CN105073666B - 用于具有有机发光二极管的器件的衬底 - Google Patents
用于具有有机发光二极管的器件的衬底 Download PDFInfo
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- CN105073666B CN105073666B CN201480010391.3A CN201480010391A CN105073666B CN 105073666 B CN105073666 B CN 105073666B CN 201480010391 A CN201480010391 A CN 201480010391A CN 105073666 B CN105073666 B CN 105073666B
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- 239000000758 substrate Substances 0.000 title claims abstract description 28
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
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- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 16
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- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
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- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 24
- 230000009477 glass transition Effects 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
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- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
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- 230000005525 hole transport Effects 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000004866 oxadiazoles Chemical class 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000007764 slot die coating Methods 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
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- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- 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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
- C03C17/04—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass by fritting glass powder
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- 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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- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
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- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
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- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
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- C03C4/00—Compositions for glass with special properties
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- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
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- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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- C03C2217/00—Coatings on glass
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- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
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- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
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- H10K2102/101—Transparent electrodes, e.g. using graphene comprising transparent conductive oxides [TCO]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明涉及用于具有有机发光二极管的器件的漫射衬底,包括在其表面之一上涂有包含玻璃质材料的层的玻璃片,使得所述玻璃质材料具有包括以下组分的化学组成,其在下文中规定的重量界限中可变:Bi2O3 60‑85%;B2O3 5‑12%;SiO2 6‑20%;MgO+ZnO 0‑9.5%;Al2O3 0‑7%;Li2O+Na2O+K2O 0‑5%;CaO 0‑5%;BaO 0‑20%。
Description
本发明涉及用于具有有机发光二极管的器件的衬底的领域。其更具体涉及特别适于形成层的玻璃质材料与玻璃料的化学组成。
具有有机发光二极管(在下文中称为OLED,这是本领域中通常使用的)的器件是凭借电致发光现象发光的器件。这些OLED器件通常包含在两个电极之间的有机发光体系。电极之一沉积在导电层形式的玻璃片上。该OLED器件可以用作可视化屏幕或用作照明装置。
在作为照明装置(灯等等)的一种应用中,由该器件提取的光是多色白光。但是,光提取效率天然较低,为大约0.25,光由于其不同元件之间不同的折射率而被截留在该器件内部。
为了解决这一问题,已知的做法,例如来自申请WO 2011/089343,是在玻璃片(当其由钠钙硅玻璃制成时具有1.5的折射率)和电极之间具有包含具有高折射率(通常为1.7至2.0)的玻璃质材料和散射元件例如粒子的内部散射层。上述申请描述了其化学组成包含40重量%至60重量%的Bi2O3和5重量%至30重量%的ZnO的玻璃质材料。
该玻璃质材料通常通过其中混合玻璃料(具有与该材料相同的化学组成)与通常有机的介质以形成糊料并将该糊料沉积在玻璃片上并随后烧制其的方法来获得。
该玻璃料的玻璃化转变温度必须足够低以便能够在玻璃片不变形的温度下对其进行烧制。同时,该玻璃料必须不能在烧制过程中结晶(失透),这会具有产生过度的粗糙度和高光吸收的效果。
该玻璃料的线性热膨胀系数还必须适于该玻璃片的线性热膨胀系数,通常必须接近后者,以避免冷却过程中在玻璃质材料中产生能够破坏其的机械应力。
为了避免在该层上沉积灰尘,能够产生短路,通常的做法是在沉积该导电层之前对该层进行彻底清洁。该清洁通常令其通过超声罐,在那里对该层施以相继的碱性洗涤剂(以分离留在该表面上的粒子)和酸性洗涤剂(为了中和该层的表面并防止粒子的任何再沉积)的作用。酸侵蚀能够降解该玻璃质材料,产生对最终应用而言不可接受的表面粗糙度。
本发明的目的在于提供在改善的耐化学性(特别是对酸)、高折射率、合适的热膨胀系数和合适的玻璃化转变温度与低失透能力之间具有良好的兼顾的玻璃质材料(以及玻璃料)的组合物。
为此,本发明的一个主题是用于具有有机发光二极管的器件的散射衬底,包含在其一个面上涂有包含玻璃质材料的层的玻璃片,使得所述玻璃质材料具有包含以下成分的化学组成,其在下文中规定的重量界限中可变:
