CN107429390A - 制备挠性有机‑无机层压材料的方法 - Google Patents
制备挠性有机‑无机层压材料的方法 Download PDFInfo
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- CN107429390A CN107429390A CN201680017247.1A CN201680017247A CN107429390A CN 107429390 A CN107429390 A CN 107429390A CN 201680017247 A CN201680017247 A CN 201680017247A CN 107429390 A CN107429390 A CN 107429390A
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- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
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- YADSGOSSYOOKMP-UHFFFAOYSA-N lead dioxide Inorganic materials O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
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- RPZHFKHTXCZXQV-UHFFFAOYSA-N mercury(I) oxide Inorganic materials O1[Hg][Hg]1 RPZHFKHTXCZXQV-UHFFFAOYSA-N 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
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- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 description 1
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 description 1
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- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910000489 osmium tetroxide Inorganic materials 0.000 description 1
- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 description 1
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- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229910052832 pyrope Inorganic materials 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- YSZJKUDBYALHQE-UHFFFAOYSA-N rhenium trioxide Chemical compound O=[Re](=O)=O YSZJKUDBYALHQE-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052834 spessartine Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- VJHDVMPJLLGYBL-UHFFFAOYSA-N tetrabromogermane Chemical compound Br[Ge](Br)(Br)Br VJHDVMPJLLGYBL-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
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
