WO2010015414A1 - Method for producing a ceramic component - Google Patents

Method for producing a ceramic component Download PDF

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Publication number
WO2010015414A1
WO2010015414A1 PCT/EP2009/005746 EP2009005746W WO2010015414A1 WO 2010015414 A1 WO2010015414 A1 WO 2010015414A1 EP 2009005746 W EP2009005746 W EP 2009005746W WO 2010015414 A1 WO2010015414 A1 WO 2010015414A1
Authority
WO
WIPO (PCT)
Prior art keywords
ceramic component
ceramic
temperature
component
sintering
Prior art date
Application number
PCT/EP2009/005746
Other languages
German (de)
French (fr)
Inventor
Helmut D. Link
Original Assignee
Deru 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
Priority claimed from PCT/EP2008/006524 external-priority patent/WO2009036845A2/en
Application filed by Deru Gmbh filed Critical Deru Gmbh
Priority to JP2011521487A priority Critical patent/JP5535212B2/en
Priority to ES09804525T priority patent/ES2570975T3/en
Priority to CN2009801294353A priority patent/CN102137827B/en
Priority to US13/057,913 priority patent/US20110127700A1/en
Priority to EP09804525.5A priority patent/EP2331483B1/en
Publication of WO2010015414A1 publication Critical patent/WO2010015414A1/en

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
    • A61F2/02—Prostheses implantable into the body
    • A61F2/30—Joints
    • A61F2/30767—Special external or bone-contacting surface, e.g. coating for improving bone ingrowth
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    • A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
    • A61F2/02—Prostheses implantable into the body
    • A61F2/30—Joints
    • A61F2/44—Joints for the spine, e.g. vertebrae, spinal discs
    • A61F2/442—Intervertebral or spinal discs, e.g. resilient
    • A61F2/4425—Intervertebral or spinal discs, e.g. resilient made of articulated components
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/486—Fine ceramics
    • 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
    • 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
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
    • 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
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    • A61F2002/30004—Material related properties of the prosthesis or of a coating on the prosthesis the prosthesis being made from materials having different values of a given property at different locations within the same prosthesis
    • A61F2002/30011—Material related properties of the prosthesis or of a coating on the prosthesis the prosthesis being made from materials having different values of a given property at different locations within the same prosthesis differing in porosity
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    • A61F2002/30001—Additional features of subject-matter classified in A61F2/28, A61F2/30 and subgroups thereof
    • A61F2002/30316—The prosthesis having different structural features at different locations within the same prosthesis; Connections between prosthetic parts; Special structural features of bone or joint prostheses not otherwise provided for
    • A61F2002/30317—The prosthesis having different structural features at different locations within the same prosthesis
    • A61F2002/30321—The prosthesis having different structural features at different locations within the same prosthesis differing in roughness
    • A—HUMAN NECESSITIES
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    • A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
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    • A61F2002/30317—The prosthesis having different structural features at different locations within the same prosthesis
    • A61F2002/30322—The prosthesis having different structural features at different locations within the same prosthesis differing in surface structures
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F2310/00—Prostheses classified in A61F2/28 or A61F2/30 - A61F2/44 being constructed from or coated with a particular material
    • A61F2310/00389—The prosthesis being coated or covered with a particular material
    • A61F2310/00395—Coating or prosthesis-covering structure made of metals or of alloys
    • A61F2310/00407—Coating made of titanium or of Ti-based alloys
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/612—Machining
    • 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
    • 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
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/963—Surface properties, e.g. surface roughness

