EP1458822A2 - Particulate coating - Google Patents
Particulate coatingInfo
- Publication number
- EP1458822A2 EP1458822A2 EP02758292A EP02758292A EP1458822A2 EP 1458822 A2 EP1458822 A2 EP 1458822A2 EP 02758292 A EP02758292 A EP 02758292A EP 02758292 A EP02758292 A EP 02758292A EP 1458822 A2 EP1458822 A2 EP 1458822A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- particles
- coating
- percent
- ito
- coating according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000000576 coating method Methods 0.000 title claims abstract description 30
- 239000011248 coating agent Substances 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 53
- 230000003287 optical effect Effects 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims description 8
- 239000008199 coating composition Substances 0.000 claims description 7
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 239000002019 doping agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims 1
- 239000011236 particulate material Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 238000007740 vapor deposition Methods 0.000 claims 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 6
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 description 5
- HCGFUIQPSOCUHI-UHFFFAOYSA-N 2-propan-2-yloxyethanol Chemical compound CC(C)OCCO HCGFUIQPSOCUHI-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- YHBWXWLDOKIVCJ-UHFFFAOYSA-N 2-[2-(2-methoxyethoxy)ethoxy]acetic acid Chemical compound COCCOCCOCC(O)=O YHBWXWLDOKIVCJ-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229920005570 flexible polymer Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/805—Electrodes
- H10K50/81—Anodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/36—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the electrodes
- H01L33/40—Materials therefor
- H01L33/42—Transparent materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/44—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the coatings, e.g. passivation layer or anti-reflective coating
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
- H10K2102/301—Details of OLEDs
- H10K2102/331—Nanoparticles used in non-emissive layers, e.g. in packaging layer
Definitions
- the present invention relates to the preambles of the independent claims and thus deals with how predetermined electrical and / or optical properties of coatings can be achieved.
- ITO indium tin oxide
- One problem with conventional ITO layers is that the conductivity of the layers is typically poorer than desired.
- An object of the present invention is to provide something new for commercial use.
- a first essential aspect of the present invention thus consists in providing a coating with predetermined electrical and / or optical properties, which is built up by particles, in which at least 10% of the particles have a size above 10 nm and at least 20 % of the particles are smaller than 50 nm.
- substantial amounts of the particles lie in a range around or between 10 nanometers and 40 nm; a particularly good conductive coating is obtained when 30%. the particles have a size around 10 nm and 70% of the particles have a size around 40 nm.
- a large part of the particles consists of those with a size in the range of 25 + - 5 nm. It has been found that a particularly good conductivity is also obtained with this size distribution.
- the coating is preferably made of.
- Indium tin oxide particles exist because ITO; represents a particularly preferred transparent, conductive oxide. To further increase the conductivity, these can be increased with a Dopants can be added, in particular with silver and / or titanium.
- Protection is also claimed for a coating composition in which the particles have a size distribution as is required to produce a coating according to the invention.
- a coating composition with such a size distribution can be obtained by first starting from the very small particles, as can be obtained in an easily redispersible form according to the known prior art.
- the particles produced in this way typically have a size of around 10 nm without aftertreatment.
- the typical size of these particles can be increased by heat treatment at different temperatures or for a different duration until the particles have grown.
- particles enlarged in this way remain readily redispersible without the formation of twins or the like.
- a multimodal size distribution for example with 30% particles around or smaller than 10 nm and 70% particles around or larger than 40 nm is desired, this can be achieved by simple mixing of different temperature-treated particles.
- the coating composition with an organic solvent without impairing and / or adversely affecting the desired positive properties.
- IPE isopropoxyethanol
- BGA butyl glycol acetate
- EG ethylene glycol
- BCA butyl carbitol acetate
- the coating composition can be used to produce a coating by first applying the particles with the fluid carrier, in particular by spin coating, the fluid carrier being removed, in particular by evaporation, and then heating the layer obtained to a temperature below 800 ° C.