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- 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
- C23C16/44—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 method of coating
- C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
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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
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- 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
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- 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
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- 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
- C23C16/44—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 method of coating
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- 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
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Abstract
本发明属于制备挠性有机‑无机层压材料的方法的领域。具体而言,本发明涉及一种制备层压材料的方法,该方法包括至少两次包含以下的序列:(a)通过进行3至150个原子层沉积方法的循环来沉积无机层,和(b)通过进行1至3个分子层沉积方法的循环来沉积包含氮的有机层。
Description
本发明属于通过原子层沉积制备挠性有机-无机层压材料以及包含挠性有机-无机层压材料的阻挡膜的方法的领域。
电子器件由于其对湿气和氧气的高敏感性需要有效包封和钝化。典型地,无机材料如氧化物、氮化物、碳化物或玻璃由于其显示出优异湿气和氧气阻挡性能而用作阻挡材料。然而,无机材料由于其刚性而强烈限制电子器件的形状因子。此外,例如大型玻璃片的脆性使得制备方法困难并且昂贵。含有材料如玻璃的电子器件受机械应力易于断裂。
US 2010/0 178 481 A1公开由两个无机非二氧化硅层组成的阻挡层,其间存在一个挠性层。然而,该阻挡层在弯曲之后,尤其是在围绕小半径弯曲之后显示出不令人满意的阻挡性能。
本发明的目的为提供一种制备具有高水和氧气阻挡性能的薄膜的方法。同时旨在提供一种制备在高机械应力如弯曲下保留其阻挡性能的薄膜的方法。另一目的为提供一种在升高的温度下在潮湿氛围中制备具有高抗降解稳定性的薄膜的方法。
该目的通过制备层压材料的方法来实现,该方法包括至少两次的包含以下的序列:
(a)通过进行3至150个原子层沉积方法的循环来沉积无机层,和
(b)通过进行1至3个分子层沉积方法的循环来沉积包含氮的有机层。
本发明进一步涉及一种层压材料,其包含至少两次的包含以下的层序列:
(a)厚度为0.3至15nm的无机层,和
(b)厚度为0.1至3nm的含氮有机层。
本发明进一步涉及一种包含本发明的层压材料的阻挡膜。
本发明进一步涉及本发明的阻挡膜在包封、包装或钝化中的用途。
本发明进一步涉及包含本发明的阻挡膜的电子器件。
本发明的优选具体实例可见于说明书和权利要求书中。不同实施方案的组合属于本发明的范围。
在本发明的上下文中,层压材料为至少两个不同化学组成的层彼此紧密接触的产品。除非此外指明,否则通常不特定限制各层的大小、组成或各层结合在一起的强度。如原子层沉积领域中通常所用,层为厚度可在单一原子尺寸至宏观厚度的范围内变化的平坦结构。
