DE4439722A1 - Prodn. of strong ceramic titanium di:oxide thin film at low temp. - Google Patents

Prodn. of strong ceramic titanium di:oxide thin film at low temp.

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Publication number
DE4439722A1
DE4439722A1 DE19944439722 DE4439722A DE4439722A1 DE 4439722 A1 DE4439722 A1 DE 4439722A1 DE 19944439722 DE19944439722 DE 19944439722 DE 4439722 A DE4439722 A DE 4439722A DE 4439722 A1 DE4439722 A1 DE 4439722A1
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Germany
Prior art keywords
ceramic layers
pref
layers
support
pts
Prior art date
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Ceased
Application number
DE19944439722
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German (de)
Inventor
Bernd Dr Penth
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Individual
Original Assignee
Individual
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
Priority claimed from DE19944421978 external-priority patent/DE4421978A1/en
Application filed by Individual filed Critical Individual
Priority to DE19944439722 priority Critical patent/DE4439722A1/en
Priority to US08/737,890 priority patent/US5885657A/en
Priority to DE59508772T priority patent/DE59508772D1/en
Priority to EP95923174A priority patent/EP0766657B1/en
Priority to PCT/DE1995/000819 priority patent/WO1996000198A1/en
Publication of DE4439722A1 publication Critical patent/DE4439722A1/en
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5041—Titanium oxide or titanates
    • 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
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • 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
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid phase
    • C03C17/256—Coating containing TiO2
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20—Light-sensitive devices
    • H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20—Light-sensitive devices
    • H01G9/2068—Panels or arrays of photoelectrochemical cells, e.g. photovoltaic modules based on photoelectrochemical cells
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/212—TiO2
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
    • C03C2217/45—Inorganic continuous phases
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475—Inorganic materials
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/542—Dye sensitized solar cells

Abstract

Prod. of ceramic films is carried out with a dispersion (I) prepd. by (i) hydrolysing a hydrolysable Ti cpd., e.g. 10-40 pref, 29 pts.wt. Ti(OPr-i)4, (II) with 5-20 pref. 14 pts.wt. water, (ii) peptising by adding a strong acid, pref. 42 pts.wt. 25% HCl, and stirring; and (iii) adding 10-25, pref. 15 pts.wt. nano-crystalline TiO2 (IIIA) and/or crystalline TiO2 (IIIB) to the soln. and stirring. The coatings are produced by applying (I) as a thin layer, e.g. 0.1-10 microns, to a glass, metal, ceramic or plastics substrate, e.g. by spreading, spraying, or printing, and hardening at 100 deg C pref. within 5 min. in a hot air stream.

Description

In der zu dieser Zusatzanmeldung gehörenden Hauptanmeldung P 44 21 978.4-33 ist die Herstellung von photovoltaischen Elementen beschrieben.In the main application P 44 21 978.4-33 belonging to this additional application, the Manufacture of photovoltaic elements described.

In der zur oben zitierten Anmeldung gehörenden Zusatzanmeldung P 44 37 767.3 ist die Herstellung photoaktiver Schichten nach dem gleichen Verfahren beschrieben.In the additional application P 44 37 767.3 belonging to the above-cited application, the Production of photoactive layers described by the same method.

Ein wesentlicher Teil der zitierten Erfindungen besteht darin, daß nach dem dort beschriebenen Verfahren reine nanoskalige Titandioxidschichten oder Schichten aus anderen nanoskaligen Halbleitermaterialien mit guter mechanischer Festigkeit bereits bei Temperaturen bis maximal 150°C hergestellt werden können.An essential part of the inventions cited is that according to the one described there Processes pure nanoscale titanium dioxide layers or layers of other nanoscale Semiconductor materials with good mechanical strength even at temperatures up to a maximum 150 ° C can be produced.

Nach dem vorher bekannten Stand der Technik waren zum Erreichen gleicher Festigkeit der Halbleiterschicht Temperaturen oberhalb 400°C erforderlich.According to the previously known prior art were to achieve the same strength Semiconductor layer temperatures above 400 ° C required.

Ziel der vorliegenden Erfindung war die Herstellung keramischer Schichten statt aus Halbleitermaterialien auch aus oder in Kombination mit anderen Materialien, wobei der Einsatzzweck von den in den oben zitierten Anwendungen Photovoltaik und Photoaktivität abweichen kann. Wie sich bei den Arbeiten zu dieser Anmeldung gezeigt hat, liegt die Festigkeit von anderen Materialkombinationen teilweise noch oberhalb der in den zitierten Anmeldungen beschriebenen Festigkeiten. Die auf diese Weise bei niedrigen Temperaturen herstellbaren rein keramischen Schichten sind für eine ganze Reihe herkömmlicher Anwendungen von Keramik einsetzbar. Dazu zählen auch der Einsatz als katalytisch aktive Schichten, sowie der Einsatz als filteraktive Schichten für den Einsatz als Filtermembranen für die Ultrafiltration.The aim of the present invention was to produce ceramic layers instead of Semiconductor materials also made of or in combination with other materials, the Purpose of the photovoltaic and photoactivity applications mentioned above can deviate. As has been shown in the work on this application, the The strength of other material combinations is sometimes even higher than that cited in the Strengths described in applications. That way at low temperatures Purely ceramic layers that can be produced are conventional for a whole series Applications of ceramics can be used. This also includes the use as a catalytically active Layers, as well as use as filter-active layers for use as filter membranes for the ultrafiltration.

