CN1531512A - 掺锑的金属氧化物的化学气相沉积 - Google Patents
掺锑的金属氧化物的化学气相沉积 Download PDFInfo
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- CN1531512A CN1531512A CNA028119053A CN02811905A CN1531512A CN 1531512 A CN1531512 A CN 1531512A CN A028119053 A CNA028119053 A CN A028119053A CN 02811905 A CN02811905 A CN 02811905A CN 1531512 A CN1531512 A CN 1531512A
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 22
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 22
- 238000005229 chemical vapour deposition Methods 0.000 title claims description 22
- 239000011521 glass Substances 0.000 claims abstract description 88
- 238000000576 coating method Methods 0.000 claims abstract description 71
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 56
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000376 reactant Substances 0.000 claims abstract description 50
- 239000011248 coating agent Substances 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 35
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 25
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims description 57
- 239000011159 matrix material Substances 0.000 claims description 50
- 238000002309 gasification Methods 0.000 claims description 30
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 18
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
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- 238000009792 diffusion process Methods 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 230000004888 barrier function Effects 0.000 claims description 6
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 claims description 6
- -1 oxygenatedchemicals Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 150000001463 antimony compounds Chemical class 0.000 claims description 5
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 2
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- HVYVMSPIJIWUNA-UHFFFAOYSA-N triphenylstibine Chemical compound C1=CC=CC=C1[Sb](C=1C=CC=CC=1)C1=CC=CC=C1 HVYVMSPIJIWUNA-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- OQOGEOLRYAOSKO-UHFFFAOYSA-N 1,1-dichloro-1-nitroethane Chemical compound CC(Cl)(Cl)[N+]([O-])=O OQOGEOLRYAOSKO-UHFFFAOYSA-N 0.000 description 1