在本发明的上下文中,无机是指含有至少1wt%,优选至少2wt%,更优选至少5wt%,尤其是至少10wt%的至少一种金属或半金属的材料。在本发明的上下文中,有机是指含有99wt%以上,优选99.5wt%以上,尤其是全部或基本全部含有非金属的材料。非金属甚至更优选为C、H、O、N、S、Se和/或P。
原子层沉积(ALD)为进行一系列自限制表面反应,由此取决于所进行的自限制反应数积累具有精确厚度的保形涂层的技术。典型地,表面反应在前体由气态吸附至基材时发生。当基材的所有可达表面位置均被占据时,不再有其他前体吸附至基材从而使反应自限制。在移除过量前体之后,沉积层经化学或物理处理,由此允许其他前体后续沉积。在ALD方法中包含该类沉积和处理的序列通常称为循环。ALD方法由George详细描述(化ChemicalReviews,110(2010),111-131)。若在ALD方法中沉积有机分子,则该方法通常称为分子层沉积方法(MLD)。
本发明方法包括通过进行3至150个原子层沉积方法的循环来沉积无机层。该方法优选包含至少4个循环,更优选至少5个循环,尤其是至少6个循环。该方法优选包含不超过50个循环,更优选不超过40个循环,尤其是不超过30个循环,例如不超过20个循环。
ALD方法中形成无机层的循环典型地包括使含金属或半金属化合物或其混合物变为气态并且将其由气态沉积于基材上。在下文中,术语“金属或半金属”缩写为“(半)金属”。使含(半)金属化合物变为气态可通过将其加热至升高的温度来实现。在任何情况下,必须选择低于含(半)金属化合物的分解温度的温度。优选地,加热温度在略高于室温至300℃,更优选30℃至250℃,甚至更优选40℃至200℃,尤其是50℃至150℃的范围内。替换地或额外地,可将惰性气体如氮气或氩气吹扫通过含(半)金属化合物。以该方式与含(半)含化合物的蒸气压对应,将惰性气体用气态的含(半)金属化合物饱和。
含金属化合物中的金属为Li、Be、Na、Mg、Al、K、Ca、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Rb、Sr、Y、Zr、Nb、Mo、Tc、Ru、Rh、Pd、Ag、Cd、In Sn、Cs、Ba、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Hf、Ta、W、Re、Os Ir、Pt、Au、Hg、Tl、Bi。含半金属化合物中的半金属为B、Si、As、Ge、Sb。优选(半)金属为B、Al、Si、Ti、Zn、Y、Zr、La,尤其是Al。
可呈气态并且可与表面反应的任何含(半)金属化合物均是适合的。含(半)金属化合物优选为(半)金属有机化合物。这些化合物包括烷基(半)金属,例如二甲基锌、三甲基铝或二丁基锡;(半)金属烷氧基化物,例如四甲氧基硅或四异丙氧基锆;环戊二烯加合物,如二茂铁或二茂钛;(半)金属碳烯,例如五新戊醇钽(tantalum pentaneopentylat)或氯化双亚咪唑烷基钌;(半)金属卤化物,例如四溴化锗或四氯化钛;一氧化碳配合物,如六羰基铬或四羰基镍。更优选地,含(半)金属化合物为烷基(半)金属,尤其是C1至C4烷基(半)金属。
可使用一种以上含(半)金属化合物。以该方式可产生包含例如混合(半)金属氧化物,例如氧化锡-锌或氧化钡-钛的无机层。
优选地,第二含(半)金属化合物以相对于含(半)金属化合物的总摩尔量为1至30mol%,更优选2至15mol%存在。在该情况下,可获得掺(半)金属无机层,例如掺铝氧化锌、掺锡氧化铟或掺锑氧化锡。作为替换,为获得掺卤素无机层,可使用含卤素和(半)金属的化合物或除含(半)金属化合物以外的含卤素的化合物,量优选相对于含(半)金属化合物和含卤素的化合物的总摩尔量为1至30mol%,更优选2至15mol%。该类含卤素化合物的实例为氯气、氟化铵或四氯化锡。
ALD方法中形成无机层的循环典型地进一步包括在其沉积于基材上之后使含(半)金属化合物分解。分解可以各种方式实现。固体基材的温度可增加超过含(半)金属化合物的分解温度。此外,可将沉积的含(半)金属化合物暴露于氧气、臭氧、等离子体(如氧等离子体)、氨、氧化剂(如氧化亚氮或过氧化氢)、还原剂(如氢气、醇、肼或羟胺)或溶剂(如水)。优选使用氧化剂、等离子体或水以获得一个(半)金属氧化物层。优选暴露于水、氧等离子体或臭氧。尤其优选暴露于水。若需要单质(半)金属的层,则优选使用还原剂。对于(半)金属氮化物的层,优选使用氨或肼。
ALD方法中形成有机层的循环典型地包括使含氮化合物变为气态并且将其由气态沉积于基材上。含氮化合物中的氮优选呈氧化态-3,即含氮化合物优选为胺。胺包括伯、仲或叔胺,优选伯或仲胺,尤其是伯胺。优选地,含氮化合物进一步包含第二官能团,更优选含有酸性氢的官能团,例如仲胺、羟基或硫醇基,优选羟基。
