CN101103653A - 应用于制造发光显示设备的材料 - Google Patents
应用于制造发光显示设备的材料 Download PDFInfo
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- CN101103653A CN101103653A CNA038243407A CN03824340A CN101103653A CN 101103653 A CN101103653 A CN 101103653A CN A038243407 A CNA038243407 A CN A038243407A CN 03824340 A CN03824340 A CN 03824340A CN 101103653 A CN101103653 A CN 101103653A
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 239000011521 glass Substances 0.000 claims abstract description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 10
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 10
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical group O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 9
- 238000002834 transmittance Methods 0.000 claims abstract description 8
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 4
- 238000000151 deposition Methods 0.000 claims description 27
- 230000008021 deposition Effects 0.000 claims description 25
- 238000000576 coating method Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 22
- 238000005516 engineering process Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- 229910044991 metal oxide Inorganic materials 0.000 claims description 11
- 150000004706 metal oxides Chemical class 0.000 claims description 11
- 239000011701 zinc Substances 0.000 claims description 11
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 229910052738 indium Inorganic materials 0.000 claims description 7
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 229910007717 ZnSnO Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910017911 MgIn Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002019 doping agent Substances 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910017784 Sb In Inorganic materials 0.000 claims 1
- 238000005234 chemical deposition Methods 0.000 claims 1
- 239000002241 glass-ceramic Substances 0.000 claims 1
- 238000010422 painting Methods 0.000 claims 1
- 239000012808 vapor phase Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 description 137
- 230000002950 deficient Effects 0.000 description 11