Bi2O3 60-85%
B2O3 5-12%
SiO2 6-20%
MgO+ZnO 0-9.5%
Al2O3 0-7%,特别是0-5%
Li2O+Na2O+K2O 0-5%
CaO 0-5%
BaO 0-20%。
本发明的一个主题还是包含本发明的散射衬底的具有有机发光二极管的器件,其中导电层放置在包含玻璃质材料的层上。
使用术语“在……上”或“在……下”不必须意在指这些层接触,仅意指其贴近该衬底(“在……下”)或远离该衬底(“在……上”)。但是其中所述层接触的情况并没有被排除。
本发明的一个主题还是一种玻璃料,其化学组成包含以下成分,其在下文中规定的重量界限中可变:
Bi2O3 65-85%
B2O3 5-12%
SiO2 6-20%
MgO+ZnO 0-9.5%
Al2O3 0-5%
Li2O+Na2O+K2O 0-5%
CaO 0-5%
CaO+MgO ≥0.5
BaO 0-20%。
在下文中详细描述的氧化物含量方面的优选特征涉及沉积在该玻璃片上的玻璃质材料的化学组成以及该玻璃料(用于该沉积)的化学组成。在通篇中所示含量为重量含量。
Bi2O3的重量含量有利地为至少62%,特别是63%和甚至64%或65%和/或最高83%,特别是82%,或甚至81%,甚至80%、79%或78%。其优选包含在65%至80%,特别是68%至75%的范围内。过低的Bi2O3含量不能获得所需折射率,而过高的含量导致玻璃不可接受的泛黄。
B2O3的重量含量优选为至少6%,特别是7%或7.5%,和/或最高11%,特别是10%,或甚至9.5%或9%。其优选包含在6%至11%,特别是7%至10%的范围内。高B2O3含量具有提高该材料的玻璃化转变温度和降低其耐化学性的效果,而过低的含量令该玻璃更容易失透。
SiO2的重量含量优选为至少7%,特别是7.5%或甚至8%,和/或最高18%、17%、16%、15%、14%或13%,特别是12%或11%和甚至10%或9%。其优选包含在7%至12%,特别是7.5%至10%的范围内。过高的SiO2含量导致折射率的有害的降低,而过低的含量降低了耐化学性与热稳定性。
ZnO的重量含量优选为最高9.5%,特别是9%或8%,或甚至7%或6%或5%,和甚至小于5%。根据一个实施方案,该ZnO含量为甚至最高1%,特别是0.5%,或0.1%,或甚至0。ZnO的重量含量优选包含在2%至8%,特别是3%至6%的范围内。高ZnO含量导向良好的耐化学性,特别是对酸,并提高了失透的风险。
MgO的重量含量优选为最高3%,特别是2.5%和甚至2%。在某些实施方案中,该含量甚至小于0.5%和甚至0.1%,或甚至0。在另一实施方案中,该MgO含量为至少0.5%,特别是1%,更特别包含在0.5%至3%,特别是1%至2.5%的范围内。添加MgO能够改善该玻璃质材料的耐化学性。
MgO与ZnO的重量含量之和(MgO+ZnO)有利地为至少1%,特别是2%或3%和甚至4%或5%和/或最高9%,特别是8%和甚至7%。其优选包含在2%至9%,特别是3%至8%或2%至5%的范围内。已经显露出MgO和ZnO的过高累积含量导致在制造该玻璃料的过程中失透的风险。
CaO的重量含量优选为最高4%和甚至3%或2%。在某些实施方案中,该含量甚至小于0.5%和甚至0.1%,或甚至0。在另一实施方案中,该CaO含量为至少0.5%,特别是1%,更特别包含在1%至4%,特别是1.5%至3.5%的范围内。
CaO与MgO的重量含量之和优选为至少0.5%,特别是1%或1.5%,或甚至2%或3%。根据一个实施方案,但是其可以小于0.5%和甚至0.1%,或甚至0。CaO与MgO的重量含量之和优选包含在0.5%至4%的范围内。作为对ZnO含量降低的补充,添加CaO和/或of MgO改善了该玻璃质材料对酸的耐受性。
该Al2O3含量优选为至少1%,特别是2%。其优选包含在1%至6%或1%至4%,特别是2%至3%的范围内。添加氧化铝能够改善该材料的耐化学性。
该BaO含量有利地为最高10%,特别是5%和甚至3%或1%或0.5%,或甚至0.1%。其可以甚至为0。
碱金属氧化物(Li2O、Na2O、K2O)的总含量优选为最高3%,特别是2%和甚至1%或0.5%。根据一个优选实施方案,该含量优选包含在0.02%至1%,特别是0.05%至0.2%的范围内。在这种情况下,存在的唯一的碱金属氧化物有利地为Na2O。添加碱金属氧化物,甚至以低含量,具有显著降低该玻璃化转变温度的效果。
对上述各氧化物或氧化物的组,各下限可以与各上限结合,为简明起见,在这里无法回忆所有可能的范围。同样,对给定氧化物的各范围可以与来自其它氧化物的任何其它范围结合。再一次,并未显示所有组合以便不至不必要地拖累本文。在下表1和2中概括了某些优选的组合。