含氮化合物可以为脂族或芳族的,优选芳族的。更优选地,含氮化合物为芳族胺,由此该胺可共轭至芳族基团或经由连接基如亚甲基连接至芳族基团。芳族基团包括芳族烃,例如苯、萘、联苯;或杂芳族基团,例如吡啶、噻吩、吡咯、呋喃。优选芳族烃,尤其是苯。
含氮化合物的一些特别优选的实例如下:
尤其优选4-氨基苯酚(C-1)和4-氨基苯甲醇(C-2)。还可使有机层具有不同有机分子,条件为至少一个有机分子含氮。
优选地,含氮化合物含有至少两个氨基,更优选两个氨基。甚至更优选地,含氮化合物含有两个氨基和一个羟基。优选地,两个氨基直接或经由连接基如亚甲基连接至芳族体系,例如苯。下文给出含有两个氮原子的含氮化合物的一些优选实例。
根据本发明,有机层通过1至3个包含含氮化合物的ALD循环,优选1或2个ALD循环,尤其是1个ALD循环制得。若进行大于一个包含含氮化合物的ALD循环,则通常在制备有机层的ALD循环中必需包括连接基化合物的沉积。实例包括光气、亚硫酰氯、二酸二氯化物(例如草酰氯)或二异氰酸酯(例如亚乙基二异氰酸酯)。无机化合物也可形成连接基,例如烷基(半)金属,例如三甲基铝。在这种情况下,有机层还包括(半)金属。
ALD方法的温度在-20℃至500℃,优选0℃至300℃,尤其是50℃至200℃的范围内。典型地,在一个ALD循环中使表面暴露于含(半)金属化合物或含氮化合物1ms至30s,优选10ms至5s,尤其是50ms至1s。优选在使表面暴露于含(半)金属化合物或不同化学结构的含氮化合物之间用惰性气体吹扫基材,通常0.1s至10min,优选1s至3min,尤其是10s至1min。
ALD方法可在宽压力范围如5000至10-5毫巴下进行。当含(半)金属化合物或含氮化合物与惰性气体混合时,压力优选大约为标准压力,例如1500至500毫巴,更优选1200至800毫巴。当含(半)金属化合物或含氮化合物不与惰性气体混合时,压力取决于含(半)金属化合物或含氮化合物的蒸气压。此时压力通常为100至10-3毫巴,更优选10至0.1毫巴。在该情况下,优选在压力可调节的设备中,例如在真空室中进行该方法。
本发明方法优选由使呈气态的含(半)金属化合物和含氮化合物通过相对于基材移动的独立孔口来进行。这意指移动基材且保持孔口不动、或保持基材不动而移动孔口、或移动基材与孔口。移动速度优选为0.01至10m/s,更优选为0.02至1m/s,尤其为0.05至0.3m/s。孔口经配置以使得含(半)金属化合物和含氮化合物按如以上方法所述的次序冲击基材表面。含(半)金属化合物的分解优选由将分解材料如水通至基材表面的孔口实现。为避免以气相形式反应,优选放置将惰性气体如氮气或氩气通至基材表面的孔口。
当通过使含(半)金属化合物和含氮化合物通过独立孔口进行该方法时,基材的压力优选为100至5000毫巴,更优选500至1500毫巴,尤其是800至1200毫巴,例如大气压力。作为替换,然而,若可将设备抽空,则可使用如上文所述的较低压力。
孔口优选安置于周围放置,优选移动放置基材的转鼓上。该类设备描述于WO2011/099 858 A1中。在基材为挠性的情况下,有机-无机基材因此可以所谓棍对棍(roll-to-roll)式方法沉积于大基材上。
在本发明方法中,进行包含(a)和(b)的序列至少两次,优选至少三次,更优选至少五次,甚至更优选至少10次,尤其是至少30次,例如至少50次或至少100次。通常,进行该序列不超过1000次。有机和无机层可通过相同数目的ALD循环或通过不同数目的ALD循环彼此独立地制得。例如,一个无机层可通过4个ALD循环制得,而不同无机层可通过8个ALD循环制得。优选地,所有无机层以相同数目的ALD循环制得。更优选地,所有无机层由相同数目的ALD循环制得且所有有机层通过一个ALD循环制得。
此外,不同化合物可用于制备不同无机层或不同有机层。优选地,所有有机层由相同有机化合物制备。优选地,所有无机层由相同含(半)金属化合物制备。
本发明方法产生对于小分子如水和氧具有低渗透性且具有高柔性的层压材料。因此,本发明还涉及该类层压材料。小分子渗透性的良好度量为水蒸气穿透率(WVTR)。优选通过将大量钙斑点蒸发于层压材料上且将另一层压材料沉积于钙斑点的顶部来测量。然后使这些样品暴露于温热潮湿,例如30℃至100℃下30%至90%相对湿度下,优选60℃至85℃下70%至90%相对湿度下,例如60℃和90%相对湿度或85℃和85%相对湿度下的空气。该暴露通常进行至少100小时,优选至少200小时,尤其是至少300小时。通常,暴露不进行超过1000小时。使用变透明的钙斑点数计算WVTR,如Paetzold等所述(Review of ScientificInstruments,74(2003)5147-5150)。通常来说,若WVTR小于10-2g/m2d,优选10-4g/m2d,更优选10-5g/m2d,尤其是10-6g/m2d,则层压材料视为对小分子具有低渗透性。
