WO2007054255A1 - Procede de fabrication d’un revetement contenant des sorbants - Google Patents

Procede de fabrication d’un revetement contenant des sorbants Download PDF

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Publication number
WO2007054255A1
WO2007054255A1 PCT/EP2006/010615 EP2006010615W WO2007054255A1 WO 2007054255 A1 WO2007054255 A1 WO 2007054255A1 EP 2006010615 W EP2006010615 W EP 2006010615W WO 2007054255 A1 WO2007054255 A1 WO 2007054255A1
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WO
WIPO (PCT)
Prior art keywords
composition
sorbent
adhesion
carrier
application
Prior art date
Application number
PCT/EP2006/010615
Other languages
German (de)
English (en)
Inventor
Brigitte Schwaiger
Mandy Erdmann
Original Assignee
Süd-Chemie AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Süd-Chemie AG filed Critical Süd-Chemie AG
Publication of WO2007054255A1 publication Critical patent/WO2007054255A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3214—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
    • B01J20/3223—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating by means of an adhesive agent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3042—Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3206—Organic carriers, supports or substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3238—Inorganic material layers containing any type of zeolite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291—Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3295—Coatings made of particles, nanoparticles, fibers, nanofibers

Definitions

  • the invention relates to a process for producing a sorbent-containing coating on a support, a sorbent-coated support obtainable thereafter and its preferred use in electronic components.
  • electroluminescent components will only work well for a long time if a desiccant is present. These desiccants are sometimes referred to in the art as “getters”. The sensitivity of these components is due to the tendency for corrosion, in particular of the cathodes and the organic electroluminescent layer (s) in the presence of moisture. Therefore, these components are provided with a desiccant and sealed as well as possible under inert gas.
  • No. 6,226,890 describes a method for drying moisture-sensitive electronic components in a hermetic seal, wherein the desiccants consist of solid grains with particle sizes between 0.1 and 200 ⁇ m.
  • the desiccant grains are embedded in a binder.
  • the binder may be in the liquid phase or dissolved in the liquid phase.
  • a pourable mixture containing at least the desiccant particles and the binder is prepared, this mixture including between 10 and 90% by weight desiccant, based on the total mixture. This mixture is poured into the inside of a hermetic encapsulation to form a desiccant film, which is then cured.
  • US 2003/0037677 A1 describes the use of drying agents such as barium oxide, calcium oxide, phosphorus pentoxide, magnesium perchlorate; Calcium sulphate, molecular sieves, calcium bromide, calcium sulphate embedded in synthetic resins in sealed moisture-sensitive electronic devices.
  • the particle size of the desiccant grains used is between 0.001 and 0.1 .mu.m. Particularly preferred are phosphorus pentoxide, calcium oxide, barium oxide and magnesium perchlorate.
  • the polymeric binders used are polyethyl methacrylate, polydiallyl phthalate, polysulphone, phenoxy resins and UV-curing acrylates.
  • the drying agents known from the above documents have the disadvantage that they contain organic constituents in the form of binders and / or solvents. During the curing of desiccant films produced from these preparations or the thermal activation of these desiccant films, residues of solvents and possibly fragments of the polymers used in the form of monomers or short-chain oligomers can be converted into the gas phase. These organic contaminants damage electronic components based on organic compounds, in particular electroluminescent components.
  • DE 199 59 957 A1 describes platelet-shaped compacts based on an inorganic sorbent and a binder having a thickness of less than 700 ⁇ m, obtainable by compressing a mixture of the inorganic sorbent from about 20-60% by weight of the binder and about 10 - 15 wt .-% of water based on the total mixture at a pressure of about min. 70 Me- gapascal and calcining the green compact obtained at temperatures of at least about 500 0 C until the removal of most of the water content.
  • the compacts thus produced are used in electronic devices such as display device, in particular in electroluminescent components.
  • DE 100 65 946 A1 describes a platelet-shaped compact based on an inorganic sorbent and a binder having a thickness of less than 700 .mu.m, obtainable by compressing a mixture of the inorganic sorbent, the binder, water and possibly pressing aids at a pressure of at least 70 megapascals, wherein in the mixture, the weight ratio of the dry sorbent and the dry binder is between about 4 and 0.7 and the water content of the mixture determined at 160 0 C between about 8 - 20%. Calcining the green compact obtained at temperatures of at least about 500 0 C until the substantial removal of the water content.