- 239000012044 organic layer Substances 0.000 description 10
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000013508 migration Methods 0.000 description 8
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- 230000008901 benefit Effects 0.000 description 7
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- 230000003287 optical effect Effects 0.000 description 5
- 229910020923 Sn-O Inorganic materials 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000010413 mother solution Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
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- 238000011160 research Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 229910000410 antimony oxide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- -1 dichloro oxalic acid tin Chemical compound 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
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- 230000002349 favourable effect Effects 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910007611 Zn—In—O Inorganic materials 0.000 description 1
- 229910007604 Zn—Sn—O Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 210000004276 hyalin Anatomy 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000013047 polymeric layer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 125000004213 tert-butoxy group Chemical group [H]C([H])([H])C(O*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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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
- 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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/54—Screens on or from which an image or pattern is formed, picked-up, converted, or stored; Luminescent coatings on vessels
- H01J1/62—Luminescent screens; Selection of materials for luminescent coatings on vessels
- H01J1/70—Luminescent screens; Selection of materials for luminescent coatings on vessels with protective, conductive, or reflective layers
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- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
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- H05B33/28—Light sources with substantially two-dimensional radiating surfaces characterised by the composition or arrangement of the conductive material used as an electrode of translucent electrodes
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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Abstract
本发明揭示了一种用于制造发光显示设备的材料,它包括玻璃或玻璃状陶瓷底物(1),沉积在底物(1)的一面、基本上包括至少一种单一或混合、掺杂或没有掺杂的透明导电氧化物(TCO)的第一层(2),至少一种单一或混合、掺杂或没有掺杂的透明导电氧化物的第二层(3),两层是这样的:所述的第一层(2)具有大于1nm的粗糙度,所述的第二层(3)具有小于或等于1nm的粗糙度,具有第一和第二层的产品在可见光范围内的透光度为至少80%,所述第二层(3)的工作性能高于所述第一层(2)的工作性能,并且高于4.6eV。优选的是大于4.8eV。第一层(2)有利的是掺入锡的氧化铟层,第二层(3)是掺杂锑的氧化锡层。本发明也描述的发光显示设备(图2),特别是在其阳极掺入这些材料的有机发光二极管。
Description
相关申请
本申请要求以下在先申请的优先权:于2002年9月3日提交的法国专利申请第02-10865号。这些专利申请内容在此引为参考。
技术领域
本发明涉及在制造发光显示设备,更具体的说是有机发光二极管中使用的材料。本发明也涉及掺入该材料的显示设备,特别是掺入该材料的有机发光二极管,和准备所述材料的方法。
技术背景
显示设备,特别是显示屏,最近正经历着许多的发展。有机发光二极管,又称为OLED,此技术能够提供一种更明亮、成本更低和更有效的显示模块,它将无庸置疑地成为下一代发光显示屏的基础。此技术本应被主要应用于平板屏幕的发展,但是目前它还不够稳定,且不被充分了解。从相似意义上说,一个基本的OLED单元是由一个透明的阳极和一个金属层的阴极以及它们之间堆集的薄的有机层所组成。
传统上,此有机层包含有一个空穴注入层,空穴转移层,一个光子发射层和一个电子转移层。在OLED单元上施加合适的电流时,正、负电荷在发射层重新组合,产生了光。选择有机层的结构和所使用的阳极和阴极的类型以使发射中重新组合的过程最大化,这也改善了OLED设备的发光能力。由此,OLED类型的显示设备能在更轻,体积更小的屏幕上更好地显示信息。目前,OLED技术正在飞速发展,但仍受到一些困难的阻碍。
目前,OLED类型二极管的一个主要发展方向是使用了一层搀杂了锡的三氧化二铟(In2O3:Sn)作为阳极的透明导电层,通常缩写为ITO。所属技术领域公知的是,此ITO层作为阳极被直接沉积于底物上。它具有出色的导电性和非常好的透明度,但不幸的是它有下列缺陷,主要是因为使用沉积在具有粗糙表面的玻璃底物上的技术,它导致了相当严重的电流密度非均一性甚至短路,从而降低了OLED设备的功能。
具有ITO层的OLED类型的设备的另一个缺陷是在ITO层中的铟原子在电场的作用下有迁移的倾向。
另外,ITO层的缺陷是其低工作性能。
到目前为止,已开展了许多的研究以解决这些缺陷,同时在不太影响此阳极的导电性的情况下,提高OLED单元的工作性能。
在试图降低此涂布于底物上的透明层的粗糙度方面,欧洲专利EP0010786提出把此底物进行化学处理以减低其粗糙度。
国际专利WO0145182建议改变此ITO层的涂布工艺以降低其表面粗糙度。
另外的一些文献,特别是国际专利WO97/48115和美国专利US6259202,建议用等离子体处理ITO层。
国际专利WO97/48115建议用等离子体处理ITO层以提高其工作性能。
美国专利US6262441描述了用半透明的金属层来提高其工作性能的方法。
国际专利WO01/15244描述了用部分氧化金属的中间层防止在沉积ITO层进程中OLED单元的有机层被氧化。
国际专利WO99/13692描述了为增强工作性能而在阳极和发光层中间夹入一层或多层聚合物的OLED类型的材料。相似的是,美国专利US5998803,US5714838和US6087730也提到了在阳极和发光层之间有一层有机层存在的OLED类型的设备。
所有上述文献中所提出的设备,其目的在于在使用ITO层时减低其至少一个已知的缺陷的影响,特别是降低此涂层的粗糙度和增强其工作性能。
因此,所有上述文献希望通过消除至少一个上文所提到的缺陷以增强OLED设备的功能。
在上述文献所提到的设备中,那些特别被感兴趣的设备包含一个透明的ITO阳极和有机发光层,一个导电的有机层,特别是具有掺杂的聚合物,如聚(亚乙二氧基)噻吩,称为PEDOT的有机层,这样可提高空穴注入层的效率及降低ITO层粗糙所带来的不利影响。
