acetate, methyl ethyl ketone, dimethyl sulfoxide, isopropyl benzene, ethyl acetate, ethyl formate, isobutyl acetate, methyl acetate, 3-methyl-1-butanol, methyl isobutyl ketone, 2-methyl-1-propanol, propyl acetate, cyclohexane, and cyclohexanone.
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CN1824691A (en) * | 2004-11-24 | 2006-08-30 | 三星康宁株式会社 | Method of preparing mesoporous thin film having low dielectric constant |
JP2006350025A (en) * | 2005-06-16 | 2006-12-28 | Ulvac Japan Ltd | Ultra-low refractive index film and method for fabricating the same |
CN101016415A (en) * | 2006-02-07 | 2007-08-15 | 东京应化工业株式会社 | Composition for forming low refractive index silica-based film |
CN101983223A (en) * | 2008-04-02 | 2011-03-02 | 三井化学株式会社 | Composition and method for production thereof, porous material and method for production thereof, interlayer insulating film, semiconductor material, semiconductor device, and low-refractive-index surface protection film |
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Patent Citations (4)
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CN1824691A (en) * | 2004-11-24 | 2006-08-30 | 三星康宁株式会社 | Method of preparing mesoporous thin film having low dielectric constant |
JP2006350025A (en) * | 2005-06-16 | 2006-12-28 | Ulvac Japan Ltd | Ultra-low refractive index film and method for fabricating the same |
CN101016415A (en) * | 2006-02-07 | 2007-08-15 | 东京应化工业株式会社 | Composition for forming low refractive index silica-based film |
CN101983223A (en) * | 2008-04-02 | 2011-03-02 | 三井化学株式会社 | Composition and method for production thereof, porous material and method for production thereof, interlayer insulating film, semiconductor material, semiconductor device, and low-refractive-index surface protection film |
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