  • the compacts thus produced are used in electronic devices such as display devices, in particular in electroluminescent components.
  • WO 2005/050736 A1 describes a method for attaching a getter material to a surface, wherein the getter composition contains not only particles of at least one getter but also particles of at least one inorganic binder.
  • compositions and methods also often have the disadvantage that after the sorbent-containing compositions have been applied to the support, activation of the sorbent in a separate step is required.
  • the present invention is therefore an object of the present invention to provide a method for producing a sorbent-containing coating on a support, which avoids the disadvantages of the prior art, allows easy production and application of the sorbent coating and as uncomplicated as possible, a particularly well-adhering and provides highly sorbent coating on the carrier.
  • this object is achieved by the method according to claim 1.
  • Providing a composition comprising at least one sorbent and at least one adhesion-promoting component, wherein the at least one adhesion-promoting component is used in liquid or dissolved form b.
  • Providing a carrier c. Applying the composition to the support, wherein during or after the application, a temperature treatment at a temperature between about 100 and 500 ° C and a reduced pressure between about 10 "7 bar and 10 ⁇ 1 bar,
  • At least one adhesion-promoting component is used in the composition for application to the carrier.
  • Adhesion-promoting is to be understood as meaning that a proportion of the other component (s), including the sorbent, is not excluded from the adhesion of the composition to the support.
  • Insofar shaftungsverffennd also includes “adhesion support”.
  • the at least one adhesion-promoting component used according to the invention stabilizes the advantageous porous matrix and the adhesion of the sorbent particles to one another and to the other components of the composition or the carrier surface even at the temperatures used for application.
  • advantageous adhesion and stability of the layer on the support the formation of a favorable porous matrix of the composition and activation of the sorbent is made possible.
  • At least one adhesion-promoting component is used in liquid or dissolved form.
  • at least one adhesion-promoting component in liquid or dissolved form, in particular using the temperature treatment described here at reduced pressure.
  • a particularly fine distribution of the adhesion-promoting component is achieved.
  • the composition is applied to the carrier, a larger contact surface is formed between the composition or the sorbent and the carrier contained therein and better adhesion to the carrier.
  • the adhesion of the particulate components of the composition eg, the sorbent particles
  • the composition dries on the support, fine particles are formed.
  • adhesion-promoting components are particularly suitable which soften at relatively low temperatures or can provide an adhesive or sticky surface.
  • a softening or sticking of the at least one adhesion-promoting component at a temperature between about 100 and 500 0 C, in particular between about 100 and 450 0 C, more preferably between about 100 and 350 0 C, optionally more than 300 to 500 0 C take place.
  • adhesion-promoting component has a transformation temperature and a transformation point, determined according ISO 7884-8, of between about 100 and 500 0 C, in particular between about 100 and 450 0 C, more preferably between about 100 and 350 0 C, optionally more than 300 up to 500 0 C on.
  • adhesion-promoting components are therefore preferably used in solid form for providing the composition according to step a) above, in particular in particulate form (see below).
  • the adhesion-promoting components in liquid or dissolved form are preferably selected from (solutions of) borates and / or water glasses, in particular sodium water glasses (see below).
  • these components enable particularly well adhering coatings having a high sorption capability in the case of the temperature treatment according to the invention under reduced pressure as described herein.
  • the upper limit may be the maximum amount soluble in the respective solvent (eg water), expressed as% by weight, based on the total solution.
  • the solids content of the solution will be between about 1 and about 50% by weight.
  • the composition according to the invention comprises between about 0.1 and 10% by weight of the at least one adhesion-promoting component, calculated in each case without solvent for the adhesion-promoting component and based on the total weight of the composition as described herein.
  • the at least one adhesion-promoting component is an inorganic component.
  • sorbent-containing coating generally refers to any sorbent-containing compositions that have been applied to (the surface of) a support (s).
  • the coating can have any thickness. According to a preferred embodiment, however, the thickness of the coating is between about 1 .mu.m and 10 mm, preferably between about 5 .mu.m and 1 mm, more preferably between about 10 .mu.m and 500 .mu.m, in particular between about 15 .mu.m and 200 .mu.m.
  • the dimensions of the coating in terms of length and width are in principle arbitrary and usually limited by the space available for application to the desired carrier or in the component of interest.