- UQRONKZLYKUEMO-UHFFFAOYSA-N 4-methyl-1-(2,4,6-trimethylphenyl)pent-4-en-2-one Chemical group CC(=C)CC(=O)Cc1c(C)cc(C)cc1C UQRONKZLYKUEMO-UHFFFAOYSA-N 0.000 description 1
- PLOURCGNBMFHHN-UHFFFAOYSA-N C(C)OC(=O)[Sn]CC Chemical compound C(C)OC(=O)[Sn]CC PLOURCGNBMFHHN-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
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- GAZVSNAEUUUDEK-JDSLSITLSA-N [(1r,3r,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-hydroxybenzoate Chemical compound O([C@H]1[C@@]2(C)CC[C@H](C1)C2(C)C)C(=O)C1=CC=CC=C1O GAZVSNAEUUUDEK-JDSLSITLSA-N 0.000 description 1
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 1
- NCXOIRPOXSUZHL-UHFFFAOYSA-N [Si].[Ca].[Na] Chemical compound [Si].[Ca].[Na] NCXOIRPOXSUZHL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000005385 borate glass Substances 0.000 description 1
- HRMIYSNVJKPYGX-UHFFFAOYSA-K butan-2-yl(trichloro)stannane Chemical compound CCC(C)[Sn](Cl)(Cl)Cl HRMIYSNVJKPYGX-UHFFFAOYSA-K 0.000 description 1
- YMLFYGFCXGNERH-UHFFFAOYSA-K butyltin trichloride Chemical compound CCCC[Sn](Cl)(Cl)Cl YMLFYGFCXGNERH-UHFFFAOYSA-K 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 230000002650 habitual effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 239000012528 membrane Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- UBOGEXSQACVGEC-UHFFFAOYSA-K phenyltin(3+);trichloride Chemical compound Cl[Sn](Cl)(Cl)C1=CC=CC=C1 UBOGEXSQACVGEC-UHFFFAOYSA-K 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- ZXNKRXWFQRLIQG-UHFFFAOYSA-N silicon(4+);tetraborate Chemical compound [Si+4].[Si+4].[Si+4].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-] ZXNKRXWFQRLIQG-UHFFFAOYSA-N 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- 238000002834 transmittance Methods 0.000 description 1