- the temperature to which it is heated will also be well below 800 ° C, for example around 200 ° C. This makes it possible in particular to coat polymer materials and the like with the coating composition according to the invention without the coated polymer object being destroyed. This is especially true when the surface is primarily heated, as is known per se in the art.
- OLED organic light-emitting devices
- the OLEDs produced according to the invention have significant advantages over OLEDs which are built up with conventionally sputtered ITO layers.
- One reason for this may be that with conventional ITO layers that are sputtered, peaks appear in the ITO surface that can penetrate or not completely penetrate through the very thin, often monomolecular layers that form the OLED substances are covered and then lead to short circuits with a covering, additional ITO layer.
- a structure according to the invention has such a smooth surface that penetration of a very thin layer of OLED material by existing ITO tips is practically completely ruled out, so that there are no short circuits between the one below an OLED layer and the one above the OLED.
- Layer arranged ITO layer are to be feared.
- the layer flatness is a particular advantage of the present invention.
- organic substances which are common as organic binders. It is preferred if these organic substances are free of alkali or alkaline earth metal and / or at least no sub- has substantial proportions of the conductivity of the ITO or other ' layer-reducing ionic components. It should also be pointed out that an unexpected, particular advantage of the invention is that the layers obtained are not only highly conductive, especially when an organic binder is used, but also against peeling or peeling with adhesive strips or the like in particular are resistant.
- the layers can be applied to a suitable carrier, in particular a flexible polymer, and / or that the layers can be provided with a corresponding protective cover and / or other elements which are required in order to produce a fully functional device such as desired to educate ..
- Figure 1 shows the crystallite size as a function of the calcination temperature
- FIG. 2 shows a typical particle size distribution for a calcined Ito powder
- FIG. 3 specific resistance values of an Ito-
- FIG. 4 top views and sectional views of a raster electron micro-examined ITO-
- ITO powder is first produced in a conventional manner, as described, for example, in DE 100 44 214 AI. This powder is made without doping silver, titanium or the like. It has a particle size around 10 nm.
- parts of the particles are heat-treated at different calcination temperatures. There is an increase in the particle size as a result of the heat treatment, as is shown by way of example in FIG. 1.
- the particle size can be determined using conventional methods, for example using a Lecotrac LTU-150 Ultra-fine Particle Size Analyzer (UPA). A typical spectrum after heat treatment is shown in FIG. 2.
- UPA Ultra-fine Particle Size Analyzer
- the powders obtained are processed in a three-roll mill, together with a solvent and methoxyethoxyethoxyacetic acid (MEEE).
- MEEE methoxyethoxyethoxyacetic acid
- One of the substances IPE, BGA, - EG, BCA is used as solvent.
- the solutions obtained are applied to borosilicate glass supports by spin coating at 1500 rpm for 15 seconds, these are heated in air at 500 ° C., cooled to room temperature and then at 300 ° C. in a reducing atmosphere in 10% H2 and 90% 2 reheated.
- ITO coatings with a Obtained thickness of 800 nm.
- the resistance values are then determined using a 4-point measurement.
- Coatings are then examined which contain different proportions by weight of ITO particles with a typical size of 10 nm or a typical size of 40 nm. A minimum of the spec. Obtained resistance in the range of a weight fraction of 30% of ITO particles with a size of 10 nm. This is shown in FIG. 3.
- the coating solutions obtained are applied in the same way and the coated supports are heated. Again, the specific resistance values are determined and no differences are found.
- the layer, which is still warm, after the reduction, is arranged closely over a polymer plate made of PVC and brought to cool over it.
- the development over time of the resistance value is compared with that which is obtained directly in the air when it cools down. It is found that the coating cooled over a PVC plate has a surprisingly improved aging behavior.
- the experiments are repeated with polycarbonate sheets and polypropylene sheets and it is shown that improved aging behavior also results. This is attributed to the sealing of capillaries or the like by organic substances from the polymer plates.