  • An advantage of the invention lies in the great flexibility of the application and dimensioning of the composition of the invention and the excellent adhesion despite preferably high content of sorbent.
  • the films are preferably formed on (solid) supports such as glass, plastic or metal, which have been found to be suitable for encapsulating moisture-sensitive electronic components.
  • solid supports such as glass, plastic or metal
  • other carriers may be used depending on the application, in particular rigid or flexible carriers.
  • no adhesive is used in the application to the carrier.
  • the application (application) of the composition of the invention as a layer or coating on the substrate is thus preferably carried out directly without a separate adhesive or adhesive layer.
  • the sorbent-containing coating (composition) is thus provided in the form of a (preferably directly) adhering or bonded to the support.
  • the reduced pressure is between about 10 and the subsequent heat treatment used in the application of the composition onto the carrier is "7 bar and 10 '1 bar, in particular between 10' 7 bar and 10" 3 bar, more preferably between 10 '7 bar and 10 ⁇ 5 bar. It has been found that a simultaneous gentle and effective removal of water or solvent from the composition can be achieved at such a pressure and the temperatures defined herein, so that a high sorption capacity of the composition without decomposition is achieved. Disturbance or impairment of their porous matrix or adhesion to the carrier can be advantageously achieved.
  • a temperature which lies at or above the transformation point at least one adhesion-promoting component. Therefore, the temperature during application of the composition is particularly preferably between 0 and 100 ° C., in particular 0 and 50 ° C., more preferably between 0 and 20 ° C., above the transformation temperature of at least one adhesion-promoting component.
  • temperatures slightly below the transformation temperature of at least one adhesion-promoting component in particular up to 50 0 C, in particular 0 and 20 0 C below the respective transformation temperature can be used, as already a positive influence of the adhesion-promoting component on the formation of a well-adherent sorbent coating on the carrier.
  • the temperature treatment of the present invention is carried out after the application of the composition under reduced pressure as set forth herein. It is preferred that the temperature treatment is directly followed by the application of the composition to the support, in particular no drying at normal pressure and in particular a temperature of more than 100 ° C before.
  • sorbent is used for both adsorbents and absorbents. All sorbent materials should be included, regardless of the sorption mechanism.
  • the at least one sorbent can be any sorbent or sorbent mixture known or suitable for the person skilled in the art.
  • other (gaseous) substances such as ammonia, volatile amines or oxygen, in principle of interest.
  • an attack on the cathodes of an EL device can also be triggered by gases which, in addition to water, form during the setting of the binding agent or solvent used for sealing.
  • the action of oxygen often leads to the failure of luminescent components.
  • Both organic and inorganic sorbents can be used. Preferred is the use of one or more inorganic sorbents.
  • the sorbent is a desiccant.
  • the at least one sorbent comprises a natural or artificial zeolite. Further non-limiting examples are amorphous silica, aluminum hydroxide, calcium oxide, barium oxide or calcium sulfate. It is also possible to use mixtures of two or more sorbents. In principle, however, organic sorbents are also included, as described, for example, in EP 1 014 758 A2, US 2002/0090531 A1 or US 2003/0110981.
  • the composition preferably contains no calcium chloride, since the liquefaction of this desiccant on moisture absorption can affect or damage both the composition itself, as well as their adhesion to the carrier and thus the moisture-sensitive device or the moisture-sensitive device. More preferably, the composition applied according to the invention generally does not contain any components that liquefy when moisture is absorbed.
  • the at least one sorbent is used in particulate form. It is further preferred that the D 50 value of the sorbent used, in particular particular of the zeolite, between about 2 and 8 microns, in particular about 3 and 6 microns.
  • the D 90 value is preferably less than 15 ⁇ m, in particular between 5 and 12 ⁇ m.
  • the at least one adhesion-promoting component comprises a glass solder, a low-melting glass or water glass, in particular a silicate, a boric or a phosphorus-containing component.
  • a glass solder a low-melting glass or water glass
  • a silicate a boric or a phosphorus-containing component.
  • water glasses and low melting SiO 2 -containing glasses can be cited.
  • particularly preferred borate or phosphate-containing components are boron or alkali phosphate glass solders. These provide particularly good results.