- MEBRQLCKPRKBOH-UHFFFAOYSA-K trichloro(ethyl)stannane Chemical compound CC[Sn](Cl)(Cl)Cl MEBRQLCKPRKBOH-UHFFFAOYSA-K 0.000 description 1
- YFRLQYJXUZRYDN-UHFFFAOYSA-K trichloro(methyl)stannane Chemical compound C[Sn](Cl)(Cl)Cl YFRLQYJXUZRYDN-UHFFFAOYSA-K 0.000 description 1
- YSCVYRUCAPMZFG-UHFFFAOYSA-K trichlorotin Chemical compound Cl[Sn](Cl)Cl YSCVYRUCAPMZFG-UHFFFAOYSA-K 0.000 description 1
- CPRPKIMXLHBUGA-UHFFFAOYSA-N triethyltin Chemical compound CC[Sn](CC)CC CPRPKIMXLHBUGA-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/245—Oxides by deposition from the vapour phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/245—Oxides by deposition from the vapour phase
- C03C17/2453—Coating containing SnO2
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/211—SnO2
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
- C03C2217/244—Doped oxides with Sb
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/152—Deposition methods from the vapour phase by cvd
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Abstract
玻璃上的掺锑的金属氧化物涂层，优选氧化锡涂层，其制备方法是提供一种均匀的气化反应物的混合物，它包含有机锡化合物和有机锑化合物，水和氧，然后将这反应物之混合物传送到热玻璃板的表面上，这些化合物在此发生反应，从而形成掺锑的金属氧化物涂层，优选氧化锡涂层。按照本发明形成的掺锑的金属氧化物涂层，优选氧化锡涂层,其显示出有着改善的玻璃涂层表面的厚度均匀性，以及提高的涂布/制造效率。
Description
发明领域
本发明通常涉及一种在玻璃上形成金属氧化物涂层的方法，更具体而言，涉及一种采用化学气相沉积法将掺锑的氧化锡涂层涂布在热玻璃基质上的方法。
发明背景
涂膜玻璃制品的典型制造方法是，在采用一种本领域内称为“浮法玻璃制造方法”制造玻璃基质的同时，在该玻璃基质上进行连续涂布。该方法包括将玻璃注入能适当地加以密封的熔锡槽内，然后，在玻璃已足够冷却后，将其转移到与该槽对中的搬运用滚筒(take-away rolls)上，当玻璃横放在该滚筒上前进时玻璃最终冷却，一开始使其通过退火炉，此后使其暴露在环境气氛中一段时间。在玻璃与熔锡槽相接触的同时要使在该方法的悬浮部分内保持非氧化气氛，以防止氧化。在退火炉中要保持大气气氛。各种涂层的化学气相沉积(CVD)能方便地在槽内或退火炉内，或甚至可在它们的中间部分的过渡区内完成，方法是使热玻璃的表面与含有蒸气的化学反应物接触，发生热解分解从而形成金属氧化物涂层。当然，这要求化学反应物具有低于其热解分解温度的气化温度。存在着许多可以被气化的含金属的化合物，采用CVD技术，可使这些化合物在玻璃上形成金属氧化物涂层。最感兴趣的是锡的化合物，它们被气化便能形成氧化锡涂层。
对涂布在玻璃上的某些金属氧化物涂层例如氧化锡涂层所希望的性能特点是，例如低辐射率，低平板电阻，高的光透射率，高的红外线反射率等等，并且通过将掺杂剂引入金属氧化涂层便能改善这些特性。在现有技术中可以用作掺杂剂的材料之一是锑。通常锑是以锑的无机化合物形式提供的，作为实例，例如卤化锑，SbCl3。
在玻璃涂布方法中采用的反应物的物理形态通常是液体，固体，气化的液体或固体，弥散在载气混合物中的液体或固体，或弥散在载气混合物中的气化的液体或固体。化学气相沉积法通常采用气化的液体或固体，它们通常是弥散于载气混合物中。