Definitions

  • the invention relates to a method for producing a ceramic component.
  • a ceramic starting material is provided in powder form and introduced into a form predetermining the shape of the ceramic component.
  • the ceramic component is pre-sintered, released from the mold, and then sintered at a temperature higher than the pre-sintering temperature.
  • Such a method for producing a ceramic component is known, for example, from EP 0 421 085. It turns out that ceramic components produced in this way have a low surface roughness and that it is therefore difficult to firmly adhere a coating to the ceramic component.
  • the invention is based on the object to present a method for producing a ceramic component, in which a ceramic component produced according to the invention provides a better starting base for applying a coating. Based on the above-mentioned prior art, the object is achieved by the features of the independent claims. Advantageous embodiments can be found in the subclaims.
  • a temperature between 880 0 C and 980 0 C is selected for the step of presintering. After presintering and before sintering, the surface of the ceramic component is treated with a blasting material.
  • a powder-shaped ceramic starting material is filled into a mold which predetermines the shape of the ceramic component. Since the volume of the ceramic component is reduced by subsequent processing steps, the shape is larger than the finished ceramic component. A stable internal structure of the ceramic component is achieved by subsequent sintering. The sintering creates solid bonds between the particles of the powder.
  • the sintering is carried out in several steps.
  • a first step the ceramic component is pre-sintered at a lower temperature, so that only narrow bridges between the grains of the powder are formed.
  • the stability of the narrow bridges should be just such that the treatment of the surface with a blasting material leads to an increased surface roughness. If the stability of the bridges is too low, the ceramic component can break into several components, if the stability of the bridges is too high, the treatment with the abrasive material is insufficient to change the surface structure of the ceramic component.
  • the desired change in the surface structure by the blasting material occurs when a temperature between 880 0 C and 980 0 C is selected for pre-sintering.
  • the inner structure of the ceramic component is then just such that fragments of the desired size can be broken out of the component with the blasting material.
  • the strength of the bond between the particles of the powder material increases when the temperature of the Pre-sintering is increased. Good results were achieved with the inventive method, if the presintering temperature was greater than 900 0 C and 95O 0 C. was less than
  • the surface roughness R a should be greater than 2.5 ⁇ m (WO 2009/036845).
  • the roughness data in the context of the invention relate to the mean roughness R a according to DIN EN ISO 4288 and 3274 and to the finished ceramic component after sintering.
  • the surface roughness achieved with the method according to the invention depends on the parameters selected during the treatment with the blasting material, such as, for example, the particle size of the blasting material and the speed at which the particles impinge on the ceramic component. Preferably, these parameters are adjusted in the inventive method so that the surface roughness R a of the finished ceramic component is greater than 2.5 microns.
  • the surface roughness R 3 of the finished ceramic component should not be greater than 7 ⁇ m.
  • the entire surface of the ceramic component can be treated with the blasting material. This is useful if the entire surface of the ceramic component is to be provided with a coating. Often, however, only part of the surface should be coated, while another part of the surface should be free from coatings. This applies, for example, to endoprothesis components whose surface is intended to form part of a connection with bone material, while another part serves as a sliding surface for interaction with another prosthesis. thesenkomponente is determined. For the sliding surface increased surface roughness is not desired. In the method according to the invention, it can therefore be provided that only a part of the surface of the ceramic component is treated with the blasting material, while another part of the surface remains recessed from the treatment with the blasting material. If, in the context of the invention, a treatment of the surface of the ceramic component is used, then the entire surface or a part of the surface may be meant.
  • the particle size of the blasting material is preferably of the same order of magnitude as the particle size of the ceramic starting material.
  • the blasting material can then act particularly effective on the ceramic component.
  • the particles then constitute impurities in the ceramic material. Impurities of this type can be prevented by using as blasting material a powder which corresponds to the powder of the ceramic starting material. If particles of this material become stuck in the ceramic component, they do not change the homogeneous composition of the ceramic material.
  • the applied to the surface of the ceramic component coating may consist of a titanium alloy or pure titanium.
  • Plasma spraying is a process by which a gas is passed through an arc and thereby ionized.
  • the coating material is introduced in powder form in the ionized gas and transported by the gas flow to the workpiece to be coated.
  • FIG. 2 shows an enlarged detail of the intervertebral disc prosthesis according to FIG. 1;
  • FIG. Fig. 3 is a schematic representation of the internal structure of the ceramic material in the initial state;
  • FIG. 4 shows the view from FIG. 3 after pre-sintering
  • Fig. 5 is the view of Fig. 3 after sintering.
  • Fig. 1 is designed as a disc prosthesis
  • the intervertebral disc prosthesis comprises a first connecting plate 1 and a second connecting plate 2.
  • the first connecting plate 1 is an endoprosthesis component designed for connection to a first vertebral body 6;
  • the second connecting plate 2 is an endoprosthesis component designed for connection to a second vertebral body 7.
  • the first connection plate 1 and the second connection plate 2 abut each other via matching sliding surfaces 3.
  • the sliding surfaces 3 form a joint for movements between the upper terminal plate 1 and the lower terminal plate 2.
  • projections 12 are formed in regions 13 of the surfaces of the connection plates 1, 2, with which the connection plates 1, 2 bear against the bone material of the vertebral bodies 6, 7, projections 12 are formed.
  • the projections 12 have a flatter edge in the direction in which the connection plates 1, 2 are inserted into the intervertebral space, and a steeper flank in the opposite direction. Due to the flatter edge, the insertion of the connection plates 1, 2 is facilitated in the intervertebral space.
  • the steeper flank offers the connection plates 1, 2 stop when the projections 12 have penetrated into the bone material of the vertebral bodies 6, 7.
  • the steeper flanks prevent the connection plates 1, 2 from being pulled out of the intervertebral space in the opposite direction.
  • connection plates 1, 2 are intended to abut against the ventral side of the vertebral bodies 6, 7.
  • connection plates 1, 2 in the dorsal direction can not be inserted beyond the desired position in the Eisenwirbelhoffm.
  • the terminal plate 1 and the terminal plate 2 are formed of a ceramic material 9.
  • the sliding surfaces 3 on the connection plates 1, 2 are formed on a surface of the ceramic material 9.
  • the regions 13, via which a connection to the bone material is produced, are covered with a coating 10 made of a titanium alloy.
  • Fig. 2 shows an enlarged section of a connection plate 1, 2, in which the interface 8 between the Ceramic material 9 and the coating 10 is shown.
  • the ceramic material 9 has at the interface 8 to the coating 10 a roughness R a , which is at least 2, 5 microns. This roughness at the interface 8 is sufficient to establish a stable bond with the coating 10, but is not sufficient for a stable bond with bone material.
  • the coating 10 has a greater roughness and greater porosity than the ceramic material 9 and therefore forms a stable connection with the bone material.
  • a starting material in powder form is first introduced into a mold whose shape corresponds to the ceramic component to be produced. Since the ceramic component loses volume through the subsequent process steps, the mold has larger dimensions than the finished ceramic component.
  • the powder is mechanically compressed, for example by shaking and pressure, the particles 14 of the powder are then adjacent to each other, as shown schematically in Fig. 3. By presintering at a temperature of 920 ° C., bridges shown in FIG. 4 form between the particles 14. The internal structure of the material is now so stable that the ceramic component can be removed from the mold.
  • the ceramic material has a greater stability in its structure than would be chosen for mechanical machining by drilling or milling.
  • the stability of the structure is just adjusted so that by irradiating with a powder containing the starting material corresponds, fragments can be removed from the pre-sintered ceramic material. The fragments are so large that forms the desired surface roughness after sintering in the finished ceramic component.
  • the ceramic component is sintered at a temperature higher than the pre-sintering temperature. At the interfaces of the previously only connected via the bridges 15 particles form planar connections 16. Since the cavities disappear from the interior, the volume of the ceramic component continues to decrease. On the part of the surface which has been treated with the blasting material, the surface now has a roughness R a of approximately 4 ⁇ m. A coating of a titanium alloy applied to this surface portion adheres firmly to the surface.