但是,尽管是密闭封装的有机聚合物也具有有限的化学稳定性和较低的导电性(通常是约1到5.10-2Ω.cm相比于ITO的10-4Ω.cm)等缺陷。
发明的内容
本发明的发明者认为,在ITO阳极和发光层之间包含导电层的OLED类型的设备中,用工作性能比ITO更高的透明的导电氧化物层来取代现有技术中的聚合物层,将可能消除以上使用ITO层技术中的所有缺陷。
更准确地说,这一导电的透明氧化物层,特别是通过溶胶-凝胶工艺沉积的氧化物层,能显著的降低表面的粗糙度。而且,通过选择合适的导电透明氧化物,可能得到比一层中间有机层所得到的更好的工作性能。同时,它能避免有机层缺乏化学稳定性,特别是在使用过程中可能的氧化等问题。
另外,通过选择合适的导电透明氧化物,其可能大大地限制了在电场作用下ITO层中铟的迁移。此导电透明氧化物层可作为防止迁移的屏蔽物。
使用此透明导电的氧化物层的另一个好处是,它能形成屏蔽,从而防止使用设备时产生的电场作用使ITO层中的铟迁移。
深入其领域的研究,发明者发现应用相同的沉积构思,在具有第一透明导电的金属氧化物层的粗糙的表面上沉积具有比第一导电氧化物层更好的工作性能的基本上由第二透明导电氧化物组成的一层,所述的沉积可延伸到除ITO以外的透明氧化物,通过在用作OLED类型设备的任何粗糙金属氧化物层的表面上沉积工作性能介于作为阳极的第一层和发光层之间的透明导电金属氧化物可避免由任何粗糙金属氧化物层为阳极的OLED类型设备所带来的缺陷。
其次,通过选择合适的两种金属氧化物,第二层的金属氧化物层可能成为防止由于电场作用造成的来自第一层的原子迁移的屏蔽物。
结合简图1和简图2描述,可以容易地清楚并完全理解本发明的上述和其他方面的优点和特性。
附图简述
图1是代表本发明的材料的示意图。图纸尺寸不按比例。
图2是掺入本发明材料的OLED设备图。
发明详述
本发明第一方面涉及一种新颖的三明治形的材料,它是有一层透明的底物,特别是玻璃或玻璃状陶瓷(vitroceramic)底物,被根据其相应的透明度,粗糙度和工作性能值而被挑选的二层透明导电氧化物层所覆盖。
本发明第二方面涉及发光显示设备,特别是含有此材料的OLED类型的二极管。
本发明第三方面涉及制造该材料的方法。
根据此发明的一个基本特征,此发明涉及一种材料,它具有:
·玻璃或玻璃状陶瓷底物,
·沉积在所述底物一面、具有至少一种单一的或混合的、掺杂的或不掺杂的透明导电氧化物的第一层,该层在下文被称为TCO层的涂层,
·沉积在所述第一TCO层上、具有至少一种单一的或混合的、掺杂的或不掺杂的透明导电氧化物的第二层,该层在下文被称为第二TCO层,
两个TCO层是这样的:
·所述的第一TCO层的粗糙度大于1nm,所述的第二TCO层的粗糙度小于或等于1nm,
·具有第一和第二TCO层的产品在可见光区间的透光度为至少80%,
·所述第二TCO层的工作性能大于第一TCO层的工作性能,且大于4.6eV,优选的是大于4.8eV。
图1是此类材料的示意图。
它是一种三明治式的材料,并具有一个玻璃或玻璃状陶瓷底物1。
此底物被具有高表面粗糙度的透明电导氧化物的第一层2所涂覆。该粗糙度在图1中用在TCO层2和TCO层3之间的折线表示出来。
此第一层透明导电氧化物层通常是用常规的真空喷涂工艺或化学蒸汽沉积工艺沉积在底物上。
对给定的氧化物类型而言,此种沉积类型会带来极好的导电性能,但众所周知,它也会产生较大的粗糙度。
在第一涂层2上沉积的第二层导电层3能使所得的表面平坦,可选择不显著降低导电率和透明度的材料。
如下的技术方案并非用作任何方式的限定,第二导电氧化物层有利地用溶胶-凝胶型工艺进行沉积,以达到其粗糙度小于或等于1nm。
另外,考虑到本发明中材料的主要应用,分别选择此二层TCO层的工作性能,使第二层的工作性能高于第一层的工作性能,并且第二层的工作性能大于4.6eV,优选的是大于4.8eV。
此二层TCO层各自基本上由至少一种为单一或混合的氧化物形式的氧化物或至少一种选自锡,锌,铟和镉的金属氧化物的混合物组成,如果有必要,其还可能与选自镓,锑,氟,铝,镁和锌的至少一种元素组合,所述的金属元素进入所述混合的氧化物所述氧化物的混合物的组合物中,或作为所述氧化物的掺杂剂。
这些氧化物可以是单一或混合的氧化物或是多种氧化物的混合物。
混合的氧化物的例子包括:
·Ga-In-O
·Ga-In-Sn-O
·Zn-In-O
·Zn-In-Sn-O
·Sb-Sn-O
·Zn-Sn-O
·Mg-In-O
·Cd-In-O
·Cd-Sn-O
·Cd-Sn-In-O
它们都是选自锌,铟和锡的至少一种金属的氧化物。
掺杂的氧化物的例子包括掺有氟的氧化锡(SnO2:F)或掺有锑的氧化锡(SnO2:Sb)或是掺有锡的氧化铟(In2O3:Sn),又被称作为ITO。
根据本发明特别有利的变体,第一TCO层包括如下的必要组成:
·掺有锡的氧化铟(In2O3:Sn),又被称为ITO
·掺有氟的氧化锡(SnO2:F),又被称为FTO
·掺有铝的氧化锌(ZnO:Al),又被称为AZO