US6005127公开了一种有机锑路易斯碱加合物，据说这种加合物可用于Sb-离子移植技术并可通过各种型式的化学气相沉积法形成锑化物薄膜。本发明不包括路易斯碱加合物，也不涉及离子移植技术或形成金属锑化物。再者，US6005127仅公开了化学气相沉积的以下方法：化学气相沉积，辅助化学气相沉积(例如激光，光，等离子体，离子等等)。
最理想的是能改进迄今所知的通过CVD将掺锑的氧化锡涂层涂布到热玻璃基质表面上的方法，并借此提高了涂膜玻璃产品的低平板电阻和平板电阻的均匀性，同时将不希望有的，在熟知的无机锑掺杂剂存在时就会出现的前体材料预加反应降至最低程度。最理想的还有希望提供一种比迄今所知的方法费用要低的将掺锑的氧化锡涂层涂布到热玻璃基质表面上的方法。
发明概述
本发明涉及一种将掺锑的金属氧化涂层涂布到热玻璃基质表面上的化学气相沉积方法。优选的金属是锡的化合物。最优选的锡化合物是有机锡化合物。意想不到的是，已发现通过利用一种以下所述的方法，便能改进涂布在玻璃上的掺锑的金属氧化涂层，尤其是氧化锡涂层所希望的性能，这方法：包含：
一种将掺锑的金属氧化物涂层涂布到热玻璃基质表面上的化学气相沉积法，它包含：
a)提供一块热玻璃基质，包括一个在其上面要被沉积一层掺锑的金属氧化物涂层的表面；
b)提供一种均匀的气化反应物的混合物，它包含金属化合物，含氧化合物，水和有机锑化合物，这种有机锑化合物在温度低于550F的条件下将不会与所述含氧化合物或水发生预加反应；
c)将这气化反应物的混合物传送到热玻璃基质的表面上，然后使这混合物起反应，以便使掺锑的金属氧化物的涂层沉积在热玻璃基质的表面上；和
d)使这涂膜玻璃基质冷却到环境温度。
氧气源是本发明的方法所必需的，并优先从空气，气态氧和分子氧中选取。
在一个优选实施方案中，在沉积掺锑的金属氧化物之前，将钠扩散膜，优选二氧化硅涂层，涂布到玻璃基质的表面上。本发明的方法尤其适用于制造具有掺锑的金属氧化物涂层的玻璃和可用于能量效率型建筑用窗户，飞机或机动车的窗户和各种光学装置和电子装置。
共同未决的美国专利申请号09/625921公开了一种沉积在并粘附于玻璃基质上的掺锑的氧化锡薄膜，和沉积在并粘附于掺锑的氧化锡涂层上的掺氟的氧化锡涂层。这样制得的涂膜玻璃制品具有高的日光选择性。美国专利申请号09/625921在此整个地被引入作为参考。
优选实施方案评述
金属氧化物涂层，尤其是掺锑的氧化锡涂层，可以采用本领域内通常称为化学气相沉积(CVD)的方法，使其沉积在热玻璃基质的表面上。按照本发明的方法，使所有反应物相组合，以便形成能被传送到热玻璃基质表面的均匀的气化的反应物流，其中这气化的反应物流起反应，从而使掺锑的金属氧化物涂层沉积在热玻璃基质的表面上。在氧化性气氛中，在热玻璃的表面处必须存在着这种气氛，有机金属化合物，优选有机锡涂层化合物，便会热解分解形成金属/锡氧化物涂层。
本方法通常是在采用浮法玻璃制造方法制造玻璃期间进行的，并发生在悬浮槽，退火炉中或发生在该槽和退火炉之间的过渡区中，此时玻璃仍是热的。提供的玻璃基质其温度通常都是在约750°F到约1500°F范围内的。这些温度是采用浮法玻璃制造方法制造玻璃时在各个阶段中的玻璃的典型温度。更准确地说，涂布方法是在900～1350°F，优选在1100～1280°F的温度下进行的。
适用于本发明方法的玻璃基质包括在制备涂膜玻璃制品领域内熟知的任何常规玻璃基质。在制造机动车辆窗户和平板玻璃中使用的一种典型的玻璃基质一般称为钠钙硅玻璃。其它适用的玻璃通常可称为碱钙硅玻璃，硅硼酸盐玻璃，硅铝酸盐玻璃，硼硅铝酸盐玻璃，磷酸盐玻璃，石英玻璃等，以及它们的组合。优选的玻璃是钠钙硅玻璃。
本发明的CVD反应物优选包含有机锡涂层化合物，该化合物被气化并移送到前置玻璃带处或其附近的位置。可用来实践本发明的适合的有机锡化合物包括，但并不限于具体所列举的那些，二甲基锡二氯化物，二乙基锡二氯化物，二丁基锡二醋酸盐，四甲基锡，甲基锡三氯化物，三乙基锡氯化物，三甲基锡氯化物，乙基锡三氯化物，丙基锡三氯化物，异丙基锡三氯化物，仲丁基锡三氯化物，丁基锡三氯化物，苯基锡三氯化物，乙酯基乙基锡三氯化物，等等，以及它们的组合。这些化合物不仅市场买得到，而且在CVD技术领域内通常是熟知的，它作为前体用来将氧化锡涂层涂布在热玻璃上。优选的有机锡化合物是二甲基锡二氯化物。有机锡化合物，和任选的载气，氧化剂，稳定剂，碳氢化合物，惰性气体等等，使它们气化从而形成气态有机锡反应物流。此处采用的术语气态有机锡反应物流通常包含气化的有机锡化合物，氧化剂和惰性载气。
气化的有机锡化合物可以采用本领域内通晓的任何方法制备。作为实例，例如使分散状或流化状有机锡粉末气化，或在填充床内通过热载气流气化有机锡颗粒，或者将增熔化有机锡化合物注入到热载气流中，或使气泡状载气通过液态有机锡化合物。一种制备含有气化的有机锡化合物的反应物流的优选方法是，在有混合气体的薄膜蒸发器中气化该化合物，作为实例，正如公开于US 5090985中的，该专利在此整个地被引入作为参考。正如以上所指出的，这种通常包含惰性载气例如氦，氮，或氩，或其混合物的气态气流可以任选包括氧化剂例如水或氧。优选载气是氦和氮，和其混合物，并含有氧作为氧化剂。通常将制得的含有气化的有机锡化合物的反应物流加热到约250°F～约450°F的温度，然后将其传送到热玻璃基质表面上的反应区，在最靠近玻璃表面的涂层器的工作面上，该处温度小于或等于大约550°F。
