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EP1268364A1 - Corps moule fritte avec couche de surface poreuse et son procede de fabrication - Google Patents

Corps moule fritte avec couche de surface poreuse et son procede de fabrication

Info

Publication number
EP1268364A1
EP1268364A1 EP01915331A EP01915331A EP1268364A1 EP 1268364 A1 EP1268364 A1 EP 1268364A1 EP 01915331 A EP01915331 A EP 01915331A EP 01915331 A EP01915331 A EP 01915331A EP 1268364 A1 EP1268364 A1 EP 1268364A1
Authority
EP
European Patent Office
Prior art keywords
layer
shaped body
substrate
sintered
pores
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.)
Ceased
Application number
EP01915331A
Other languages
German (de)
English (en)
Inventor
Dirk Rogowski
Hans-Georg Pfaff
Alwin Nagel
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.)
Ceramtec GmbH
Original Assignee
Ceramtec GmbH
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 Ceramtec GmbH filed Critical Ceramtec GmbH
Publication of EP1268364A1 publication Critical patent/EP1268364A1/fr
Ceased legal-status Critical Current

Links

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
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
    • A61L27/30—Inorganic materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56—Porous materials, e.g. foams or sponges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
    • 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
    • C04B41/4582—Porous coatings, e.g. coating containing porous fillers
    • 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
    • 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
    • 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
    • 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
    • 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
    • C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers
    • 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
    • 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
    • C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
    • 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
    • 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
    • C04B2111/0087—Uses not provided for elsewhere in C04B2111/00 for metallurgical applications
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y10T428/249981—Plural void-containing components
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y10T428/249987—With nonvoid component of specified composition
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y10T428/249987—With nonvoid component of specified composition
    • Y10T428/249988—Of about the same composition as, and adjacent to, the void-containing component
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y10T428/249987—With nonvoid component of specified composition
    • Y10T428/24999—Inorganic
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the invention relates to a molded article according to the preamble of the first claim and to a method for producing a molded article according to the sixteenth claim.
  • Coatings serve to improve mechanical, electrical, chemical, optical or other material properties on the surface of a component in order to achieve application advantages or to prevent or delay negative effects on the component during use.
  • the application of dense layers in the form of glazes to ceramic substrates has been known for a long time.
  • the substrate materials are mostly coarse or refractory ceramics with a correspondingly low level of mechanical properties and structure.
  • the dense coating should essentially cover these disadvantages.
  • the glazes significantly increase chemical resistance, for example.
  • Layers made of various chemical elements and compounds, which are applied to the substrate by means of CVD, PVD, plasma or similar techniques and also combinations thereof, are used and tested in technology.
  • a disadvantage of these application methods is the way via the gas phase, which severely limits the number of materials that can be used for coating.
  • the layer thicknesses that can be achieved are in the range from a few ⁇ m to approximately 25 ⁇ m and, due to the coating process, are very cost-intensive. With the methods mentioned it is only possible to To change surface properties. However, it is not possible to significantly influence the structure of the surfaces.
  • the adhesiveness of the layers depends on the method used. In the case of coatings using the plasma process, the layer adheres only via adhesive forces, which naturally limits long-term adhesion.
  • Ceramic molded parts that consist entirely of an open-pore material are state of the art. However, their mechanical strength is greatly reduced.
  • the invention is therefore based on the object of avoiding the known disadvantages in the production of a porous layer on a sintered body from an inorganic material.
  • the invention avoids the disadvantages of the prior art in the production of a shaped body with a porous layer on its surface in that first a base body, the substrate, is formed as a green body from an inorganic material and a suspension is formed on the substrate in the state of the green body the same inorganic material from which the substrate is made, or a different material is applied. In addition to the inorganic material, this suspension also contains a pore-forming substance. Only after the layer has been applied is there a common heat treatment of substrate and layer by drying and sintering to produce a monolithic shaped body. The method for producing the substrate does not differ from that which is known from the prior art.
  • the base body can either be pore-free, densely sintered, or also contain pores. In the latter case, it also contains a portion of a pore-forming substance in its state as a green body. However, the proportion of this substance is then such that the proportion of pores per unit volume in the layer is always larger than in the substrate.
  • Ceramic materials such as the known oxide ceramics, silicates, phosphates, apatites and related materials as well as nitrides, carbides and silicides are particularly suitable as inorganic materials for the base body, the substrate. It is also possible to produce moldings with a porous surface layer from metals produced by powder metallurgy using the process according to the invention.
  • the same inorganic materials that are suitable for producing the base body, the substrate, are suitable for producing the layer.