1 | 2 | 3 | 4 | 5 | |
Bi<sub>2</sub>O<sub>3</sub> | 60-85 | 65-80 | 70-78 | 65-80 | 65-80 |
B<sub>2</sub>O<sub>3</sub> | 5-12 | 6-11 | 7-10 | 6-11 | 6-11 |
SiO<sub>2</sub> | 6-20 | 7-12 | 7.5-10 | 7-12 | 7-12 |
MgO+ZnO | 0-9.5 | 2-9 | 3-8 | 2-5 | 2-9 |
Al<sub>2</sub>O<sub>3</sub> | 0-5 | 1-4 | 2-3 | 1-4 | 1-4 |
Li<sub>2</sub>O+Na<sub>2</sub>O+K<sub>2</sub>O | 0-5 | 0-2 | 0.05-0.2 | 0-2 | 0-2 |
CaO | 0-5 | 0-3 | 0-2 | 0-3 | 1-4 |
BaO | 0-20 | 0-5 | 0-1 | 0-5 | 0-5 |
表1。
6 | 7 | 8 | 9 | 10 | |
Bi<sub>2</sub>O<sub>3</sub> | 60-85 | 65-80 | 70-78 | 65-80 | 65-80 |
B<sub>2</sub>O<sub>3</sub> | 5-12 | 6-11 | 7-10 | 6-11 | 6-11 |
SiO<sub>2</sub> | 6-20 | 7-12 | 7.5-10 | 7-12 | 7-12 |
ZnO | 0-9.5 | 2-8 | 3-6 | 2-8 | 0-1 |
MgO | 0-3 | 0.5-3 | 1-2.5 | 0-2 | 1-2.5 |
MgO+ZnO | 0-9.5 | 3-9 | 2-9 | ||
Al<sub>2</sub>O<sub>3</sub> | 0-5 | 1-4 | 2-3 | 1-4 | 1-4 |
Li<sub>2</sub>O+Na<sub>2</sub>O+K<sub>2</sub>O | 0-5 | 0-2 | 0.05-0.2 | 0-2 | 0-2 |
CaO | 0-5 | 0-3 | 0-2 | 1-4 | 0-5 |
BaO | 0-20 | 0-5 | 0-1 | 0-5 | 0-5 |
表2。
表1和2限定了10种衍生自之前定义的范围的组合的特别优选的组成。无须赘述,这些范围各自可以与对于其它氧化物衍生自该表的其它范围组合。
优选地,Bi2O3、B2O3、SiO2、ZnO、MgO、BaO和CaO的重量含量之和为至少95%,特别是96%或97%和甚至98%或99%。优选地,Bi2O3、B2O3、SiO2、ZnO、MgO和CaO的重量含量之和为至少95%,特别是96%或97%和甚至98%或99%。
P2O5、Nb2O5和V2O5的总含量优选为最高1%,特别是0.5%,和甚至为0。该组合物优选不含氧化铅。
该玻璃质材料或该玻璃料的化学组成可以有利地包含氧化物TiO2和/或SnO2,其已经证实在改善对酸的耐受性方面特别有效。该TiO2含量优选为至少0.5%或1%和/或最高5%,特别是2%。该SnO2含量优选为至少0.2%或0.5%和/或最高5%,特别是3%或2%。
根据另一实施方案,TiO2与ZrO2的总含量为最高1%,特别是0.5%和甚至0.1%,或甚至0,对于这些氧化物,有可能对这种类型的玻璃的失透具有有害的效果。
着色元素(Fe2O3、CuO、CoO、Cr2O3、MnO2、Se、Ag、Cu、Au、Nd2O3、Er2O3)的总含量还优选为0(除了不可避免的杂质)。
氧化锑(Sb2O3)可以添加到该组合物中以降低该层的光吸收,特别是使其较少变黄。其含量优选为至少1%,特别是2%和/或最高5%,特别是4%或3%。
构成该玻璃质材料或该玻璃料的玻璃在550纳米波长下的折射率优选包含在1.8至2.2,特别是1.85至2.1,和甚至1.88至2.0,或甚至1.89至1.98的范围内。
构成该玻璃质材料或该玻璃料的玻璃的玻璃化转变温度优选包含在440至500℃,特别是450至480℃的范围内。通过差示扫描量热法(DSC)测量该玻璃化转变温度,升温速率为10℃/分钟。曲线开始(起始温度)在本文中考虑用于测定该Tg。
结晶温度Tx与玻璃化转变温度Tg之间的差值优选为至少100℃以避免在其成型过程中该玻璃质材料的任何失透。通过考虑由差示扫描量热法获得的结晶曲线的开始(起始温度)来测定该结晶温度。
构成该玻璃质材料或该玻璃料的玻璃的在20至300℃之间的线性热膨胀系数优选包含在70至100 × 10-7/℃,特别是75至95 × 10-7/℃,和甚至80至90 × 10-7/℃的范围内。