Abstract
Description
Claims
Applications Claiming Priority (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10131494A DE10131494A1 (en) | 2001-07-02 | 2001-07-02 | A coating containing particles of specific particle size range useful in the production of optical devices, e.g. computer monitors and displays with anti-reflection properties |
DE10131494 | 2001-07-02 | ||
DE10203545 | 2002-01-29 | ||
DE10203545 | 2002-01-29 | ||
DE10205906 | 2002-02-13 | ||
DE10205906 | 2002-02-13 | ||
PCT/EP2002/007267 WO2003004571A2 (en) | 2001-07-02 | 2002-07-02 | Particulate coating |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1458822A2 true EP1458822A2 (en) | 2004-09-22 |
Family
ID=27214492
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02758292A Withdrawn EP1458822A2 (en) | 2001-07-02 | 2002-07-02 | Particulate coating |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP1458822A2 (en) |
AU (1) | AU2002325285A1 (en) |
WO (1) | WO2003004571A2 (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1701395B1 (en) | 2005-03-11 | 2012-09-12 | Novaled AG | Transparent light emitting element |
EP1895608A3 (en) * | 2006-09-04 | 2011-01-05 | Novaled AG | Organic light-emitting component and method for its manufacture |
DE102007013181B4 (en) | 2007-03-20 | 2017-11-09 | Evonik Degussa Gmbh | Transparent, electrically conductive layer |
DE202008005553U1 (en) | 2008-04-22 | 2008-08-14 | Evonik Degussa Gmbh | Highly conductive, transparent metal oxide layers by plasma immersion |
DE102008042694A1 (en) * | 2008-10-09 | 2010-04-22 | Evonik Degussa Gmbh | UV irradiation of indium tin oxide layers |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100214428B1 (en) * | 1993-06-30 | 1999-08-02 | 후지무라 마사지카, 아키모토 유미 | Infrared ray cutoff material and infrared cutoff powder used for the same |
US5763091A (en) * | 1994-10-27 | 1998-06-09 | Sumitomo Metal Mining Co., Ltd. | Electroconductive substrate and method for forming the same |
DE19625993A1 (en) * | 1996-06-28 | 1998-01-02 | Philips Patentverwaltung | Organic electroluminescent device with charge transport layer |
JP5358050B2 (en) * | 1998-06-26 | 2013-12-04 | 出光興産株式会社 | Light emitting device |
JP2000268973A (en) * | 1999-03-17 | 2000-09-29 | Tdk Corp | Organic el element |
JP2000268969A (en) * | 1999-03-17 | 2000-09-29 | Tdk Corp | Organic electroluminescent element |
JP4543446B2 (en) * | 1999-04-05 | 2010-09-15 | Tdk株式会社 | Organic EL device |
TW533446B (en) * | 2000-12-22 | 2003-05-21 | Koninkl Philips Electronics Nv | Electroluminescent device and a method of manufacturing thereof |
-
2002
- 2002-07-02 EP EP02758292A patent/EP1458822A2/en not_active Withdrawn
- 2002-07-02 WO PCT/EP2002/007267 patent/WO2003004571A2/en not_active Application Discontinuation
- 2002-07-02 AU AU2002325285A patent/AU2002325285A1/en not_active Abandoned
Non-Patent Citations (1)
Title |
---|
See references of WO03004571A3 * |
Also Published As
Publication number | Publication date |
---|---|
AU2002325285A1 (en) | 2003-01-21 |
WO2003004571A3 (en) | 2004-06-24 |
WO2003004571A2 (en) | 2003-01-16 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
AK | Designated contracting states |
Kind code of ref document: A2 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LI LU MC NL PT SE SK TR |
|
AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO SI |
|
RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: NANOGATE ADVANCED MATERIALS GMBH |
|
17P | Request for examination filed |
Effective date: 20041221 |
|
RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: AIR PRODUCTS AND CHEMICALS, INC. |
|
17Q | First examination report despatched |
Effective date: 20060913 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION HAS BEEN WITHDRAWN |
|
18W | Application withdrawn |
Effective date: 20091114 |