测量层压材料挠性的合适方法为在半径为0.1至10cm,优选0.1至2cm的圆柱形制品周围弯曲如上文所述含有钙斑点和顶部的第二层压材料的层压材料数次,例如100次,且此后如上文所述测量WVTR率。若WVTR与弯曲前的相应层压材料性比高不超过1000倍,优选高不超过100倍,尤其是高不超过10倍,则层压材料视为具有高柔性。
根据本发明,无机层的厚度为0.3至15nm。无机层的厚度优选为至少0.4nm,更优选至少0.5nm,尤其是至少0.6nm。无机层的厚度优选不超过9nm,更优选不超过5nm,尤其是不超过4nm,例如不超过3nm或不超过2nm。含氮有机层的厚度优选为0.1至3nm,更优选0.2至2nm,尤其是0.3至1.5nm,例如0.4至1nm。层的厚度典型通过X射线衍射,例如宽角X射线衍射(WAXD),优选用如X射线来源的同步加速器测量。
无机层可选自宽范围化合物。这些包括无机氧化物、无机氮化物、无机碳化物、钙钛矿、石榴石、烧绿石、透明导体和II-VI化合物。优选无机氧化物。
无机氧化物的实例包括碱土金属氧化物,例如BeO、MgO、CaO、SrO、BaO;主族金属氧化物,例如Al2O3、SiO2、Ga2O3、GeO2、In2O3、SnO2、Tl2O、PbO、PbO2、Bi2O3;过渡金属氧化物,例如Sc2O3、TiO2、V2O5、CrO2、MnO、Mn2O3、FeO、Fe3O4、Fe2O3、CoO、Co2O3、NiO、Ni2O3、Cu2O、CuO、ZnO、Y2O3、ZrO2、Nb2O5、MoO、MoO2、Tc、RuO2、Rh2O、PdO、Ag2O、CdO、HfO2、Ta2O5、WO3、ReO3、OsO4、IrO2、PtO2、AuO、Hg2O;镧系元素氧化物,例如La2O3、Ce2O3、CeO2、Pr2O3、Nd2O3、Pm2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3。优选B2O3、Al2O3、SiO2、La2O3、Y2O3、ZnO、ZrO2,尤其是Al2O3。通常,在一定程度上,本发明的薄层中的氧化物为水合的。然而,在本发明的上下文中,这些水合物视为由上式表示的氧化物。作为替换,例如氧化物Al2O3可由更普遍的式AlOx(OH)y表示,其中0≤x≤1.5;0≤y≤3且2x+y=3,优选1≤x≤1.5;0≤y≤1且2x+y=3。
无机氮化物的实例包括BN、AlN、Si3N4、Ti3N4、TaN、NbN、WN、MoN、GaN、Zr3N4、InN和Hf3N4,优选BN、AlN、Si3N4、Ti3N4、Zr3N4。无机碳化物的实例包括B4C3、SiC、ZrC。钙钛矿的实例包括BaTiO3、SrTiO3、LaNiO3和LaCoO3。石榴石的实例包括Fe3Al2(SiO4)3、Mg3Al2(SiO4)3和Mn3Al2(SiO4)3。烧绿石的实例包括La2Zr2O7、Gd1.9Ca0.1Ti2O6.9、Dy2Ti2O7和Y2Mo2O7。透明导体的实例包括掺Sn的In2O3、掺Sb的SnO2、掺F的SnO2、掺Al的ZnO。II-VI化合物的实例为ZnS、ZnSe、ZnTe、CaS、SrS、BaS、CdS、CdTe、CdSe。此外,可为混合的氧化物和/或氮化物,例如AlON、SiAlON。
根据本发明,层压材料包含至少两次的包含无机层和含氮层的层序列,层压材料优选包含序列至少三次,更优选至少五次,甚至更优选至少十次,尤其是至少30次,例如至少50次或至少100次。通常,层压材料包含序列不超过1000次。
有机层优选含有呈氧化态-3的氮。本发明的层压材料中的氮的氧化态可通过层压材料的红外(IR)光谱中的特征带确定。
本发明的层压材料尤其适用于制备阻挡膜。因此,本发明进一步涉及一种包含本发明的层压材料的阻挡膜。