Dies geschieht erfindungsgemäß dadurch, daß auf eine (eventuell poröse für Filtermembranen) flache Unterlage oder eine Rohrinnenwandung eine Paste in einer Schichtdicke von < 1 mm aufgetragen wird, wobei die stark saure Paste aus einem pulverförmigen Metalloxid und einer sauer hydrolysierten metallorganischen Verbindung besteht.This is done according to the invention in that a (possibly porous for filter membranes) a flat surface or a tube inside a paste in a layer thickness of <1 mm is applied, the strongly acidic paste consisting of a powdered metal oxide and acid hydrolyzed organometallic compound.

Die Paste wird erfindungsgemäß in diesem stark sauren Zustand aufgebracht und bei einer Temperatur bis max. 150°C innerhalb weniger Minuten verfestigt. Zur Entfernung überschüssiger Säure wird mit Wasser gewaschen und erneut bei Raumtemperatur oder leichter Erwärmung getrocknet.According to the invention, the paste is applied in this strongly acidic state and at one Temperature up to max. 150 ° C solidified within a few minutes. For removal Excess acid is washed with water and again at room temperature or dried slightly warming.

Statt der reinen Metalloxidpulver können auch Zusätze verschiedener anderer anorganischer oder organischer Verbindungen verwendet werden.Instead of pure metal oxide powders, various other inorganic additives can also be added or organic compounds can be used.

Der Vorteil gegenüber den bekannten Herstellungsverfahren für keramische Schichten besteht erfindungsgemäß also darin, daß das Ziel der Herstellung keramischer Schichten bereits bei milden thermischen Bedingungen erreicht wird. Neben den Einsparungen bei den Herstellungskosten für rein keramische Schichten ergeben sich völlig neue Möglichkeiten, da auch thermisch empfindliche Verbindungen, wie z. B. organische Verbindungen, mit definierten katalytischen optischen oder elektrischen Eigenschaften im Keramikverbund fest eingeschlossen werden können. The advantage over the known production processes for ceramic layers is So according to the invention in that the goal of producing ceramic layers already mild thermal conditions is achieved. In addition to the savings on the Manufacturing costs for purely ceramic layers open up completely new possibilities because also thermally sensitive connections, such as. B. organic compounds with defined catalytic optical or electrical properties in the ceramic composite can be included.  

Ein wesentliches Merkmal der auf diese Weise herzustellenden keramischen Schichten zeigt sich weiterhin darin, daß diese keramischen Schichten eine hervorragende Haftung auf glatten Oberflächen zeigen. Beschichtungen aus der Materialkombination Titandioxid (sauer hydrolysiert aus Titantetraisopropylat) und Aluminiumoxid zeigen so hervorragende Festigkeit auf Glas und Metallen.An essential feature of the ceramic layers to be produced in this way shows furthermore that these ceramic layers have excellent adhesion to smooth Show surfaces. Coatings from the material combination titanium dioxide (acid hydrolyzed from titanium tetraisopropylate) and aluminum oxide show excellent strength on glass and metals.

AusführungsbeispielEmbodiment

Zu 10 ml Wasser gibt man unter Rühren 3 ml Titantetraisopropylat und 3 ml konzentrierte Salzsäure. Sobald die Lösung klar wird, gibt man unter Rühren 3 g Aluminiumoxid CT 3000 SG (Fa. ALCOA) zu. Es wird 2 Stunden weitergerührt. Die entstandene Paste wird mit einem Rakel auf einer Glasplatte oder einer Stahlplatte (VA-Stahl) in einer Dicke von 300 µm aufgetragen. Die entstandene Schicht wird mit einem Heißluftfön bei 100°C innerhalb 10 Minuten getrocknet und verfestigt. Die beschichtete Platte wird für 2 Stunden in einem Wasserbad belassen und erneut mit einem Fön getrocknet.3 ml of titanium tetraisopropoxide and 3 ml of concentrated are added to 10 ml of water with stirring Hydrochloric acid. As soon as the solution becomes clear, 3 g of CT 3000 aluminum oxide are added with stirring SG (from ALCOA). The stirring is continued for 2 hours. The resulting paste is mixed with a Squeegee on a glass plate or a steel plate (VA steel) with a thickness of 300 µm applied. The resulting layer is blown with a hot air dryer at 100 ° C within 10 Minutes dried and solidified. The coated plate is in one for 2 hours Leave in a water bath and dry again with a hair dryer.

