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EP1594596A1 - Composite ceramique multicouche - Google Patents

Composite ceramique multicouche

Info

Publication number
EP1594596A1
EP1594596A1 EP03815521A EP03815521A EP1594596A1 EP 1594596 A1 EP1594596 A1 EP 1594596A1 EP 03815521 A EP03815521 A EP 03815521A EP 03815521 A EP03815521 A EP 03815521A EP 1594596 A1 EP1594596 A1 EP 1594596A1
Authority
EP
European Patent Office
Prior art keywords
layer
substrate
layers
ceramic composite
sintered
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Withdrawn
Application number
EP03815521A
Other languages
German (de)
English (en)
Inventor
Frank Ehlen
Olaf Binkle
Ralph Nonninger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Itn Nanovation AG
Original Assignee
Itn Nanovation 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 Itn Nanovation AG filed Critical Itn Nanovation AG
Publication of EP1594596A1 publication Critical patent/EP1594596A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • B01D67/00411—Inorganic membrane manufacture by agglomeration of particles in the dry state by sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • B01D67/00413—Inorganic membrane manufacture by agglomeration of particles in the dry state by agglomeration of nanoparticles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10—Supported membranes; Membrane supports
    • B01D69/108—Inorganic support material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/0215—Silicon carbide; Silicon nitride; Silicon oxycarbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/024—Oxides
    • B01D71/0271—Perovskites
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/024—Multiple impregnation or coating
    • B01J37/0244—Coatings comprising several layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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    • 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
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    • 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
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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    • 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
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    • 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
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/04—Characteristic thickness
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
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Definitions

  • Ceramic membranes usually consist of a multi-layer system made of porous ceramic, the individual layers of which have different pore sizes.
  • the actual filtering layer (functional layer) is usually the thinnest and most porous of the system. This is located on a substrate of the system that has a coarser porous structure. At the same time, the substrate takes on the mechanical support function of the overall system and often also forms filtrate collection structures.
  • the multilayer filter is produced by first molding, drying and sintering the substrate, then applying the functional layer and sintering it onto the substrate.
  • a layer that contains ceramic particles but is not yet sintered is called a green layer, a body made of this material corresponding to green bodies.
  • the sintering of a ceramic composite is a manufacturing process in the course of which a green body is transformed into a porous binder-free solid or into a more or less one highly compacted binder-free solids are transferred with a corresponding increase in mechanical strength, or the compression of an already sintered body.
  • the starting body during sintering can be seen as a dense packing of spherical particles, which are slightly connected at contact points, ie they touch each other with adhesion in so-called "necks".
  • the spaces between the particles form the pores of the starting body.
  • the original pores are complex structures of different geometries.
  • the sintering process takes place in two stages at elevated temperature. In the first stage, the overall porosity is essentially retained.
  • the centers of the particles remain approximately the same distance apart. Nevertheless, a gain in surface energy is achieved because the shape of the cavities, ie the pores, from the complicated structures of the initial state to the simple spherical shape. Thus, the lowest surface is achieved for a given porosity.
  • the particles touch in the "necks", which become thicker in the first stage of sintering due to mass transport , The pores round off, whereby the smallest pore surface is achieved. This mass transfer is also called grain boundary diffusion.
  • the pores are then gradually closed. The material is compacted by removing empty spaces to the inner and outer surface (volume diffusion). Due to the compression of the sintered body, the overall porosity is reduced. The pores are filled via grain boundary diffusion and volume diffusion. In this step, the centers of the original powder particles move together. This causes the sintered body to compact or shrink.
  • the extent of a grain boundary diffusion can be determined via the capillary pressure that arises in the pores.
  • the shape of the pores is changed by mass transfer, which is initiated by different radii of curvature becomes.
  • the substance is transported from the "bellies" of the particles to the "necks" of the particles.
  • the atoms are more firmly bound on an inwardly curved surface (concave) than on an outwardly curved surface (convex).
  • the capillary pressure which initiates the sintering of the ceramic green body, depends not only on the temperature and the type of particle, but also on the size of the particles used, since the convex radius of curvature increases with decreasing particle size.
  • the temperature at which the sintering of a ceramic green body begins (assuming the same packing density in the green body) thus decreases with decreasing particle size of the starting particles.
  • the object of the present invention is therefore to provide a method with which a defect-free ceramic layer can be applied to a sintered ceramic substrate.
  • this object is achieved by a method for producing a multilayer porous ceramic composite by sintering, in which one or more layers are applied to the surface of a sintered substrate, at least one layer containing nanoscale particles with a particle size of x ⁇ 100 nm, the roughness depth the surface of the substrate is smaller than the layer thickness s of the nanoscale particles applied to the surface of the substrate and the layer thickness s of the applied nanoscale particles after a sintering process with the substrate at temperatures between 500 ° C. and 1300 ° C. a layer thickness of s ⁇ 2 , 5 ⁇ m.
  • the minimum thickness of the functional layer is determined by the roughness depth of the sintered substrate. The roughness depth must not exceed the layer thickness of the functional layer.
  • the ceramic materials used are preferably derived from metal (mixed) oxides and carbides, nitrides, borides, silicides and carbonitrides from metals and non-metals. Examples of this are A1 2 0 3 , partially and fully stabilized Zr0 2 , mullite, cordierite, perovskite, spinels, for example BaTi0 3 , PZT, PLZT, and SiC, Si 3 N 4 , B 4 C, BN, MoSi 2 , TiB 2 , TiN, TiC and Ti (C, N). It goes without saying that this list is not exhaustive. Mixtures of oxides or non-oxides and mixtures of oxides and non-oxides can of course also be used.
  • two layers are applied to the sintered substrate, at least one of the layers containing the nanoscale particles.
  • the filter property of the porous ceramic composite can be influenced in a targeted manner by means of several layers of different porosity. Particularly good filtration results can be achieved if one of the layers is defect-free.
  • more than two layers are applied to the sintered substrate, at least two layers comprising the nanoscale particles. This measure allows a multilayer porous ceramic composite to be built up which has good filter properties.
  • nanoscale particles have a particle size of x ⁇ 20 nm, preferably x ⁇ 10 nm, grain boundary sliding can be triggered with a low activation energy. This enables the use of low sintering temperatures at sintering voltages of around 200MPa.
  • nanoscale particles are applied to the sintered substrate by spraying, dipping, flooding or film casting. If the nanoscale particles are contained in a suspension, they can be applied to the sintered substrate in a particularly simple manner by the process steps mentioned. In particular, these measures enable the layer thickness of the green layer that is applied to the sintered substrate, and thus the sintered functional layer, to be controlled and adjusted particularly well.
  • an intermediate layer in particular an organic intermediate layer
  • An organic binder can compensate for unevenness in the surface of the sintered substrate and / or the organic binder prevents the infiltration of the nanoparticles forming the functional layer into the surface of the coarse-porous substrate.
  • the organic binder can block and / or smear the pores on the surface of the substrate, so that penetration of the nanoparticles forming the functional layer into the surface of the substrate is prevented.
  • the substrate can be processed into a suitable carrier structure using an organic binder.
  • the organic intermediate layer evaporates during the sintering process, so that the filter properties of the finished ceramic composite are not influenced by the organic binder.
  • the object is also achieved by a multilayer porous ceramic composite which has a sintered substrate and a defect-free functional layer sintered from nanoscale particles, which has a layer thickness s ⁇ 2.5 ⁇ m.
  • a porous ceramic composite has a particularly high-quality filter layer, since it is defect-free.
  • the ceramic composite has three layers, one layer having the nanoscale particles.
  • the material properties of the layers can be coordinated with one another in such a way that at least one filter layer is defect-free and a high-quality filter is produced.
  • the ceramic composite has more than three layers, at least two layers having nanoscale particles. This measure allows the filter effect to be gradually increased within the ceramic composite, at least two layers being provided which are particularly fine-pored and free of defects.
  • multilayer conductor track structures can be constructed in which the defect-free layer made of nanoscale particles is an insulator. As a result, conductor tracks can be arranged electrically insulated at a short distance from one another.
  • a green layer is applied to an already sintered ceramic substrate and is coated with the already sintered substrate. strat sintered at temperatures between 500 ° C and 1300 ° C, the green layer having only ceramic particles with a particle size x 100 nm and the sintered green layer having a layer thickness s ⁇ 2.5 microns.
  • the layer produced in this process is defect-free and fine-pored and is therefore particularly well suited for filtration processes and can be used as a catalyst.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Filtering Materials (AREA)