本发明的阻挡膜典型地进一步包含基材。基材可为任何固体材料。这些包括例如金属、半金属、氧化物、氮化物和聚合物。基材还可为不同材料的混合物。金属的实例为铝、钢、锌和铜。半金属的实例为硅、锗和砷化镓。氧化物的实例为二氧化硅、二氧化钛和氧化锌。氮化物的实例为氮化硅、氮化铝、氮化钛和氮化镓。优选聚合物。聚合物包括聚酯,例如聚对苯二甲酸乙二醇酯(PET)或聚萘二甲酸乙二醇酯(PEN);聚酰亚胺;聚丙烯酸酯,例如聚甲基丙烯酸甲酯(PMMA);聚丙烯酰胺;聚碳酸酯,例如聚(双酚A碳酸酯);聚乙烯醇和其衍生物,如聚乙酸乙烯酯或聚乙烯醇缩丁醛;聚氯乙烯;聚烯烃,例如聚乙烯(PE)或聚丙烯(PP);聚环烯烃,例如聚降冰片烯;聚醚砜;聚酰胺,如聚己内酰胺或聚(六亚甲基己二酰胺);纤维素衍生物,例如羟乙基纤维素、羟丙基纤维素、甲基纤维素、甲基羟丙基纤维素或硝化纤维;聚氨酯;环氧树脂;三聚氰胺甲醛树脂;酚甲醛树脂。聚合物包括共聚物,例如聚(乙烯-共-降冰片烯)或聚(乙烯-共-乙酸乙烯酯)。优选聚酯和聚环烯烃。
基材可具有任何大小和形状。基材优选为薄膜。基材膜的厚度取决于应用。若阻挡膜围绕超过10mm的半径弯曲,则基材膜的厚度优选为100至1000μm,更优选100至500μm,例如100至200μm。若阻挡膜以小于10mm的半径弯曲,则基材膜的厚度优选为1至100μm,更优选10至70μm,例如40至60μm。
基材表面优选具有高平坦度。在本发明的上下文中,高平坦度意指表面上的最高点高于表面上的最低点不超过100nm,优选不超过50nm。平坦度可用原子力显微法,优选在敲击模式中测量。
通常例如由于小刮痕,或颗粒例如粘附于其表面的粉尘而不可获得具有高平坦度的基材。因此,阻挡膜优选进一步包含平坦化层以避免损害,例如刺穿层压材料。平坦化层更优选处于基材与层压材料之间。在该情况下,平坦化层可额外用于使基材和层压材料更好地保持在一起,尤其是在弯曲或加热时。平坦化层可包含有机聚合物,例如丙烯酸酯或环氧化物;陶瓷,例如碳化物,例如SiC;或有机-无机混合材料,例如聚烷基硅氧烷。优选有机聚合物。
通常平坦化层通过在施加层压材料之前将构成平坦化层的材料沉积于基材上而制得。在有机聚合物的情况下,将包含单体的液体浇铸于基材上,然后例如通过加热或UV引发固化。优选UV引发,包含单体的液体更优选进一步包含固化助剂,例如官能化二苯甲酮。包含单体的液体优选包含单和双官能单体的混合物以使得在固化之后获得交联有机聚合物。包含陶瓷的平坦化层通常通过将材料溅镀于基材上获得。包含有机-无机混合材料的平坦化层可通过将包含有机-无机前体的溶液浇铸于基材上、蒸发溶剂和例如通过加热使有机-无机前体凝结而获得。该方法通常称为溶胶凝胶法。有机-无机前体的实例为烷基三烷氧基硅烷。前体优选由UV可固化侧基,例如丙烯酸酯基官能化。以该方式,可使有机-无机混合材料交联。
构成平坦化层的材料的弹性模数优选处于基材材料与层压材料之间,例如为10至30GPa。确定弹性模数的方法描述于ISO 527-1(Plastics-Determination of tensileproperties,2012)中。
本发明的阻挡膜优选进一步包含保护层以避免层压材料的例如通过刮擦产生的机械损害。保护层可例如包含环氧树脂。保护层可进一步为例如使层压材料连接至电子器件的粘合剂。令人惊奇地发现,就WVTR而言,本发明的阻挡膜与保护层的组合显示出协同效应,即WVTR低于当阻挡膜与保护层组合时所期望的WVTR。
本发明的阻挡膜优选进一步包含吸气剂材料。该吸气剂材料结合小分子如水或氧气,且因此甚至进一步降低阻挡膜的渗透性。吸气剂材料的实例为高度反应性金属,例如Ca;或强吸水性氧化物,例如CaO或SiO2。
本发明进一步涉及本发明的阻挡膜在包封、包装或钝化中的用途。可用本发明的阻挡膜包封、填或充钝化对小分子如水或氧气具有敏感性的任何制品(例如食品、药物、反应性化学物质、电池或优选电子器件)。电子器件的实例为场效应晶体管(FET)、太阳电池、发光二极管、传感器或电容器,在电子器件中的活性材料为有机分子的情况下尤其如此。本发明的阻挡膜可此外用作电绝缘体,例如用作晶体管中的电介质。
使用本发明方法,可获得对小分子扩散具有高阻挡作用的层压材料。这些层压材料在弯曲时维持其高扩散阻挡作用。当使用挠性基材时,可获得具有高扩散阻挡作用的挠性阻挡膜。
附图描述
图1-4显示了实施例的断裂样品的扫描电子显微图象。
实施例
实施例1(本发明)
阻挡膜使用PET基材制得。PET基材的尺寸为2.5×2.5cm2,厚度为100μm,且密度为1.4g/cm3。PET基材通过用去离子水、丙酮和乙醇冲洗,随后用100W的等离子体电源进行30min O2等离子体处理来清洗。此后,PET基材在真空室内脱气30min,直至压力达到5·10-5毫巴。将包括PET基材的真空室加热至80℃。通过打开含有呈液体形式的TMA的侧室的阀2s将气态三甲基铝(TMA)引入真空室中,然后再将真空室抽空以达到5·10-5毫巴并保持15s。