  • a porous layer can form on the base body, the substrate, the inorganic material provided for the layer is mixed in a suitable grain size with a suitable liquid and a suitable pore-forming substance to form a suspension and this suspension taking into account the shrinkage during the Heat treatment, drying and sintering, applied in the required layer thickness on the green body.
  • the production of a suspension from an inorganic material in a liquid matched to this material and a substance suitable for the size, shape and number of pores are known from the prior art, for example from DE 44 42 810 A1, DE 44 32 477 C2 or the publication "Influence of Organic Compounds on Ceramic Masses", W. Mann, Ber. DKG, 37 (1960), pp. 11 to 22.
  • Solution process the sublimation process, the evaporation process, the swelling process, the gas blowing process and the foam process.
  • Particularly suitable as pore-forming substances are organic substances, for example starches, cellulose or waxes, and natural and synthetic polymers which evaporate, gasify, consume or burn during the thermal treatment of the substrate and the layer applied to it and thereby form the pores.
  • the number of pores per unit volume, their size, that is to say their diameter, and their shape can advantageously be determined by the selection of a suitable pore-forming substance.
  • the quantity of particles, their size and their shape are the decisive influencing factors.
  • the shape of a solid pore-forming material can, for example, be spherical, globular, platelet-shaped or fibrous.
  • the pore-forming substances are converted into a gas phase during the thermal treatment of the shaped body, which leads to open pores when the gas escapes from the shaped body, that is to say the pores are interconnected.
  • the gases blowing and the foam process there are also processes, for example the gas blowing and the foam process, in which the pores remain closed.
  • the type of pores depends on the intended use of the shaped body. Open pores are always advantageous if liquids or gases are to flow through the molded body and, for example, additional substances are to be stored in the pores.
  • Shaped bodies with closed pores are suitable, for example, for sound and heat insulation and for electrical insulation.
  • the porosity that is to say the proportion of pores per unit volume, can be controlled in the case of solid substances by the amount, in the case of liquid substances optionally by the concentration of the pore-forming substance added, so that the porosity is approximately between 25% and 90%, preferably approximately is between 25% and 70%.
  • the pore size the diameter of the pores, depends in particular on the particle size of the substance forming the pores and can have values of approximately between 1 ⁇ m and 1000 ⁇ m, preferably between 20 ⁇ m and 500 ⁇ m can be set.
  • the prerequisite is that the substances used do not undergo any change in volume during the burning out or gasification.
  • the moisture content of the suspension when the layer is applied to the green body, to the substrate, the moisture content of the suspension can be adapted to the precompression of the material of the substrate.
  • the moisture content of the substrate and suspension must be coordinated with one another in such a way that the shrinkage of the substrate and layer is approximately the same in the subsequent heat treatments, so that cracks, deformations or detachment of the layer do not occur during drying.
  • the layer materials and the pore-forming substances are suspended in water or in another suitable liquid, which is known from the prior art already mentioned, in such a way that the suspension has a consistency suitable for the application process.
  • dispersants can be added to produce a suspension, which advantageously achieve a uniform distribution of the solids within the suspension.
  • the viscosity of the suspension can be influenced by adding organic or inorganic auxiliaries. When strongly wetting liquid is added, the adhesion of the suspension to the substrate can be increased in the green state.
  • the method for applying the layer on the substrate can advantageously be based on the geometry and the surface shape of the substrate and the desired thickness of the Layer to be matched.
  • the layer can be applied to the entire surface of the substrate or only to one or more partial areas.
  • the immersion method is particularly suitable for complicated surface structures and thin layers of approximately 0.02 mm to approximately 2 mm.
  • the dipping process also enables a layer to be built up in several dipping steps in succession up to the desired overall thickness. After each dipping process that builds up a layer of a certain thickness, this layer is first dried to a degree suitable for building up the new layer before the next layer is built up.
  • the suspension can also be spread on flat surfaces and filled with thick layers.
  • Spraying requires a sprayable suspension.
  • Sprayed layers have a rough surface, which can be advantageous for implants or catalysts, for example.
  • the layers can also be easily applied in multiple layers by spraying. With the aid of the methods presented, layers in the range from approximately 0.02 mm to 10 mm, preferably from approximately 0.1 mm to 2 mm, can be applied.
  • the moldings according to the invention can be used, for example, as implants in medical technology.
  • Medical implants for example socket inserts for hip joints, are made from high-purity aluminum oxide ceramics because of their good compatibility and biocompatibility as well as their very good wear behavior.
  • the bone tissue is given the opportunity to grow or ingrowth into the layer and the pan can be anchored directly in the bone.
  • the pan as the base body can also be coated with a layer of hydroxylapatite or other calcium phosphate compounds with the same thickness and with the same pore structure.
  • the hydroxyapatite stimulates bone growth and facilitates the ingrowth of the bone tissue in the pores of the layer of the implant. Hydroxyapatite can also be applied in a thin layer on the porous aluminum oxide layer.
  • a further layer of porous silicon nitride is applied to a silicon nitride substrate, Si 3 N 4 , of a cutting tool, so that a good adherent, active coating with precursors can then take place.
  • the moldings according to the invention are also suitable as catalyst supports.
  • the porous layer on the high-temperature ceramic materials serves as a carrier for the catalyst material.