该玻璃片优选具有包含在1.4至1.6的范围内的在550纳米波长下的折射率。其优选为钠钙硅类型的玻璃,通过浮法获得,所述浮法包括将熔融玻璃倾倒在熔融锡浴上。该玻璃片优选是无色的,并具有根据标准EN 410:1998为至少80%,或甚至90%的透光率因子。该玻璃片的厚度优选包含在0.1至6毫米,特别是0.3至3毫米的范围内。
该玻璃片在其一个面上涂有包含玻璃质材料的层。优选地,该层沉积接触该玻璃片。有利地,该层涂布该玻璃片表面的至少80%,特别是90%和甚至95%。
根据本发明的一个实施方案,该层有利地由该玻璃质材料组成。在这种情况下,为了获得散射衬底,对于该玻璃片优选的是散射光(其特别可以为丝光玻璃,例如借助酸处理提供丝光面精整),或对于散射层优选放置在包含玻璃质材料的层下方,特别是与该玻璃片和由该玻璃质材料组成的层均接触。该散射面因此并不通过该层本身获得。
根据本发明的另一实施方案,包含玻璃质材料的层还包含散射元件。该层甚至有利地由玻璃质材料与散射元件组成。在这种情况下,该层本身是散射的,其将描述为散射层。
优选地,该散射元件选自粒子和空腔。该散射层可以既含有粒子也含有空腔。
该粒子优选选自氧化铝粒子、氧化锆粒子、二氧化硅粒子、二氧化钛粒子、碳酸钙粒子和硫酸钡粒子。该散射层可以包含单一类型的粒子,或几种类型的不同粒子。
该空腔优选在烧制过程中通过除去有机化合物,例如该介质来形成。它们优选是封闭的和不连接的。
该散射元件优选具有允许散射可见光,特别是在200纳米至5微米的可见光的特征尺寸。特征尺寸可以是中值粒径。
该散射层中粒子的重量浓度优选包含在0.2%至10%,特别是0.5%至8%,和甚至0.8%至5%的范围内。
该散射元件可以均匀分布在该玻璃质材料中。或者它们可以通过例如梯度排列不均匀地分布。该散射层还可以由几个基本层组成,这些层通过散射元件的性质、尺寸或不同比例彼此不同。
包含玻璃质材料的层的物理厚度优选包含在0.5至100微米,特别是1至80微米和更特别是2至60微米,或甚至2至30微米的范围内。
其它层可以放置在包含玻璃质材料的层上,特别是与所述层接触。
这可以是例如平面化层,意在回收位于该包含玻璃质材料的层,特别是该散射层的表面处的任何粒子,以便降低后者的粗糙度。该平面化层例如可以由此前定义的玻璃质材料组成,或由另一种玻璃质材料组成。
例如二氧化硅或氮化硅的阻挡层,其厚度特别包含在5至30纳米的范围内,可以沉积在包含玻璃质材料的层或该平面化层上,与所述层接触。
使用形容词“散射的”来描述该衬底,并在适当的情况下来描述该玻璃片或包含玻璃质材料的层优选意在指该雾度为至少40%,特别是50%,和甚至60%或70%,或甚至80%。该雾度,有时称为“模糊”,根据标准ASTM D1003使用雾度计测量。
包含玻璃质材料的层有利地涂有导电层。后者优选与包含玻璃质材料的层直接接触,或者在适当的情况下与该平面化层或阻挡层直接接触。该导电层优选基于透明导电氧化物(TCO),如铟锡氧化物(ITO)。其它导电材料是可能的,例如银或导电聚合物的层。
作为实例,该散射衬底可以由此包含(或由此组成):
- 非散射玻璃片,随后是由玻璃质材料和散射元件组成的散射层,随后(任选)是平面化层,随后(任选)是阻挡层,最后是导电层,提到的各个层与其之前和之后的层均直接接触,
- 非散射玻璃片,随后是散射层,随后是由该玻璃质材料组成的层,随后(任选)是阻挡层,最后是导电层,提到的各个层与其之前和之后的层均直接接触,
- 散射玻璃片,随后是由该玻璃质材料组成的层,随后(任选)是阻挡层,最后是导电层, 提到的各个层与其之前和之后的层均直接接触。
在本发明的具有有机发光二极管的器件中,涂有包含玻璃质材料的层和导电层(充当第一电极)的玻璃片与至少一个有机材料的层形式的有机发光体系结合,该有机材料层本身涂有充当第二电极的导电层。该有机发光体系因此位于衬底与第二电极之间,与第一和第二电极直接接触。
该发光体系优选由几个层组成:空穴注入层(例如掺杂有聚苯乙烯磺酸或铜酞菁的聚乙烯二氧噻吩)、空穴传输层(例如三苯胺衍生物)、发光层(例如喹啉衍生物的金属络合物)、电子传输层(例如噁二唑衍生物、***衍生物、红菲绕啉衍生物等等)、电子注入层(例如锂或铯)等等。
本发明的OLED器件优选用作多色照明光源,特别是白光光源。其优选是底部发光器件,在此意义上光穿过该玻璃片发射。在这种情况下,该第二电极由反射材料组成,例如金属膜,特别是铝、银、镁等等。
优选地,该OLED器件由此依次包含玻璃片、包含玻璃质材料的层、任选阻挡层或平面化层、导电层(通常为ITO)、由几个层组成的发光体系和反射电极。
本发明的玻璃料优选通过熔融起始材料并随后成形玻璃料来获得。该起始材料(氧化物、碳酸盐等等)可以在大约950至1100℃的温度下熔融,并随后将获得的玻璃浇铸,例如在两个辊之间辊压。随后将获得的玻璃粉碎,例如在球磨、喷射磨、珠磨机或盘磨机中。