  • Particularly preferred glass solders or low-melting glasses have, for example, the following composition (in% by weight):
  • Both individual adhesion-promoting components and mixtures of two or more adhesion-promoting components in the composition can be used.
  • the at least one adhesion-promoting component is preferably in an amount of up to about 10% by weight, more preferably in the range of between about 0.1 and 7% by weight, based on the total weight of the composition containing at least one sorbent (sorbent-containing composition). It is further preferred that the at least one adhesion-promoting component at a temperature of up to 500 0 C, in particular at most 48O 0 C, preferably in the range of about 250 to 480 0 C softens.
  • Some preferably used glass solders have for example a transformation temperature of about 300 to 330 0 C, in particular 305 to 315 ° C. Above the transformation temperature the glass solders soften. As a result, the particles in the composition stick together and a good bond to the substrate is supported.
  • a borate in particular sodium borate, is used as the adhesion-promoting component. It is further preferred that between about 0.1 and 10 wt .-%, in particular about 0.5 and 7 wt .-% borate, based on the total weight of the sorbent composition are used.
  • the at least one adhesion-promoting component particularly preferably comprises or consists of a sodium borate and / or a water glass.
  • Borates are preferably used as solutions, in particular aqueous solutions having a solids content of borate of about 1 to 50% by weight, in particular about 20 to 25% by weight, based on the total solution.
  • aqueous solutions having a solids content of borate of about 1 to 50% by weight, in particular about 20 to 25% by weight, based on the total solution.
  • Particularly preferred is a binary B 2 O 3 -Na 2 O system with a content of B 2 O 3 between about 15 and 20 mol% and 85 to 80 mol% Na 2 O.
  • Such binary systems are characterized by a low melting point out.
  • Water glasses are preferably used as solutions, in particular aqueous solutions having a solids content of water glass of about 1 to 50% by weight, in particular dere about 30 to 40% by weight, based on the total solution used.
  • the molar ratio of SiO 2 to alkali oxide is preferably between 2.1 and 3.9.
  • the invention makes it possible, in particular, to produce a coating with a particularly high content of sorbent.
  • the composition used for the application based on the solids content, to at least 80 wt .-%, preferably at least 90% by weight, more preferably at least 95 wt .-%, in particular at least 98 wt .-%, in particular at least 99 9% by weight of at least one sorbent as defined herein.
  • adhesion-promoting components are contained as main constituents in the composition.
  • the composition based on the solids content of at least one sorbent and at least one adhesion-promoting component. This provides both a particularly high sorbent content and good interaction between the adhesion-promoting component and the sorbent in the composition.
  • the duration of the heating at reduced pressure during or after the application of the composition to the carrier can in principle be chosen arbitrarily and routinely optimized by the person skilled in the art for the respective composition.
  • the duration should at least be chosen so as to cause the composition to adhere to the carrier.
  • the duration should also be selected so that a good activation or drying of the sorbent used is already at the same time as the Forming adhering to the carrier layer takes place. In general, heating under reduced pressure for about 1 to 240 minutes will be sufficient.
  • the composition containing at least one sorbent does not contain a binder (except for the adhesion-promoting component). According to a particularly preferred embodiment of the invention, therefore, the composition does not comprise any natural or synthetic layered silicate.
  • the carrier is heated before or during the application of the composition, in particular before the application of the composition.
  • no compression or pressing of the composition or sorbent-containing coating takes place within the scope of the method according to the invention.
  • This is intended to ensure an impairment of the advantageous porous matrix and thus the accessibility of the sorbent, for example, for water vapor.
  • it can be but be beneficial, for example, to assist in the adhesion of the composition during or after application to the support with pressure, for example using a pressing pressure on a roller, a stamp or the like.
  • the composition can be applied in powder form or in liquid or fluid form, in particular as a paste.
  • at least one liquid phase may also be contained in the composition.
  • liquid phase is understood as meaning any liquid which can serve as solvent or suspending agent for the at least one sorbent.
  • the liquid phase also serves as a solvent or suspending agent for the at least one adhesion-promoting component.
  • the liquid phase is used in mixing the sorbent and the adhesion-promoting component to produce a slurry which can then be more easily applied (e.g., without dusting) to the support.
  • the liquid phase is preferably removed.
  • the liquid phase is not taken into account.
  • it is an inorganic liquid, in particular water. But it can also be used mixtures of different liquids.