一种含有有机锑化合物，氧化剂和惰性载气的单独的反应物流是本发明的涂布系统的另一种组分。
可用于本发明的有机锑化合物通常可用以下分子式描述。
(R1)XSb(R2)3-X，式中R1是芳基，R2是烷基，X＝3或2。
在上述分子式中，当X＝2时，所涉及的化合物系称为二芳基烷基锑化合物，虽然适用于本发明，然而此类化合物更可能与氧发生预加反应，将在下文中对此作更详细的陈述。
在上述分子式中，当X＝3时，优选的化合物系，三芳基锑化合物便形成。这类化合物的实例是(Mes)3Sb，式中Mes是基(mesityl)或1，3，5-三甲基苯基，(Tolyl)3Sb，Ph3Sb，和(RXC6H5-X)3Sb，式中R是短链型有机族，具有1～4个碳原子，(亦即C1～C4)和X＝1-5。这些中尤其优选Ph3Sb，其理由将在下文中论及。
已经发现少数锑化合物满足在沉积温度下必需是高反应活性的要求，但不与水或氧发生预先反应。已发现上面所述的三芳基锑化合物满足这些准则，故而它们是本发明所优选的化合物。尤其优选Ph3Sb，因为除了它是具有上述所希望性能的三芳基锑化合物外，还有它能获得大量供应。
与常规的无机锑前体材料例如SbCl3不同，当Ph3Sb与有机锡试剂，水和氧一起使用时，它仍是稳定的，不会发生预先反应，所以只产生少量有害的Sb/O/Cl固态化合物。已知许多材料例如SbCl3对水是敏感的，除了与水发生反应形成如上所述的不希望的，不挥发的固态化合物外，它们还具有腐蚀性。
这样的固体物质积集在主涂布装置上，降低了涂布效率，或者在最坏的情况下，会导致涂布作业实际上完全停止。本发明使用对空气和水都是稳定的有机锑前体，将会减少停工时间，这是由于因Sb/O/Cl固体的积集而造成频繁停机维修的情况少了。
在将反应物传送到热玻璃基质的要沉积涂层的表面上之前，使含有有机锑的反应物流与有机锡反应物在某处相组合，但该处优选极接近上述玻璃涂布表面。含有有机锑的反应物流可以采用任何适合的方法，例如上文中所论及的有关有机锑气化的方法，通过气化该化合物而制得。含有机锑的气化的反应物流与含气化的有机锡化合物的反应物流，在将它们传送到热玻璃基质的表面上之前，可以通过将这二种气态气流混合的方法使它们相组合。另一种方法是可以将呈液态或溶液形态的含有有机锑的反应物流引入到含有气化的有机锡化合物的热反应物流中，借此气化这含锑溶液或液态化合物。在组合之后，有机锡和有机锑的气化的反应物，水和含氧化合物被传送到热玻璃的表面，它们在该处相互发生反应，从而在其上沉积出掺锑的氧化锡涂层。
在一个优选实施方案中，有机锡反应物流通过在例如以上所述的那种蒸发器中气化二甲基锡二氯化物和惰性载气例如氮，氦或其混合物的方法形成。然后使所得的气态反应物流与气态氧相组合。同时，使Ph3Sb和水气化，制得的有机锑和水蒸气的气态反应物流与气态有机锡反应物流相组合，从而形成均匀的气态反应物流。将这均匀的气态反应物流传送到热玻璃基质的表面上，其中掺锑的氧化锡涂层被沉积在热玻璃基质的表面上。这均匀的气态反应物流可通过任何合适的涂布装置将其传送到玻璃表面上。在US4504526中阐明了一种优选的涂布装置，该专利在此整个地被引入作为参考。
按照本发明被传送到热玻璃基质表面上的均匀的气态反应物流，优选包含约10％～约60％的氧，约2％～约50％的水，和约0.01％～约4％的有机锑，而最优选的是包含约10％～约50％的氧，约15％～约35％的水，和约0.01％～约0.05％的有机锑(以上所有的百分率均是摩尔％)。这均匀的气态反应物的混合物还包括有机锡化合物，对其要求的浓度是对氧化锡涂层要求的厚度和玻璃基质的线速度的函数。这样，在气态反应物的混合物中所含有机锡的数量要足以能在要求的基质线速度下涂布出要求厚度的涂层，这是本领域内的那些技术人员能理解的。供典型的商业经营用的气态反应物的混合物通常包含约0.01％～约8％的有机锡。
还应指出，当按照本发明形成掺锑的氧化锡涂层时，优选在玻璃基质和掺锑的氧化锡涂层之间涂上一层起钠扩散膜作用的材料。已经发现，当将按照本发明沉积的掺锑的氧化锡涂层，涂布在该处中间带有钠扩散膜的玻璃上时，由此制得的涂膜玻璃制品与直接涂布在玻璃上的不同，它们显示出较低的辐射率，较低的平板电阻和较低的霾现象。这钠扩散涂层优选由二氧化硅形成的涂层。这二氧化硅涂层优选使用常规的CVD技术形成。