  • Such catalysts are used, for example, in motor vehicles or in the chemical industry.
  • the moldings according to the invention are suitable for lining containers, pipelines and channels in metallurgy and in the chemical industry.
  • a porous layer of cordierite on dense cordierite or a porous layer of aluminum titanate on dense aluminum titanate is proposed. This increases the surface tension compared to the melt and reduces wetting.
  • the invention is explained using the following exemplary embodiments. Show it:
  • Fig. 3 shows the insert shell of a hip joint endoprosthesis with a layer promoting the ingrowth of the bone tissue
  • Fig. 4 is a sectional view of the porous layer and the adjacent material of the insert shell in an enlarged view.
  • silicon nitride Si 3 N 4
  • FIG. 1 The production of a molded article according to the invention from silicon nitride, Si 3 N 4 , is described below, as is shown in FIG. 1 and is designated by 1.
  • silicon nitride is prepared into a pressable mass by dispersing it in water with the addition of water-soluble binders, grinding and spray drying.
  • the granules obtained by spray drying are pressed into a square plate 1 with an edge length of 17 mm and a height of 7 mm at an axial pressure of 2000 bar.
  • the embodiment is shown in Fig. 1 on an enlarged scale.
  • the density of the green body 2 is 1.9 g / cm 3 , corresponding to 60% of the theoretical density of Si 3 N 4 .
  • a portion of the aqueous Si 3 N 4 dispersion is branched off before spray drying.
  • the solids content is about 60 w% (weight percent).
  • 15% by weight of a starch powder with a grain size between 20 ⁇ m and 50 ⁇ m are added to the dispersion.
  • the viscous dispersion produced in this way is coated as layer 3 on the pressed Si 3 N 4 platelets, the substrate 2.
  • the water portion of the spread dispersion is sucked up by the green body 2 and the applied layer 3 solidifies.
  • the thickness 4 of the layer 3 can be adjusted as desired, for example up to 2 mm, by repeated spreading.
  • Substrate 2 as a green body and layer 3 during application are coordinated with one another in such a way that tensions and cracks are avoided during drying and subsequent firing.
  • the substrates 2 provided with a layer 3, the platelets 1, are dried like conventional moldings made of silicon nitride and sintered at the usual sintering temperature of up to 1800 ° C.
  • Layer 3 sinters monolithically with substrate 2.
  • the burned-out organic components leave open pores 5.
  • FIG. 2 shows a section through the layer 3 on the plate 1 and the area of the substrate 2 located underneath it.
  • the image shows a 200-fold magnification through a light microscope.
  • the thickness of the porous layer 3 arranged on the right is approximately 0.3 mm.
  • Layer 3 clearly shows an approximately uniform distribution of coherent, spherical pores 5 of approximately the same size, which have a diameter 6 of approximately 20 ⁇ m to 30 ⁇ m.
  • the proportion of pores per unit volume, the porosity is approximately 35%.
  • the edge layer 7 of the substrate 2 also has pores 8, which are sometimes larger and irregularly arranged than the pores in the porous layer 3.
  • This effect which is generally referred to as sintered skin in ceramic materials, results from reactions of the surface with the sintering atmosphere.
  • the edge layer 7 in the present exemplary embodiment is formed, for example, when silicon nitride is sintered in the presence of substances which, when decomposed, emit gases containing carbon and oxygen, which react with the nitrogen and the silicon and likewise form gaseous phases, for example SiO and N 2 . This was the case with the sintering of the present exemplary embodiment because the starch powder has decomposed. The gases that have formed have reacted with the material of the surface layer 7 to form pores.
  • the porosity decreases from the surface of the substrate 2 towards the inside.
  • the sinter skin can reach a thickness of up to 3/10 mm. While the so-called sintered skin is usually removed by grinding because its porosity interferes with the otherwise intended purpose of sintered ceramics, it can even be called desirable in the present case because it opens the pores into the base body. In the case of infiltration of these pores, for example, this results in the possibility of firmly anchoring the porous layer to the base body, the substrate 2, via the infiltrated materials.
  • FIG. 3 shows an insert shell 10 of a hip joint endoprosthesis made of aluminum oxide, Al 2 O 3.
  • the insert shell 10 shown schematically consists of the base body 11 with the sliding surface 12 and the surface 13 on which a porous layer 14, also made of aluminum oxide, has been applied is.
  • This porous layer 14 is intended to promote the growth and ingrowth of the bone tissue.
  • the layer 14 has a uniform distribution of open pores 15.
  • Layer 14 is branched off from the material provided for the production of the insert shell. 15% by weight of a polyethylene wax with a grain size between 100 ⁇ m and 500 ⁇ m are added to this dispersion. The viscous dispersion produced in this way is spread onto the outer surface 13 of the base body 11, the procedure being as described in the previous exemplary embodiment.
  • FIG. 4 shows the structure of the porous layer 14 and the adjoining base body 11 after sintering in a light microscope image with a microsection magnified fifty times.
  • the pore-free base body 11 and its outer surface 13 can be clearly seen as the boundary between the base body 11 and the porous coating 14.
  • the sample from an insert shell is embedded in a synthetic resin 16 suitable for the preparation of micrographs.
  • the embedding material 16 appears dark in the micrograph. It has filled the pores 15, which is why they are hardly recognizable, particularly in the transition to the surface 17 of the coating 14.
  • the layer 14 has a thickness 19 of approximately 1.5 mm and one Porosity of about 50%. It consists of the same material as the material of the base body 11, Al 2 O 3 .
  • the rounded pores 15 of up to 400 ⁇ m in diameter form an essentially coherent structure. As can be seen, this results in a very strongly jagged surface, which advantageously supports the growth and ingrowth of the bone tissue.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Dermatology (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Veterinary Medicine (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)
  • Materials For Medical Uses (AREA)