·掺有锑的氧化锡(SnO2:Sb),又被称为ATO
如上所述,最常见的OLED类型设备中的阳极由ITO组成,它具有优良的导电性能,但由于表面粗糙度的问题,在使用显示设备过程中由粗糙度引起的短路降低二极管的性能,从而使之成为一个缺陷。
尽管有这些缺陷,但由于使用第二层TCO使第一层TCO变平这一优势,因此,ITO仍将是制造本发明的第一TCO层优选的透明导电氧化物。
因此,根据本发明特定的有利变体,该材料包括具有ITO的第一TCO层,和工作性能高于4.6eV或优选地高于4.8eV的第二TCO层。
在此情况下,选择组成第二层TCO层的氧化物应优先选择从以下的氧化物组:
· SnO2
· SnO2:F
· SnO2:Sb
· In4Sn3O12
· Zn2In2O5
· ZnSnO3
· Zn2SnO4
· GaInO3
· MgIn2O4
此第二TCO层有可能和第一层互补,从而使第二层的表面粗糙度小于1nm。
另外,所选的第二TCO层可限制在ITO层中铟原子在电场作用下的迁移,从而对此迁移构成了真正的化学屏蔽。
通过在第一ITO层上覆盖选自上述的第二透明导电氧化物层可达到前述的全部或至少部分的益处。
在此需要注意是,当第一层是ITO层时,上述不同的材料用作第二层TCO层,尽管具有较ITO层高的电阻率(通常在10-4Ω.cm和3.10-4Ω.cm),但就导电率来说,它们还是可接受的。
下表给出了在ITO材料为第一层的情况下可以作用第二TCO层的透明导电氧化物的例子及其工作性能和电阻率值。
TCO | 工作性能(eV) | 电阻率(10-4Ω.cm) |
SnO2 | 4.84 | 3-8 |
SnO2:F | 4.9 | 2-5 |
SnO2:Sb | 5 | 20 |
In4Sn3O12 | 4.9 | 2 |
Zn2In2O5 | 4.95 | 3-4 |
ZnSnO3 | 5.3 | 40 |
Zn2SnO4 | 53 | 40 |
GaInO3 | 5.4 | 27 |
对于各种性能要求来说,特别适合的材料是掺有锑的氧化锡(SnO2:Sb),称之为ATO。
选择两个连续的氧化层,第一ITO层和第二ATO层可以完美地替代二极管中的有机-聚合物空穴注入层。
ATO层的特性被特别感兴趣,原因是它的工作性能超过4.8eV,于有机发光层的工作性能(通常是5.2eV)非常相似,并且它形成了对铟迁移的良好化学屏障。
另外,通过溶胶-凝胶方式从母体溶液中在ITO层上沉积ATO层将大大地降低ITO层的表面粗糙度。
此外,从实施例中可容易地看到,在玻璃或玻璃状陶瓷底物上沉积ITO层和ATO层的材料可被用作为OLED类型设备中有效的阳极以注入空穴。
更精确地说,在玻璃或玻璃状陶瓷底物上沉积ITO层后再涂布ATO层所形成的设备的优点如下:
第二层的ATO层可以使用溶胶-凝胶工艺涂布,从而使表面的粗糙度非常低,
ATO层的工作性能较ITO层的工作性能要高,并与有机发光层的工作性能相似,
ATO层的化学稳定性远远大于ITO层。因此它可以作为一个化学屏蔽以阻止铟向有机层的迁移,
ATO层在化学稳定性上远远大于传统的空穴注入层,例如PEDOT或其他的聚合物,
当使用了二个连续的透明导电金属氧化物层后,有机注入层就不必再使用了,
此底物和ATO/ITO可直接在准备生产OLED类型的设备中使用。
本发明中三明治式材料各层的厚度取决于材料的应用。
尽管如此,一般来说,透明玻璃或玻璃状陶瓷底物有利的厚度为0.1到3mm之间的厚度。
这样选择厚度,可使OLED类型的材料的厚度小于1mm。
对第一TCO层的厚度没有特别的限制,通常在100-150nm。此厚度相当于目前用作透明阳极的OLED类型设备中ITO层的厚度。
第二TCO层的厚度最好在30-200nm,优选的是在50-150nm。
如前所描述的,上述材料最适合使用作为发光显示设备的阳极部分。
我们可以引用数量众多的不论其体积大小的发光显示屏幕来作为此发光显示设备的例证,特别是移动电话,电视和电脑屏幕。
发光显示设备更具体的说包含有有机发光二极管(OLED),而二极管是由本发明的材料组成阳极部分,并在之上覆盖了电子发光层和一个阴极。
图2是包含有此发明材料作为阳极部分的OLED设备的示意图。层3上覆盖了有至少一个发光层和金属阴极5的部分4。
构成各种发光层4和阴极5的材料都是目前生产OLED类型设备的过程中使用的那些。
本发明最后一方面也涉及制造本发明材料的方法和含有这些材料的设备。
可以使用现有技术中所有的已知技术,在玻璃底物上沉积二个连续的透明导电氧化物层并能达到所需的粗糙度。
尽管如此,考虑到两个连续的TCO层之间相对的粗糙度,优选的是,在已涂布上粗糙度大于1nm的第一层TCO层上使用底物溶胶-凝胶的沉积将第二TCO层进行沉积。
事实上,如前所述,此溶胶-凝胶类型的沉积工艺使表面粗糙度值特别低,特别是低于1nm。
通常,使用溶胶-凝胶沉积步骤后是对第二TCO进行加热固结的步骤。
沉积具有较高粗糙度值的第一TCO层通常使用真空喷涂工艺或是化学蒸汽沉积。