在一种更优选的实施方案中，首先将氧化锡薄膜沉积到在其上已沉积了一层二氧化硅薄膜的热玻璃基质的表面上，这样便在玻璃和随后沉积的掺锑的氧化锡涂层之间形成了一个氧化锡/二氧化硅基层结构。在这实施方案中，二氧化硅薄膜不仅起到钠扩散膜作用，而且和第一层(无掺杂的)氧化锡薄膜结合在一起，有助于消除制得的涂膜玻璃制品中的虹色。这样的抗虹色涂层的应用公开于US 4377613中，该专利在此整个地被引入作为参考。
必须指出，工艺条件并不是成功地组合和传送本发明的气化的反应物的重要关键。上文中所述的工艺条件通常公开于用来实践本发明的那些常规条款中。但是，偶尔会发生如上所述的工艺条件不能精确地应用于公开的技术领域内所包含的每种化合物。对于会出现上述情况的那些化合物，都将会被本领域内的那些技术人员很容易地识别出来。在所有这些情况中，本方法既可以通过本领域内的那些普通技术人员所熟知的惯用的改进措施成功地加以实施，例如采取增加或降低温度条件，采取改变有机锡和有机锑组合的速率，采取气化工艺条件的常规改进措施等等，也可以采用适用于实践本发明的不同于常规的其它工艺条件。
还应指出，本发明的方法可以根据要求在玻璃上重复涂布以便形成由若干层组成的涂层，且每一层的组合物未必是同样的。当然，很明显的是在反应物给定的流动速度下，涂层的厚度取决于基质的移动速度。根据这些条件，如需要，可以采用并置二台或更多台涂布装置的办法来增多反应工段。在这种情况下，在涂层已有时间冷却之前，逐次涂布的涂层被重叠形成了一个特别均匀的整体涂层。
通过参阅那些足以代表本发明的具体实施方案能更容易地理解本发明。但是，必须明白，所提供的这些具体的实施方案目的只是为了阐明本发明，并必须明白，可以采用与专为阐明用的实施方案不同的方法来实践本发明，只要该方法没有违反本发明的精神和范围。
实施例
实例1和实例2
以下的实验条件适用于实例1和实例2。
一台实验室用加热炉，它有一个活动传送装置用来移动一块玻璃板，或数块玻璃板，以200英寸/分钟的速度通过上述加热炉，它还包括单独一台10英寸宽的双向涂布器，这涂布器适用于将气化的反应物传送到玻璃板的表面，以便通过化学气相沉积形成一层薄膜或薄膜叠层。
玻璃板被加热到近似1170°F，而位于反应釜表面处的涂布器，亦即最靠近玻璃表面的部分，该处温度大约为500°F。
各种前体材料的制备通过采用称为“起泡器”的多路反应物源聚集室来实现，醋酸乙酯(EtOAc)，三苯锑(Ph3Sb)和二甲基锡二氯化物(Me2SnCl2)各有一个起泡器，它们被保持在特定的温度下。将氦气以特定的流速引人起泡器内。
特定源或起泡器的温度和流速如下：
起泡器
EtOAc
Ph3Sb
Me2SnCl2
温度 97°F 465°F 355°F
氦流速 0.5～0.75slm 1.0slm 1.2slm
将制得的反应物连同氧(O2)和水(H2O)一起引人实验室用涂布器中，氧以5.25slm的流速引人，水以12.4slm的流速引人。
上述各种反应物在涂布器中被组合，以便在此状况下将掺锑氧化锡涂层沉积在清洁的钠钙硅玻璃板上，该玻璃板上已预先沉积了一层200厚度的SiO2层。
薄膜厚度
平板电阻
Tvis
Tsol
实例1 1951 142欧姆/方 63％ 48％
实例2 2158 119欧姆/方 67％ 55％
薄膜厚度由轮廓测定仪测量确定。
Tvis是可见光谱段(400nm～800nm)中的光通过涂膜玻璃的透光度。
Tsal是总的日光通过涂膜玻璃的透光度。
还应指出，在实例1中通过EtoAc起泡器的He流速是0.75slm，在实例2中是0.50slm。其它的参数见前面对二个实例的陈述。
由这些试验生成的薄膜的厚度和导电率是均匀的，显示出低成雾现象和良好的日光选择吸附性。
实例3
还已发现，可以接受的掺锑的氧化锡薄膜可以通过采用溶解于醋酸乙酯(EtoAc)的芳基锑化合物，例如三苯锑(Ph3Sb)的溶液制得。其它合适的溶剂包括，但不限于这些，己烷，甲苯，二氯甲烷和乙腈。使惰性气体成气泡状通过气态二甲基锡二氯化物(Me2SnCl2)，如在实例1和实例2中那样。这二种反应物流都与氧和水相组合，如在实例1和实例2中那样。
实例3所采用的实验室用加热炉的状况和涂布器与实例1和实例2的相同。
包含18wt％Ph3Sb的Ph3Sb/EtOAc反应物流，以11厘米3/分钟的流速流动，它与由成气泡状的惰性气体以1.2slm的流速通过气态Me2SnCl2所产生的反应物流Me2SnCl2相组合，连同以5.25slm流速流动的氧和以12.4slm流速流动的水一起，在钠钙硅基质上生成一层薄膜，这基质上预先沉积有一层200的二氧化硅膜层，上述沉积的薄膜具有以下特性：
薄膜厚度
平板电阻
T vis
T sol
实例3 ≈2000 135欧姆/方 74％ 58％