该玻璃料优选为粒子形式,其d90最高为10微米,特别是5微米,或甚至4微米。该粒径分布可以使用激光粒度分析仪来测定。
包含玻璃质材料的层优选通过以下方法获得,其中:
- 将本发明的玻璃料与有机介质混合以获得糊料,
- 将所述糊料沉积在该玻璃片上,
- 将整个组装件烧制。
该有机介质通常选自醇类、二醇类和萜品醇酯。介质的重量比例优选包含在10%至50%的范围内。
该糊料的沉积可以特别通过丝网印刷、通过辊涂、通过浸涂、通过刮刀涂布、通过喷涂、通过旋涂、通过流涂或通过狭缝模具式涂布来进行。
在丝网印刷的情况下,丝网具有纺织物或金属网,优选使用流涂工具和刮刀,通过选择丝网的网目及其张力、通过选择玻璃片与丝网之间的距离和通过刮刀移动的压力与速度来控制该厚度。根据该介质的性质,通常通过红外或紫外辐射在100至150℃的温度下干燥该沉积物。
该烧制优选在包含在500至600℃,特别是510至580℃的范围内的温度下在炉中进行。
该导电层可以通过用于沉积薄层的各种技术来沉积,例如溅射,特别是磁控管溅射(磁控管法)、化学气相沉积(CVD),特别是等离子体增强化学气相沉积(PECVD、AOOECVD),或液体沉积技术。
下面的实施例以非限制性方式描述本发明。
第一系列实施例
通过熔融起始材料获得各种玻璃料。为此,将足以获得300克玻璃的起始材料在通过焦耳效应加热的400立方厘米坩埚中升温至1000℃下1小时30分钟。
表3、4和5概括了获得的结果。在这些表中描述了以下内容:
- 该玻璃料的化学组成(以氧化物的重量百分比的形式),
- 该玻璃化转变温度,称为“Tg”并以℃为单位表示,
- 结晶温度,称为“Tx”并以℃为单位表示,
- 线性热膨胀系数,称为α并以10-7/K为单位表示,
- 对550纳米的波长的折射率,表示为n,通过椭圆光度法测得,
- 3毫米厚度的光吸收,称为AL,通过分光光度法测得,
- 铋在酸性介质中的浸出,称为L并以毫克/升为单位表示。
类似于Tg,该Tx通过差示扫描量热法测得。
铋浸出通过将涂有所研究的玻璃质材料层的玻璃衬底浸没在酸性溶液中来测得。为此,使用d90为3.4微米和d50为1.7微米的玻璃料通过在钠钙硅玻璃衬底上丝网印刷来沉积10微米厚的层。该酸性溶液是由Franklab公司以名称Neutrax出售的基于乙酸的溶液,在去离子水中稀释至1.3体积%以获得3的pH值。该样品在50℃的温度下浸没在该溶液中一小时,每十分钟取出少量溶液并随后进行分析以由此推测进入溶液的Bi2O3的量。表中所示数字对应于10分钟后侵蚀溶液中Bi2O3的浓度。
实施例1至10(表3和4)是本发明的实施例,而实施例C1至C6是对比例。
1 | 2 | 3 | 4 | 5 | |
Bi<sub>2</sub>O<sub>3</sub> | 73.1 | 74.5 | 73.7 | 72.3 | 72.4 |
ZnO | 5.54 | 5.31 | 5.39 | 9.34 | 7.9 |
SiO<sub>2</sub> | 7.9 | 7.7 | 7.9 | 7.6 | 9.4 |
B<sub>2</sub>O<sub>3</sub> | 7.71 | 7.8 | 7.74 | 6.31 | 6.86 |
Al<sub>2</sub>O<sub>3</sub> | 2.5 | 2.5 | 2.4 | 2.4 | 2.5 |
Na<sub>2</sub>O | 0.1 | 0.11 | 0.11 | 0.1 | 0.08 |
CaO | 3.1 | 0 | 1.7 | 1.9 | 0.04 |
MgO | 0 | 2 | 1 | 0 | 0 |
MgO+ZnO | 5.54 | 7.31 | 6.39 | 9.34 | 7.9 |
MgO+CaO | 3.1 | 2 | 2.7 | 1.9 | 0.04 |
Tg(℃) | 460 | 468 | 464 | 456 | 455 |
T<sub>x</sub> (℃) | 693 | 678 | 668 | ||
α(10<sup>-7</sup>/K) | 88.7 | 82.2 | 84.2 | 84.9 | 77.5 |
n | 1.91 | 1.93 | 1.93 | 1.92 | 1.90 |
AL (%) | 9.4 | 7.3 | 10.3 | 11.1 | 7.4 |
L (mg/l) | 1.6 | 1.5 | 1.56 | 1.62 | 1.72 |
表3。
6 | 7 | 8 | 9 | 10 | |
Bi<sub>2</sub>O<sub>3</sub> | 72 | 74.8 | 75.9 | 77.2 | 77 |
ZnO | 4.87 | 2.68 | 0.08 | 4.51 | 2.51 |
SiO<sub>2</sub> | 11.4 | 9.2 | 8.4 | 7.8 | 7.6 |