  • the proportion of the composition, as far as it is not used in powder form, of at least one liquid component, in particular water, is preferably between 50 and 20% by weight, in particular between 40 and 30% by weight, based on the total composition.
  • the composition for application to the carrier becomes a paste or slurry provided with a dispersion or suspension of the at least one sorbent and the at least one adhesion-promoting component in the liquid phase.
  • This favors the formation of a highly porous and well-adherent matrix after removal of the liquid phase.
  • the preparation of such a paste or slurry can be carried out, for example, by simple mixing or stirring of sorbent, adhesion-promoting component and optionally liquid component.
  • This mixture is preferably not a solid mixture or plasticine but a liquid or fluid or pourable composition. This allows, inter alia, a light and uniform application to the carrier and ensures a particularly advantageous adhesion.
  • the composition according to the invention preferably has a solids content of more than 15% by weight, in particular 15 to 80% by weight, more preferably about 25 to 78% by weight, even more preferably about 50 to 75 wt .-% on.
  • the viscosity of such a paste or slurry is preferably between about 10 and 7000 mPa.s, preferably 10 and 6000 mPa.s, more preferably 10 and 1000 mPa.s, in particular between 100 and 1000 mPa.s, more preferably between 100 and 500 mPa.s at one Shear rate of 100 s -1 (determination method see below)
  • Such pastes or slurries preferably show no or only little syneresis or separation or settling of individual components, a high storage stability and a viscosity which is suitable for the respective application Values for the solids content and the viscosity thus apply both to the composition according to the invention before application to the support and to the film-like composition already applied to the support (before drying or activation).
  • compositions according to the invention may be applied to the carrier in any suitable manner.
  • Such methods are known in principle to the person skilled in the art.
  • the application may be by spraying, sprinkling, pouring, dispensing, knife coating, spin coating or printing, in particular screen printing, rolling or the like.
  • the carrier is a rear wall (a so-called back lid w ) of an electronic component, in particular an OLED or OLED display.
  • an electronic component in particular an OLED or OLED display.
  • the carrier is a carrier made of metal, glass or plastic.
  • the application of the composition comprising at least one sorbent into a depression or cavity of the carrier takes place.
  • a depression or cavity may be produced in any manner known to those skilled in the art, depending on the carrier material used.
  • the depression or cavity can already be produced during molding or casting of the carrier.
  • embossing, punching, milling or the like is conceivable.
  • a method will be used to fabricate the cavity, wherein a heating or other treatment resulting in softening of the substrate surface is used. This treatment can then be used at the same time for the inventive application of the sorbent composition.
  • composition comprising at least one sorbent after application to the support and the temperature treatment according to the invention at reduced pressure is preferably already in activated form, and thus no separate activation of the at least one sorbent is required to fully provide the sorption properties of the sorbent.
  • a separate or additional activation step for activating the sorbent may optionally be carried out after application of the composition to the support.
  • Such an activation step may e.g. by means of microwave energy, infrared radiation, muffle furnace, vacuum drying oven or the like.
  • microwave energy infrared radiation
  • muffle furnace infrared radiation
  • vacuum drying oven or the like.
  • the composition applied to the carrier contains at least 30% by weight, in particular at least 50% by weight, preferably at least 75% by weight, more preferably at least 85% by weight, even more preferably at least 90% by weight .-%, more preferably at least 95 wt .-%, even more preferably at least 98 wt .-%, even more preferably at least 99 wt .-%, even more preferably at least 99.5 wt .-% of sorbent, based on the total weight of the sorbent composition.
  • the sorbent-containing coatings according to the invention are preferably able, in addition to water vapor, other gases (eg Ammonia, amines, oxygen).
  • gases eg Ammonia, amines, oxygen.
  • the sorption of different substances is naturally dependent on the choice of the respective sorbent. Since the sorbents preferably used in the present invention have a high sorption capacity and / or speed, an electronic component or device to be used in need not be completely hermetically sealed, ie the rate of diffusion of water vapor into the device may be greater than 0 be.
  • the selection of a suitable substance for sealing the device z. As an epoxy resin, since the critical time to which this substance has reached its final low Wassermannampf biolass- stechnik must be extended by the use of the sorbent film.
  • a rheological additive can be added to the composition according to an embodiment of the invention.
  • the additives known to the person skilled in the art can be used (for example smectites, precipitated silica, pyrogenic silica).