本发明已公开于被认为是优选的实施方案中，可是必须明白，所提供的这些具体的实施方案目的只是为了阐明本发明，并必须明白，可以采用与专为阐明用的实施方案不同的方法来实践本发明，只要这方法没有违反本发明的精神和范围。
Claims (18)
1.一种化学气相沉积法，它将掺锑的金属氧化物涂层涂布到热玻璃基质表面上，它包含：
a)提供一块热玻璃基质，包括一个在其上面要被沉积一层掺锑的金属氧化物涂层的表面；
b)提供一种均匀的气化反应物的混合物，它包含金属化合物，含氧化合物，水和有机锑化合物，这种有机锑化合物在温度低于550°F的条件下将不会与所述含氧化合物或水发生预加反应；
c)将气化反应物的混合物传送到热玻璃基质的表面上，然后使这混合物起反应，以便使掺锑的金属氧化物的涂层沉积在热玻璃基质的表面上；和
d)使这涂膜玻璃基质冷却到环境温度。
2.权利要求1的方法，其中所述有机锑化合物是以下形式的化合物：(R1)xSb(R2)3-x式中R1是芳族，R2是烷基，和X＝3或2。
3.权利要求1的方法，其中所述有机锑化合物是二芳基烷基锑化合物。
4.权利要求1的方法，其中所述有机锑化合物是三芳基锑化合物，它选自：(Mes)3Sb，Ph3Sb，(Tolyl)3Sb，和(RxC6H5-x)3Sb，(式中R是短链型有机族，具有1～4个碳原子)，和X＝1-5。
5.权利要求1的方法，其中所述有机锑化合物是Ph3Sb。
6.一种化学气相沉积法，它将掺锑的氧化锡涂层涂布在热玻璃基质表面上，它包含：
a)提供一块热玻璃基质，包括一个在其上面要被沉积一层掺锑的氧化锡涂层的表面；
b)提供一种均匀的气化反应物的混合物，它包含锡的化合物，氧，水和有机锑化合物，这种有机锑化合物在温度低于550°F的条件下将不会与所述氧或水发生预加反应；
c)将气化反应物的混合物传送到热玻璃基质的表面上，然后使这混合物起反应，以便使掺锑的氧化锡的涂层沉积在热玻璃基质的表面上；和
d)使这涂膜玻璃基质冷却到环境温度。
7.权利要求6的方法，其中所述锡前体是有机锡化合物。
8.权利要求6的方法，其中所述锡前体是二甲基锡二氯化物。
9.权利要求6的方法，其中所述涂布方法是作为浮法玻璃制造方法的一部分进行的。
10.权利要求9的方法，其中所述涂布方法是在悬浮槽中，或在其附近进行的。
11.权利要求10的方法，其中所述涂布方法是在900～1350°F温度下进行的。
12.权利要求11的方法，其中所述涂布方法是在1100～1280°F温度下进行的。
13.权利要求11的方法，其中所述沉积的涂层厚度为1000～5000。
14.权利要求12的方法，其中所述沉积的涂层厚度为1000～3500。
15.权利要求1的方法，其中在沉积含锑涂层之前先将一层色彩抑制涂层涂布到其上面要沉积上述含锑涂层的基质上。
16.权利要求1的方法，其中所述有机锑化合物基本上是与水和氧不会发生反应的。
17.一种化学气相沉积法，它将掺锑的金属氧化物涂层涂布到热玻璃基质表面上，它包含：
a)提供一块热玻璃基质，包括一个在其上面要被沉积一层掺锑的金属氧化物涂层的表面；
b)提供一种钠扩散膜涂层并将其直接沉积在上述热玻璃基质上；
c)提供一种均匀的气化反应物的混合物，它包含金属化合物，含氧化合物，水和有机锑化合物，这种有机锑化合物在温度低于550°F的条件下将不会与所述含氧化合物或水发生预加反应；
d)将气化反应物的混合物传送到热玻璃基质的表面上，然后使这混合物起反应，以便使掺锑的金属氧化物的涂层沉积在热玻璃基质的表面上；和
e)使这涂膜玻璃基质冷却到环境温度。
18.权利要求17的方法，其中钠扩散膜涂层是二氧化硅。
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| US09/836,647 US6521295B1 (en) | 2001-04-17 | 2001-04-17 | Chemical vapor deposition of antimony-doped metal oxide and the coated article made thereby |
| US09/836,647 | 2001-04-17 |
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| GB8630918D0 (en) | 1986-12-24 | 1987-02-04 | Pilkington Brothers Plc | Coatings on glass |
| US5090985A (en) | 1989-10-17 | 1992-02-25 | Libbey-Owens-Ford Co. | Method for preparing vaporized reactants for chemical vapor deposition |