B<sub>2</sub>O<sub>3</sub> | 8.37 | 8.36 | 10.4 | 6.18 | 9.46 |
Al<sub>2</sub>O<sub>3</sub> | 2.7 | 2.7 | 2.6 | 2.3 | 2.4 |
Na<sub>2</sub>O | 0.09 | 0.08 | 0.09 | 0.09 | 0.09 |
CaO | 0 | 0 | 0 | 0 | 0 |
MgO | 0 | 2.1 | 2.1 | 1.9 | 1 |
MgO+ZnO | 4.87 | 4.78 | 2.18 | 6.41 | 3.51 |
MgO+CaO | 0 | 2.1 | 2.1 | 1.9 | 1 |
Tg(℃) | 457 | 475 | 478 | 475 | 458 |
T<sub>x</sub> (℃) | 682 | 678 | 683 | 677 | 668 |
α(10<sup>-7</sup>/K) | 76.9 | 77.1 | 86.4 | 77.2 | 82.9 |
AL (%) | 8.3 | 10.5 | 8.5 | 7.3 | 8.1 |
n | 1.89 | 1.91 | 1.89 | 1.96 | 1.92 |
L (mg/l) | 1.48 | 1.52 | 1.42 | 1.76 | 1.7 |
表4。
C1 | C2 | C3 | C4 | C5 | C6 | |
Bi<sub>2</sub>O<sub>3</sub> | 71.9 | 72.7 | 72.5 | 72.2 | 72.3 | 70 |
ZnO | 10.7 | 10.7 | 10.4 | 9.87 | 9.23 | 10 |
SiO<sub>2</sub> | 7.8 | 7.6 | 7.6 | 7.6 | 7.8 | 7 |
B<sub>2</sub>O<sub>3</sub> | 5.62 | 5.7 | 5.8 | 6.58 | 6.29 | 9 |
Al<sub>2</sub>O<sub>3</sub> | 2.5 | 2.4 | 2.4 | 2.5 | 2.6 | 3 |
Na<sub>2</sub>O | 0.1 | 0.09 | 0.11 | 0.1 | 0.1 | 1 |
CaO | 1.4 | 0 | 0.7 | 0 | 1 | 0 |
MgO | 0 | 0.9 | 0.4 | 1.2 | 0.6 | 0 |
MgO+ZnO | 10.7 | 11.6 | 10.8 | 11.07 | 9.83 | 10 |
MgO+CaO | 1.4 | 0.9 | 1.1 | 1.2 | 1.6 | 0 |
AL (%) | 24.5 | 28.6 | 22.4 | 22.9 | 15.8 | - |
L (mg/l) | - | - | - | - | - | 1.9 |
表5。
对比例C1至C5太过容易失透以至于不能成型为玻璃质材料,因为它们极高的光吸收。本发明的实施例均表现出显著优于对比例C6的对酸的耐受性。
第二系列实施例
本发明的其它玻璃通过熔融来获得,如在第一系列实施例中那样。其化学组成小时在下表6中。
可以对批量玻璃样品评估这些玻璃对酸的耐受性。该样品(均具有相同的表面积)浸没在如前所述的相同侵蚀溶液中18小时。样品的质量损失(以mg/cm²为单位表示)在表6中称为“Ma”。在对比玻璃C6的情况下的质量损失为15 mg/cm²。
也通过测量质量损失(称为“Mb”)来评估对碱的耐受性,所述质量损失通过在50℃下将样品浸没在pH 11的溶液(由Borer公司以商标deconex® PV 110出售的浓缩物的稀释至1%的溶液)中18小时来获得。
11 | 12 | 13 | 14 | 15 | |
Bi<sub>2</sub>O<sub>3</sub> | 77.8 | 74.0 | 75.1 | 70.6 | 78.6 |
ZnO | 0 | 0 | 0 | 0 | 0 |
SiO<sub>2</sub> | 10.5 | 11.0 | 10.2 | 10.8 | 10.1 |
B<sub>2</sub>O<sub>3</sub> | 9.5 | 7.4 | 6.8 | 10.4 | 7.7 |
Al<sub>2</sub>O<sub>3</sub> | 2.0 | 5.4 | 5.0 | 3.4 | 2.7 |
Na<sub>2</sub>O | 0 | 0.1 | 0.1 | 0.1 | 0.1 |
CaO | 0 | 0 | 0 | 4.7 | 0 |
TiO<sub>2</sub> | 0 | 2.1 | 0 | 0 | 0 |
SnO<sub>2</sub> | 0 | 0 | 0 | 0 | 0.8 |
Sb<sub>2</sub>O<sub>3</sub> | 0 | 0 | 2.9 | 0 | 0 |