所选择的操作条件取决于所需沉积的氧化物的类型和需要的厚度。当考虑使用溶胶-凝胶方式沉积时,其条件取决于商业供应的TCO母体。在此以供氧化锡沉积的母体为例,可以选择SnCl2(OAc)2,SnCl2,一种Sn(II)的醇盐如Sn(OEt)2,Sn(II)乙基-2-正己酸酯,SnCl4,Sn(IV)的酚盐如Sn(OtBu)4。任何已知的锡的盐类或有机金属化合物母体都可以使用。在使用氧化锑沉积时,所有通常所使用的用来沉积氧化锑的母体均可使用。这些母体包括金属有机化合物和它们的盐,特别是Sb(III)的醇盐和氯化物如SbCl3或SbCl5。
总的来说,对于金属氧化物母体,可使用任何常规使用的化合物。特别是可以使用这些金属的有机金属化合物或这些金属的盐类。更准确地说,金属氧化物母体以在有机溶剂,如挥发醇中的溶液或悬浮液的形式使用。挥发性醇的例子包括C1到C10的直链或支链醇类,特别是甲醇,乙醇,己醇和异丙醇。也可使用二元醇,特别是乙二醇,或使用挥发性酯如乙酸乙酯。
用于沉积氧化物层的组合物有利地包括其他的成分,特别是水或稳定剂,如双丙酮醇,乙酰丙酮、乙酸和甲酰胺。
通过现有技术中已知的用来从液体组合物中制造涂层的任何方法来沉积该薄层。通过把要涂布的底物浸入母体溶液或是用离心的方法把溶液施加到底物上,或是使用把溶液喷洒到底物表面上的方法得到该薄层。
通常,沉积层再经过热处理,通常在22到150摄氏度之间,有利的是先在60摄氏度左右,其后再在450到600摄氏度范围内进行2分钟到1小时的热处理,最好是在550摄氏度左右进行15分钟。
如上所述,溶胶-凝胶工艺能有利地用于沉积第二TCO层,由此可以得到较好的平整度,最终得到了所需的低粗糙度。使用基于溶胶-凝胶方式沉积TCO层的技术的另一个优点是可以用软平版印刷方式在此层固结之前印上有规则的结构,特别上由OLED类型二极管的发射层发射出的波长范围内的周期性的微结构。此方法大大地降低了在二极管周边的光损失。
用溶胶-凝胶工艺沉积TOC层的另外一个优点是它有可能降低现有OLED某一缺陷,这在与本发明同一天申请的另一发明中有阐述。即,现有OLED低的光发射效率是因为由光发射层发出的光线被禁固在二极管的结构内,在我们熟知的波长导向效应作用下,光线仅仅从二极管的边缘发射到二极管外,但从此方位发出的光线对显示应用是没有帮助的。事实上,光线只有通过透明导电氧化物(TCO)层到达发射平面才能被有效地质点化并形成图像在OLED上显示出来。
当使用溶胶-凝胶工艺沉积时,特别是在沉积第二TCO层时,对本发明的发明者来说,尽管从理论角度上普通的溶胶-凝胶溶液涂布条件可以被使用,当涂布薄的底物时,经常会有利地调整这些过程,特别是当底物的厚度小于1mm的情况下。
事实上,当底物相对较薄时,特别是小于1mm的厚度时,在使用溶胶-凝胶涂布后的干燥过程中就后有问题出现。在已覆盖的底物干燥时出现的问题的严重性随着底物厚度的变小而增大。应用不同的溶液来解决这一问题的方法是另一个同一天专利申请的主题。其主要涉及到一个经过改进的用溶胶-凝胶方法涂布的工艺过程,特别是当底物的厚度小于1mm时。
如后续的待批专利所示,它提供了三种解决在相对较薄的底物上用溶胶-凝胶方式涂布层在干燥时由蒸发步骤造成的雾缺陷的方法。
更精确地说,本发明的发明者为解决这些问题所进行的研究,通过下列方法克服这些困难:通过改变溶剂或修饰用作沉积的液体介质,从而降低发热和/或蒸发率,或是通过升高溶胶-凝胶过程中溶液介质的温度,从而使干燥有更好的均一性,或在蒸发液体介质和涂布层结固之前,在覆盖上液体层后立即加热。
以下的实施例中实施的是此类改良的工艺。以下给出的这些实施例仅供阐述用,并非用来限定本发明。
实施例
准备的和使用的各种材料具有如下的特征:
a.膜厚度的测量
使用型号为TENCOR P10的针状表面靠模仿形工具机(needle surfaceprofiler)来测量膜的厚度。以下所给出的厚度值是在7个不同位置测量所得到的数值。
b.表面阻抗
膜的阻抗的测量是在24小时后,使用所谓的四点直线技术,每个黄金接触点的间距为2mm。根据此技术的原理,用测量到的阻抗乘上一个4.53的系数即得到此层的阻抗。
c.粗糙度
使用白色光干涉仪(Zygo New View 500)并通过原子显微镜(又被称为AFM技术)可以来测量峰-谷粗糙度(Rpv)和平均粗糙度(Rrms)。
d.工作性能
使用开尔文探测器(KP-科技有限公司)来测量。
e.光学性质
使用Cary 5E(瓦里安)型分光光度计,在200到3000nm的波长范围内,使用空气作为自然入射的参照物,可以测量样品的透光度。
实施例1:涂覆了ITO层和ATO层的玻璃支持物
1.使用了由三星康宁公司出售的,使用真空喷涂技术在0.7mm的玻璃底物上覆盖ITO层的产品。
此ITO层具有如下的性质:
· 厚度为192nm,
· 表面阻抗为7.6Ω/□,
· 平均粗糙度(Rrms)测量5μm2为4.7nm,
· 峰-谷粗糙度(Rpv)测量5μm2为31.1nm,
· 工作性能在4.3-4.6eV之间,