Claims (5)

1. Verfahren zur Herstellung keramischer Schichten, gekennzeichnet dadurch, daß eine Paste, hergestellt aus Wasser, Mineralsäure, einer hydrolysierbaren Metallverbindung, wie Metallalkoholat oder -chlorid, vorzugsweise Titanalkoholat, und einem pulverförmigen Metalloxid als dünne Schicht auf einen Träger aufgebracht wird und auf dem Träger bei niedriger Temperatur verfestigt wird.1. A method for producing ceramic layers, characterized in that a paste made of water, mineral acid, a hydrolyzable metal compound, such as metal alcoholate or chloride, preferably titanium alcoholate, and a powdery metal oxide is applied as a thin layer on a support and on the support solidified at low temperature. 2. Verfahren zur Herstellung keramischer Schichten, gekennzeichnet dadurch, daß eine Paste, hergestellt aus Wasser, einer im wäßrigen Medium hydrolysierbaren, saures Medium erzeugenden Metallhalogenidverbindung, wie z. B. Titanchlorid, und einem pulverförmigen Metalloxid als dünne Schicht auf einen Träger aufgebracht wird und auf dem Träger bei niedriger Temperatur verfestigt wird.2. Process for the production of ceramic layers, characterized in that a paste, produced from water, an acid medium which is hydrolyzable in the aqueous medium producing metal halide compound, such as. B. titanium chloride, and a powder Metal oxide is applied as a thin layer on a support and on the support low temperature is solidified. 3. Verfahren zur Herstellung keramischer Schichten nach Anspruch 1 oder Anspruch 2, gekennzeichnet dadurch, daß in die Paste andere organische oder anorganische Materialien mit definierten katalytischen, optischen, oder elektrischen Eigenschaften eingemischt werden und damit keramische Schichten mit gezielten Eigenschaften hergestellt werden können.3. A method for producing ceramic layers according to claim 1 or claim 2, characterized in that other organic or inorganic materials with defined catalytic, optical, or electrical properties are mixed in and so that ceramic layers with specific properties can be produced. 4. Verfahren zur Herstellung keramischer Schichten nach Anspruch 1, Anspruch 2 und Anspruch 3, gekennzeichnet dadurch, daß die Schichten als filteraktive Schichten für die Membranfiltration eingesetzt werden.4. A method for producing ceramic layers according to claim 1, claim 2 and claim 3, characterized in that the layers as filter-active layers for the Membrane filtration can be used. 5. Verfahren zur Herstellung keramischer Schichten nach Anspruch 1, Anspruch 2 und Anspruch 4, gekennzeichnet dadurch, daß die Schichten als Sensoren oder als Träger für Sensoren eingesetzt werden.5. A method for producing ceramic layers according to claim 1, claim 2 and claim 4, characterized in that the layers as sensors or as carriers for sensors be used.
DE19944439722 1994-06-23 1994-11-09 Prodn. of strong ceramic titanium di:oxide thin film at low temp. Ceased DE4439722A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
DE19944439722 DE4439722A1 (en) 1994-06-23 1994-11-09 Prodn. of strong ceramic titanium di:oxide thin film at low temp.
US08/737,890 US5885657A (en) 1994-06-23 1995-06-20 Production of ceramic layers and their use
DE59508772T DE59508772D1 (en) 1994-06-23 1995-06-20 PRODUCTION OF CERAMIC LAYERS AND THEIR USE
EP95923174A EP0766657B1 (en) 1994-06-23 1995-06-20 Production of ceramic layers and their use
PCT/DE1995/000819 WO1996000198A1 (en) 1994-06-23 1995-06-20 Production of ceramic layers and their use

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19944421978 DE4421978A1 (en) 1994-06-23 1994-06-23 Economical prodn. of photo:electrochemical elements from cheap materials
DE19944439722 DE4439722A1 (en) 1994-06-23 1994-11-09 Prodn. of strong ceramic titanium di:oxide thin film at low temp.

Publications (1)

Publication Number Publication Date
DE4439722A1 true DE4439722A1 (en) 1996-05-15

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DE19944439722 Ceased DE4439722A1 (en) 1994-06-23 1994-11-09 Prodn. of strong ceramic titanium di:oxide thin film at low temp.

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005063645A1 (en) * 2003-12-19 2005-07-14 Ferro Gmbh Substrates with a transparent, reflecting metal oxide partial coating, production and use thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005063645A1 (en) * 2003-12-19 2005-07-14 Ferro Gmbh Substrates with a transparent, reflecting metal oxide partial coating, production and use thereof

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