  • smectite clay, in particular bentonite has proved to be particularly favorable since it can simultaneously act as a binder and rheological additive.
  • additional components which may be present in the composition according to the invention may, for example, be selected from the group of superplasticizers, (fluxing agents), sintering aids, rheological additives, pigments and preservatives. Such substances are familiar to the expert and therefore need not be discussed further here.
  • the compositions of the invention can also be protected by the addition of a biocide against infestation with microorganisms. These agents, such as Parmetol K40 or Acticid LV706, may be as low as possible Concentration, for example, about 0.1% based on the total mixture used.
  • the present invention relates to an electronic device or component, in particular an electroluminescent component such as an OLED display or panel, a polymer light-emitting component, CCD sensors (charge-coupled devices) or micro-electro-mechanical sensors ( MEMS) containing a sorbent-containing coating as described herein or preparable by a method as described herein.
  • an electroluminescent component such as an OLED display or panel
  • CCD sensors charge-coupled devices
  • MEMS micro-electro-mechanical sensors
  • the (micro) electronic devices or components are e.g. in a capsule hermetically sealed by connecting a substrate of the OLED to the capsule element so that the microelectronic elements are enclosed in a watertight capsule.
  • the substrate of the OLED may be bonded with a suitable adhesive or any other method known in the manufacture of electronic components.
  • a suitable adhesive is, for example, an epoxy resin.
  • the manufacturing steps described above are all part of the usual knowledge of those skilled in the field of manufacturing electronic components and are carried out in the usual way.
  • the sorbent-containing composition may be disposed on the substrate (back lid) of the OLED and / or the microelectronic elements and / or the capsule element.
  • Another aspect of the present invention relates to a support having a sorbent-containing coating obtainable by the process as described herein.
  • such carriers are distinguished by particularly good adhesion and intimate bonding of the carrier material with the sorbent-containing coating, without it being necessary to use adhesives or adhesives.
  • a sorbent content of the coating of more than 90 wt .-%, in particular more than 95 wt .-% allows.
  • the sorbent-containing composition or coating consists entirely or essentially of at least one sorbent.
  • the carrier is the back wall (back lid) of an electronic component, in particular an OLED as described above.
  • a further aspect of the invention is thus directed to an electronic component, in particular an OLED or OLED display, comprising a carrier with a sorbent-containing coating as described herein, and a method for its production.
  • an OLED Organic Light Emitting Diode
  • ITO indium tin oxide
  • an organic material is applied as the anode.
  • the light is created in these active organic layers when pairs of electrons and "holes” recombine and produce a photon.
  • Suitable "hole transport layer", “emitter” or “electron transport layer” organic layers are known in the art.
  • one or more additional layers are therefore applied for the transport of charge carriers.
  • a cathode (optically non-transparent) metal contact preferably with low work function.
  • an external voltage is applied between the cathode and the anode, it emits light whose color depends on the materials used. hangs.
  • This component is provided for encapsulation with a rear wall, wherein the inventively coated with a sorbent-containing composition carrier can be used.
  • a sorbent-containing coating is thus applied to at least one arbitrary point on the inside in relation to the finished OLED capsule.
  • the connection of the back wall (back lid) with the OLED substrate is usually carried out by means of an adhesive for sealing.
  • the viscosity of the pastes or suspensions or dispersions was measured according to DIN 53019 / ISO 3219.
  • a Rheostress 600 rheometer from Haake (DE) was used with a Z40 DIN Ti cylinder according to the manufacturer's instructions.
  • the particle size was determined using a Mastersizer S Ver. 2.17 (Malvern Instruments GmbH,dorfberg, DE) according to the manufacturer's instructions.
  • the data of the D50 and D90 values refers to the sample volume. The measurement was carried out in water.
  • FIG. 1 shows the schematic structure of an electronic component (OLED) according to the present invention.
  • OLED organic electroluminescent device measuring 45 mm x 29 mm was produced using the glass lid prepared in Example 1 as the back of the device.
  • the structure of the OLED is shown schematically in FIG.
  • the rear wall (6) with the sorbent coating (9) according to the invention by means of an adhesive (7; Epoxykleber) on the glass substrate (1) with the cathode (3), the anode (4) and the light-emitting layer (5) of the component attached and sealed as much as possible.