Ma (mg/cm²) | 9 | 3.8 | 8 | 14 | 11.6 |
Mb (mg/cm²) | 4 | 1 | 4 | 8 | 4 |
表6。
Claims (14)
1.用于具有有机发光二极管的器件的散射衬底,包含在其一个面上涂有包含玻璃质材料的层的玻璃片,使得所述玻璃质材料具有包含以下成分的化学组成,其在下文中规定的重量界限中可变:
Bi2O3 65-85%
B2O3 5-10%
SiO2 6-20%
MgO 0.1-3%
MgO+ZnO 1-9.5%
Al2O3 0-7%
Li2O+Na2O+K2O 0.02-5%
CaO 0-5%
BaO 0-20%
其中构成该玻璃质材料的玻璃的玻璃化转变温度包含在450至480℃的范围内。
2.如权利要求1中所要求保护的散射衬底,使得Bi2O3的重量含量包含在65%至80%的范围内。
3.如权利要求1-2之一中所要求保护的散射衬底,使得SiO2的重量含量包含在7%至12%的范围内。
4.如权利要求1-2之一中所要求保护的散射衬底,使得MgO与ZnO的重量含量之和包含在2%至9%的范围内。
5.如权利要求1-2之一中所要求保护的散射衬底,使得CaO与MgO的重量含量之和包含在0.5%至4%的范围内。
6.如权利要求1-2之一中所要求保护的散射衬底,使得所述玻璃质材料的化学组成包含氧化物TiO2和/或SnO2。
7.如权利要求6中所要求保护的散射衬底,使得TiO2含量为至少0.5%,和最高5%。
8.如权利要求6中所要求保护的散射衬底,使得SnO2含量为至少0.2%,和最高5%。
9.如权利要求1-2之一中所要求保护的散射衬底,使得包含玻璃质材料的层还包含选自粒子和空腔的散射元件。
10.如权利要求9中所要求保护的衬底,使得所述粒子选自氧化铝粒子、氧化锆粒子、二氧化硅粒子、二氧化钛粒子、碳酸钙粒子和硫酸钡粒子。
11.如权利要求1至2之一中所要求保护的衬底,使得包含玻璃质材料的层由所述玻璃质材料组成,并使得所述玻璃片散射光,或在包含玻璃质材料的层之下放置散射层。
12.如权利要求1-2之一中所要求保护的散射衬底,使得导电层位于包含玻璃质材料的层之上。
13.具有有机发光二极管的器件,包含如权利要求1-12之一中所要求保护的散射衬底。
14.用于沉积在玻璃片上的玻璃料,该玻璃片被包含在具有有机发光二极管的器件的散射衬底中,该玻璃料的化学组成包含以下成分,其在下文中规定的重量界限中可变:
Bi2O3 65-85%
B2O3 5-9.5%
SiO2 6-20%
MgO 0.1-3%
MgO+ZnO 1-9.5%
Al2O3 0-5%
Li2O+Na2O+K2O 0.02-5%
CaO 0-5%
CaO+MgO ≥0.5%
BaO 0-20%
其中构成该玻璃质材料的玻璃的玻璃化转变温度包含在450至480℃的范围内。
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CN102574727A (zh) * | 2009-10-15 | 2012-07-11 | 旭硝子株式会社 | 有机led元件的散射层用玻璃以及使用该玻璃的有机led元件 |
CN102762510A (zh) * | 2010-01-22 | 2012-10-31 | 法国圣-戈班玻璃公司 | 在电极涂层下用高指数层涂布的玻璃基材、以及包含所述基材的有机发光装置 |
WO2012035565A1 (en) * | 2010-09-16 | 2012-03-22 | Daunia Solar Cell S.R.L. | Sealing agent with low softening temperature useful in the preparation of electronic devices |
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JP6449788B2 (ja) | 2019-01-09 |
CN105073666A (zh) | 2015-11-18 |
MY174696A (en) | 2020-05-08 |
RU2015140758A (ru) | 2017-03-30 |
US20160013432A1 (en) | 2016-01-14 |
RU2683454C2 (ru) | 2019-03-28 |
US10084144B2 (en) | 2018-09-25 |
JP2016508952A (ja) | 2016-03-24 |
EP2958867A1 (fr) | 2015-12-30 |
WO2014128421A1 (fr) | 2014-08-28 |
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