Abstract

Pour les couches poreuses sur des céramiques haute performance, l"invention vise à combiner les propriétés mécaniques et thermiques du matériau du substrat satisfaisant aux sollicitations extrêmes à des propriétés avantageuses de certains matériaux de recouvrement. Dans de nombreuses applications, l"application ultérieure de telles couches sur un substrat déjà fritté ne donne pas de résultat satisfaisant en termes d"épaisseur de couche possible, de porosité et d"adhérence. C"est pourquoi, selon l"invention, la fabrication d"un corps moulé en matériau inorganique fritté avec une couche de surface poreuse comprend les étapes suivantes : le corps de base est d"abord moulé ; sur sa surface ou une partie de sa surface est ensuite appliquée une couche sous forme de suspension, qui contient également un matériau inorganique ; une portion prédéfinie d"un matériau formant des pores est alors mélangée au moins au matériau de cette couche ; enfin, le corps de base et la couche qui lui est appliquée sont soumis ensemble à des traitements thermiques nécessaires à la fabrication d"un corps fritté monolithique.
EP01915331A 2000-03-29 2001-03-14 Corps moule fritte avec couche de surface poreuse et son procede de fabrication Ceased EP1268364A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10015614 2000-03-29
DE10015614A DE10015614B4 (de) 2000-03-29 2000-03-29 Gesinterter Formkörper mit poröser Schicht auf der Oberfläche sowie Verfahren zu seiner Herstellung und seine Verwendungen
PCT/EP2001/002841 WO2001072664A1 (fr) 2000-03-29 2001-03-14 Corps moule fritte avec couche de surface poreuse et son procede de fabrication

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EP1268364A1 true EP1268364A1 (fr) 2003-01-02

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US (1) US7074479B2 (fr)
EP (1) EP1268364A1 (fr)
DE (1) DE10015614B4 (fr)
WO (1) WO2001072664A1 (fr)

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WO2016005236A1 (fr) 2014-07-09 2016-01-14 Ceramtec Gmbh Prothèse de resurfaçage en céramique intégrale, pourvue d'une face interne poreuse
WO2016005235A1 (fr) 2014-07-09 2016-01-14 Ceramtec Gmbh Prothèse totale du genou en céramique intégrale pourvue d'une face arrière orientée vers l'os poreuse
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WO2016005236A1 (fr) 2014-07-09 2016-01-14 Ceramtec Gmbh Prothèse de resurfaçage en céramique intégrale, pourvue d'une face interne poreuse
DE102015212260A1 (de) 2014-07-09 2016-01-14 Ceramtec Gmbh Vollkeramische Oberflächenersatzprothese mit poröser Innenseite
WO2016005235A1 (fr) 2014-07-09 2016-01-14 Ceramtec Gmbh Prothèse totale du genou en céramique intégrale pourvue d'une face arrière orientée vers l'os poreuse
DE102015212258A1 (de) 2014-07-09 2016-01-14 Ceramtec Gmbh Vollkeramischer Kniegelenksersatz mit poröser knochenzugewandter Rückseite
AU2016300118B2 (en) * 2015-07-28 2020-07-30 Ceramtec Gmbh Metallic and/or ceramic components with at least one osseointegrative and osteoinductive surface (multi)layer structure

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WO2001072664A1 (fr) 2001-10-04
US7074479B2 (en) 2006-07-11
DE10015614A1 (de) 2001-10-04
DE10015614B4 (de) 2009-02-19
US20030180518A1 (en) 2003-09-25

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