  • the capsule 8 is formed.
  • the size of the luminous pixels of the component was determined. Subsequently, the component was subjected to conditions of 85 ° C and 85% RH for 500 hours. After this time, the size of the luminous pixels and the number of non-luminous pixels (dark spots) were determined. It was found that no non-luminous pixels appeared, and the size of the pixels was unchanged from the original component.
  • a paste was prepared consisting of zeolite 4A (54.1% by weight), glass frit (Glass Frits) (5.4 wt .-%) and water (to 100 wt .-%) as a solvent.
  • the glass frit consists of 7.11 wt% SiO 2 , 2.13 wt% Al 2 O 3 , 8.38 wt% B 2 O 3 , 0.53 wt% CaO, 12.03 wt% ZnO and 69, 82 wt% Bi 2 O 3 .
  • the paste is stirred for 10 minutes with the disperser.
  • a paste was prepared consisting of zeolite 4A (54.1 wt .-%), sodium borate (5.4 wt .-%) in the form of an aqueous solution and water (to 100 wt .-%) as a solvent , The paste is stirred for 10 minutes with the disperser. The paste showed no significant syneresis after one week.
  • Example 6 Analogously to Example 3, a paste was prepared consisting of zeolite 4a (54.1 wt .-%), water glass (5.4 wt .-%) in the form of an aqueous solution and water (to 100 wt .-%) as a solvent , The paste is stirred for 10 minutes with the disperser. The paste showed no significant syneresis after one week.
  • Example 6
  • the pastes described in Examples 3, 4 and 5 were each applied with 2 g of commercially available glass slides by means of dispensers to obtain coated eyelids.
  • the layer thickness was about 200 ⁇ m.
  • a set of the coated eyelids thus obtained were pre-dried at 150 ° C. under normal pressure. Another set were dried at 300 0 C for 30 minutes at a pressure of 10 -6 bar in a vacuum drying cabinet, and a further set of coated lids was at 400 0 C in vacuum (10 -6 bar) dried for 30 minutes also in a vacuum drying cabinet , In addition, additional tests were carried out at 400 ° C. under atmospheric pressure with another set of coated eyelids. The adhesion or detachment of parts of the coating was visually checked. In addition, the adhesion was tested.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Electroluminescent Light Sources (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

L’invention concerne un procédé de fabrication d’un revêtement contenant des sorbants sur un support, ledit procédé comportant les étapes suivantes : (a) utiliser une composition comprenant au moins un sorbant et au moins un composant adhésif, le ou les composants adhésifs étant sous forme liquide ou dissoute ; (b) utiliser un support ; (c) placer la composition sur le support, un traitement thermique à une température comprise entre environ 100 et 500 °C et à une pression réduite comprise entre environ 10-7 bar et 10-1 bar étant effectué pendant ou avant l’application.
PCT/EP2006/010615 2005-11-09 2006-11-06 Procede de fabrication d’un revetement contenant des sorbants WO2007054255A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005053431 2005-11-09
DE102005053431.7 2005-11-09

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WO2007054255A1 true WO2007054255A1 (fr) 2007-05-18

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024017556A1 (fr) 2022-07-21 2024-01-25 Volkswagen Aktiengesellschaft Procédé et système de production d'un élément de sorption pour éliminer du dioxyde de carbone de l'air ambiant

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4089185A (en) * 1974-10-31 1978-05-16 Eckhard Kellner High vacuum pump system
EP0711598A2 (fr) * 1994-11-14 1996-05-15 Praxair Technology, Inc. Adsorbants sélectifs pour l'oxygène

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4089185A (en) * 1974-10-31 1978-05-16 Eckhard Kellner High vacuum pump system
EP0711598A2 (fr) * 1994-11-14 1996-05-15 Praxair Technology, Inc. Adsorbants sélectifs pour l'oxygène

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024017556A1 (fr) 2022-07-21 2024-01-25 Volkswagen Aktiengesellschaft Procédé et système de production d'un élément de sorption pour éliminer du dioxyde de carbone de l'air ambiant
DE102022207442A1 (de) 2022-07-21 2024-02-01 Volkswagen Aktiengesellschaft Verfahren und Anlage zur Herstellung eines Sorptionselements zur Abtrennung von Kohlenstoffdioxid aus der Umgebungsluft

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