此后,将呈气态的水引入真空室中2s,此后再将真空室抽空38s。进行该序列8次。然后,如上所述将TMA引入真空室中并保持2s,将真空室抽空15s,此后通过在120℃下打开含有液体4AP的腔室的阀8s将4-氨基苯酚(4AP)引入真空室中,此后将真空室抽空200至300s。
上述序列通过[[TMA-H2O]8-TMA-4AP]表示。连续进行该序列250次。在硅晶片上制备相同有机-无机层压材料。使该晶片断裂且经受扫描电子显微法。由此获得的图象描绘于图1中。由图象评估有机-无机层压材料的厚度为300nm。
实施例2(本发明)
阻挡膜如同实施例1中制得,其中连续进行序列[[TMA-H2O]13-TMA-4AP]180次。在硅晶片上制备相同有机-无机层压材料。使该晶片断裂且经受扫描电子显微法。由此获得的图象描绘于图2中。由图象评估有机-无机层压材料的厚度为295nm。
实施例3(本发明)
阻挡膜如同实施例1中制得,其中连续进行序列[[TMA-H2O]25-TMA-4AP]100次。在硅晶片上制备相同有机-无机层压材料。使该晶片断裂且经受扫描电子显微法。由此获得的图象描绘于图3中。由图象评估有机-无机层压材料的厚度为310nm。
实施例4(对比)
阻挡膜通过在实施例1中所述的条件下使PET基材交替暴露于TMA和H2O 500次制得。
实施例5(对比)
阻挡膜通过在实施例1中所述的条件下使PET基材交替暴露于TMA和H2O 250次制得。
实施例6(本发明)
阻挡膜如同实施例1中制得,其中使用保持在120℃下的4-氨基苯甲醇(4ABA)替代4AP。
实施例7(本发明)
阻挡膜如同实施例2中制得,其中使用保持在120℃下的4ABA替代4AP。
实施例8(本发明)
阻挡膜如同实施例3中制得,其中使用保持在120℃下的4-氨基苯甲醇(4ABA)替代4AP。在硅晶片上制备相同有机-无机层压材料。使该晶片断裂且经受扫描电子显微法。由此获得的图象描绘于图4中。由图象评估有机-无机层压材料的厚度为307nm。
阻挡膜的测试
通过在1.3·10-7毫巴下在各薄膜上蒸发厚度为350nm且尺寸为10×10μm2的144个Ca斑点测试PET基材上所制备的阻挡膜的水蒸气穿透率(WVTR)。在Ca斑点的顶部,如相应实施例中所述制得另一层压材料。然后将薄膜放于70℃下相对湿度为70%的干燥箱内480h。通过在如上文所述的该存储程序之后变成透明的Ca斑点的数目计算WVTR。
阻挡膜以0.5的弯曲半径弯曲100次。此后,如上文所述计算WVTR,其中不同之处在于将样品储存360h。结果概述于下表中。
Claims (15)
1.一种制备层压材料的方法,包括至少两次包含以下的序列:
(a)通过进行3至150个原子层沉积方法的循环来沉积无机层,和
(b)通过进行1至3个分子层沉积方法的循环来沉积包含氮的有机层。
2.根据权利要求1的方法,其中在该分子层沉积方法中使用伯胺来沉积该有机层。
3.根据权利要求1或2的方法,其中在该分子层沉积方法中使用芳族胺来沉积该有机层。
4.根据权利要求1-3中任一项的方法,其中在该分子层沉积方法中使用含有羟基的芳族胺来沉积该有机层。
5.根据权利要求1-4中任一项的方法,其中在该原子层沉积方法中使用含Al化合物来沉积该无机层。
6.根据权利要求1-5中任一项的方法,其中包含(a)和(b)的序列进行至少30次。
7.一种层压材料,包含至少两次的包含以下的层序列:
(a)厚度为0.3至15nm的无机层,和
(b)厚度为0.1至3nm的含氮有机层。
8.根据权利要求7的层压材料,其中该有机层含有呈氧化态-3的氮。
9.根据权利要求7或8的层压材料,其中该无机层包含AlOx(OH)y,其中0≤x≤1.5;0≤y≤3并且2x+y=3。
10.根据权利要求7-9中任一项的层压材料,其中该层压材料包含该包含至少30次的(a)和(b)的层序列。
11.一种阻挡膜,包含根据权利要求7-10中任一项的层压材料。
12.根据权利要求11的阻挡膜,其中该阻挡膜进一步包含聚合基材。
13.根据权利要求11或12的阻挡膜,其中该阻挡膜进一步包含平坦化层。
14.根据权利要求11-13中任一项的阻挡膜在包封、包装或钝化中的用途。
15.一种电子器件,包含根据权利要求11-13中任一项的阻挡膜。
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