| JP3201209B2 (ja) | 1994-03-29 | 2001-08-20 | 日本板硝子株式会社 | 建築物用ガラス |
| GB2302102B (en) | 1995-06-09 | 1999-03-10 | Glaverbel | A glazing panel having solar screening properties and a process for making such a panel |
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- 2002-04-09 JP JP2002581347A patent/JP4290993B2/ja not_active Expired - Lifetime
- 2002-04-09 RU RU2003132541/03A patent/RU2302393C2/ru active
- 2002-04-09 BR BRPI0208966-1A patent/BR0208966A/pt not_active Application Discontinuation
- 2002-04-09 CN CNB028119053A patent/CN1263696C/zh not_active Expired - Lifetime
- 2002-04-09 MX MXPA03009494A patent/MXPA03009494A/es active IP Right Grant
- 2002-04-09 PL PL02371598A patent/PL371598A1/xx unknown
- 2002-04-09 EP EP02762022.8A patent/EP1379476B1/en not_active Expired - Lifetime
- 2002-04-09 WO PCT/US2002/011120 patent/WO2002083588A1/en active Application Filing
- 2002-04-09 KR KR10-2003-7013529A patent/KR20030092075A/ko active IP Right Grant
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104736740A (zh) * | 2012-12-28 | 2015-06-24 | 财团法人工业技术研究院 | 氧化锡膜及其制造方法 |
| CN105951061A (zh) * | 2012-12-28 | 2016-09-21 | 财团法人工业技术研究院 | 氧化锡膜及其制造方法 |
| CN104736740B (zh) * | 2012-12-28 | 2016-10-19 | 财团法人工业技术研究院 | 氧化锡膜及其制造方法 |
| CN105951061B (zh) * | 2012-12-28 | 2018-07-13 | 财团法人工业技术研究院 | 氧化锡膜及其制造方法 |
| CN113924279A (zh) * | 2019-05-20 | 2022-01-11 | 皮尔金顿集团有限公司 | 减小涂覆的玻璃制品的发射率的方法 |
| CN115196884A (zh) * | 2022-06-30 | 2022-10-18 | 深圳市楠轩光电科技有限公司 | 一种光学玻璃镀膜方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1263696C (zh) | 2006-07-12 |
| JP2005508819A (ja) | 2005-04-07 |
| BR0208966A (pt) | 2006-11-28 |
| US6521295B1 (en) | 2003-02-18 |
| EP1379476B1 (en) | 2017-10-04 |
| WO2002083588A1 (en) | 2002-10-24 |
| KR20030092075A (ko) | 2003-12-03 |
| MXPA03009494A (es) | 2004-02-12 |
| EP1379476A1 (en) | 2004-01-14 |
| JP4290993B2 (ja) | 2009-07-08 |
| RU2302393C2 (ru) | 2007-07-10 |
| PL371598A1 (en) | 2005-06-27 |
| RU2003132541A (ru) | 2005-04-27 |
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