· 透光度在可视范围内为83%。
2.涂布溶液的准备是把二氯二乙酸锡SnCl2(OAc)2溶解在乙醇中,同时加入4-羟基-4-甲基-戊酮(CAS 123-42-2)作为稳定剂。计算得到锡和锑的相对量为最终掺杂7摩尔%。相对于锡的稳定剂浓度为2摩尔%。加入乙醇使最终锡的浓度为0.5摩尔/升。
这样沉积涂覆溶液:在25℃下将底物浸在该介质中,以24cm/min的速度把底物从溶液中取出。
在沉积了单层的ATO层之后,此被涂布的底物被加热至550摄氏度达15分钟。
此涂层具有如下的性质:
· 表面阻抗:17到20Ω/□,
· 光学透光度:82%,
· 工作性能:4.8到5.2eV,
· 涂层厚度:108nm(若是ITO,则加192nm),
· 平均粗糙度(Rrms):在100nm2方形面积内测得为0.4nm,
· 峰-谷粗糙度(Rpv):在100nm2方形面积内测得为3.8nm,
实施例2(对比)
为了对比的目的,在相同的沉积和热处理条件下,用实施例1中使用的相同的母体溶液在玻璃底物上直接沉积一层ATO层,但玻璃底物上不存在涂覆的ITO层。
得到的涂层的特性为:
· 表面阻抗:1890Ω/□,
· 光学透光度:85%,
· 工作性能:4.8到5.2eV,
· 涂层厚度:108nm,
· 平均粗糙度(Rrms):在100nm2方形面积内测得为1nm,
· 峰-谷粗糙度(Rpv):在100nm2方形面积内测得为3.6nm,
实施例3(对比)
为了对比的目的,在相同的沉积和热后处理条件下,用与实施例2使用的相同母体溶液在底物上直接沉积8个连续的ATO层。
这些涂层的特性为:
· 表面阻抗:50到55Ω/□,
· 光学透光度:65%,
· 工作性能:4.8到5.2eV,
· 涂层厚度:600nm,
· 平均粗糙度(Rrms)测量100nm2方形面积内为2.5nm,
· 峰-谷粗糙度(Rpv)测量100nm2方形面积内为8nm,
下表中列出了只涂覆ITO层的支持物、根据本发明实施例1(ATO/ITO)的涂覆支持物和根据对比实施例2和3的涂覆支持物的特性:
ITO | ATO/ITO实施例1 | ATO实施例2 | ATO实施例3 | |
表面阻抗(Ω/□) | 7.6 | 7 | 1890 | 50-55 |
光学透射性(%) | 83 | 82 | 85 | 65 |
工作性能(eV) | 4.3-4.6 | 4.8-5.2 | 4.8-5.2 | 4.8-5.2 |
涂层厚度(nm) | 192 | 45/192 | 108 | 600 |
Rrms(nm) | 4.7 | 0.4 | 1 | 2.5 |
Rpv(nm) | 31.1 | 3.8 | 3.6 | 8 |
本发明业已通过实施例和附图作了一般和详细的描述。但是,所属技术领域中的人员应了解,本发明不仅仅局限于发明中所揭示的实施方案,在不偏离本发明的精神的前提下,可以作相应的改动和变更。因此,除非是对背离本发明权利要求书限定的范围进行改变,其它的改变都包括在本发明的范围内。
Claims (14)
1.一种材料,包括:
玻璃或玻璃状陶瓷底物,
沉积在底物的一面、有至少一种单一或混合、掺杂或没有掺杂的透明导电氧化物的第一层,下面称为第一TCO层,
沉积在所述第一TCO层上、有至少一种单一或混合、掺杂或没有掺杂的透明导电氧化物的第二层,下面称为第二TCO层,
两个TCO层都具有:
所述的第一TCO层具有大于1nm的粗糙度,所述的第二TCO层具有小于或等于1nm的粗糙度,
所述的第一和第二TCO层的产品在可见光范围内的透光度为至少80%,
所述第二TCO层的工作性能高于所述第一TCO层的工作性能,并且高于4.6eV。
2.根据权利要求1所述的材料,其中所述的第二TCO层的工作性能高于4.8eV。
3.根据权利要求1所述的材料,其中两个TCO层包括至少一种为单一或混合的氧化物形式的氧化物或至少一种选自锡,锌,铟和镉的金属氧化物的混合物,其还可能与选自镓,锑,氟,铝,镁和锌的至少一种元素组合,所述的金属元素进入所述混合的氧化物所述氧化物的混合物的组合物中,或作为所述氧化物的掺杂剂。
4.根据权利要求1所述的材料,其中所述的第一TCO层包括如下基本组成:
●掺有锡的氧化铟(In2O3:Sn),又被称为ITO
●掺有氟的氧化锡(SnO2:F),
●掺有铝的氧化锌(ZnO:Al),
●掺有锑的氧化锡(SnO2:Sb)。
5.根据权利要求3所述的材料其中所述的第二TCO层基本上由至少一种掺杂或没有掺杂的氧化物组成,所述的氧化物选自:
SnO2
SnO2:F
SnO2:Sb
In4Sn3O12
Zn2In2O5
ZnSnO3
Zn2SnO4
GaInO3
MgIn2O4。
6.根据权利要求3所述的材料,其中所述的第二TCO层是掺杂了锑的氧化物层(ATO),SnO2:Sb。
7.根据权利要求1所述的材料,其中所述第二TCO层的厚度为30-200nm。
8.根据权利要求6所述的材料,其中所述第二TCO层的厚度为50-150nm。