Abstract

L'invention concerne un procédé de production d'un composite céramique poreux, selon lequel, une couche verte est appliquée sur un substrat de céramique déjà fritté, puis frittée avec ledit substrat déjà fritté à une température comprise entre 500 DEG C et 1300 DEG C, la couche verte comprenant exclusivement des particules de céramique d'une taille x </= 100 nm et la couche verte frittée présentant, en tant que couche fonctionnelle, une épaisseur s </= 2,5 mu m. La couche fonctionnelle obtenue selon ce procédé est exempte de défauts, présente des pores fins et convient donc particulièrement bien pour des processus de filtration.
EP03815521A 2003-01-30 2003-11-19 Composite ceramique multicouche Withdrawn EP1594596A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10303897 2003-01-30
DE10303897A DE10303897A1 (de) 2003-01-30 2003-01-30 Mehrlagiger Keramikverbund
PCT/DE2003/003833 WO2004067154A1 (fr) 2003-01-30 2003-11-19 Composite ceramique multicouche

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EP1594596A1 true EP1594596A1 (fr) 2005-11-16

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EP03815521A Withdrawn EP1594596A1 (fr) 2003-01-30 2003-11-19 Composite ceramique multicouche

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US (1) US20060231988A1 (fr)
EP (1) EP1594596A1 (fr)
CN (1) CN100337728C (fr)
AU (1) AU2003300488A1 (fr)
DE (1) DE10303897A1 (fr)
WO (1) WO2004067154A1 (fr)

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CN101215190B (zh) * 2007-12-29 2010-10-06 中国科学院广州能源研究所 表面具有透明热反射涂层的陶瓷制品及其制备方法
US7892435B2 (en) * 2008-05-21 2011-02-22 Honeywell International Inc. System and method for recycling using nanoceramics
CN101429052B (zh) * 2008-12-05 2012-09-12 株洲阳光电瓷有限责任公司 一种电瓷产品外观的修补方法
US8461462B2 (en) 2009-09-28 2013-06-11 Kyocera Corporation Circuit substrate, laminated board and laminated sheet
JP2012152727A (ja) * 2011-01-28 2012-08-16 Tokyo Electron Ltd 濾過用フィルタ及び濾過用フィルタの製造方法
US20130043067A1 (en) * 2011-08-17 2013-02-21 Kyocera Corporation Wire Substrate Structure
CN105637987A (zh) * 2013-10-29 2016-06-01 京瓷株式会社 布线基板、使用了该布线基板的安装结构体以及层叠片
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Also Published As

Publication number Publication date
US20060231988A1 (en) 2006-10-19
CN100337728C (zh) 2007-09-19
DE10303897A1 (de) 2004-08-12
AU2003300488A1 (en) 2004-08-23
CN1744941A (zh) 2006-03-08
WO2004067154A1 (fr) 2004-08-12

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