9.根据权利要求7所述的材料,其中所述第二TCO层的厚度为0.1-3mm。
10.一种发光显示设备,包括一个阳极和一个阴极,所述的阳极部分包括如权利要求1所述的材料。
11.根据权利要求9所述的发光显示设备,其中所述的设备是有机发光二极管,在其阳极部分掺入了一种材料,所述的材料用在所述材料的第二TCO层和金属阴极之间插入的至少一个发光层涂覆。
12.一种制造材料或设备的方法,包括:
通过溶胶-凝胶型涂覆方法在已涂覆了第一TCO层的玻璃或玻璃陶瓷底物沉积上第二TCO层。
13.根据权利要求11所述的方法,其中该方法也包括对所述的第二TCO层进行热处理固化的步骤。
14.根据权利要求11所述的方法,其中所述的第一TCO层的初步沉积通过真空喷涂工艺或是用蒸汽相下的化学沉积形式进行。
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-
2002
- 2002-09-03 FR FR0210865A patent/FR2844136B1/fr not_active Expired - Fee Related
-
2003
- 2003-09-02 US US10/654,462 patent/US7161171B2/en not_active Expired - Lifetime
- 2003-09-03 KR KR1020057003720A patent/KR20050086413A/ko not_active Application Discontinuation
- 2003-09-03 JP JP2004534592A patent/JP2006516793A/ja not_active Abandoned
- 2003-09-03 CN CNA038243407A patent/CN101103653A/zh active Pending
- 2003-09-03 WO PCT/US2003/027759 patent/WO2004023436A2/en active Application Filing
- 2003-09-03 EP EP03794619A patent/EP1573702A4/en not_active Withdrawn
- 2003-09-03 AU AU2003265927A patent/AU2003265927A1/en not_active Abandoned
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103579524A (zh) * | 2012-07-27 | 2014-02-12 | 三星康宁精密素材株式会社 | 透明传导氧化物薄膜基板、制造方法、有机发光装置和光电池 |
CN103579524B (zh) * | 2012-07-27 | 2016-08-10 | 康宁精密素材株式会社 | 透明传导氧化物薄膜基板、制造方法、有机发光装置和光电池 |
CN109841743A (zh) * | 2013-03-12 | 2019-06-04 | Vitro可变资本股份有限公司 | 用于有机发光二极管和太阳能器件的透明导电氧化物涂层 |
CN109841743B (zh) * | 2013-03-12 | 2022-12-27 | 维特罗平板玻璃有限责任公司 | 用于有机发光二极管和太阳能器件的透明导电氧化物涂层 |
CN105776889A (zh) * | 2016-03-26 | 2016-07-20 | 上海大学 | 一种增强导电玻璃透过性及导电性的方法 |
CN105776889B (zh) * | 2016-03-26 | 2019-02-01 | 上海大学 | 一种增强导电玻璃透过性及导电性的方法 |
Also Published As
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AU2003265927A1 (en) | 2004-03-29 |
US20040113146A1 (en) | 2004-06-17 |
WO2004023436A2 (en) | 2004-03-18 |
KR20050086413A (ko) | 2005-08-30 |
JP2006516793A (ja) | 2006-07-06 |
EP1573702A4 (en) | 2008-07-23 |
US7161171B2 (en) | 2007-01-09 |
FR2844136A1 (fr) | 2004-03-05 |
WO2004023436A3 (en) | 2007-07-12 |
AU2003265927A8 (en) | 2004-03-29 |
EP1573702A2 (en) | 2005-09-14 |
FR2844136B1 (fr) | 2006-07-28 |
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