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  • Orthopedic Medicine & Surgery (AREA)
  • Transplantation (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Heart & Thoracic Surgery (AREA)
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  • Public Health (AREA)
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Abstract

The invention relates to a method for producing a ceramic component. With the method, a ceramic base material in powdered form and a mold having the shape of the ceramic component are provided. The ceramic base material is introduced into the mold. The ceramic component is presintered at a temperature between 880°C and 980°C and is then removed from the mold. The surface of the ceramic component is treated with a blasting material and the ceramic component is sintered at a temperature that is higher than the presintering temperature. With the method according to the invention, ceramic components having higher surface roughness can be produced. Due to the higher surface roughness it is easier to apply a firmly adhering coating to the ceramic component.

Description

Verfahren zum Herstellen eines Keramikbauteils Method for producing a ceramic component
Die Erfindung betrifft ein Verfahren zum Herstellen eines Keramikbauteils. Bei dem Verfahren wird ein Keramikausgangsmaterial in Pulverform bereitgestellt und in eine die Gestalt des Keramikbauteils vorgebenden Form eingebracht. Das Keramikbauteil wird vorgesintert, aus der Form herausgelöst und anschließend bei einer Temperatur gesintert, die höher ist als die Temperatur des Vorsinterns.The invention relates to a method for producing a ceramic component. In the method, a ceramic starting material is provided in powder form and introduced into a form predetermining the shape of the ceramic component. The ceramic component is pre-sintered, released from the mold, and then sintered at a temperature higher than the pre-sintering temperature.
Ein solches Verfahren zum Herstellen eines Keramikbauteils ist beispielsweise aus EP 0 421 085 bekannt. Es zeigt sich, dass auf diese Weise hergestellte Keramikbauteile eine ge- ringe Oberflächenrauigkeit haben und dass es deswegen schwierig ist, eine Beschichtung festhaftend auf das Keramikbauteil aufzubringen.Such a method for producing a ceramic component is known, for example, from EP 0 421 085. It turns out that ceramic components produced in this way have a low surface roughness and that it is therefore difficult to firmly adhere a coating to the ceramic component.
Der Erfindung liegt die Aufgabe zu Grunde, ein Verfahren zum Herstellen eines Keramikbauteils vorzustellen, bei dem ein erfindungsgemäß hergestelltes Keramikbauteil eine bessere Ausgangsbasis zum Aufbringen einer Beschichtung bietet. Ausgehend vom eingangs genannten Stand der Technik wird die Aufgabe gelöst durch die Merkmale der unabhängigen Ansprüche. Vorteilhafte Ausführungsformen finden sich in den Unteransprüchen. Erfindungsgemäß wird für den Schritt des Vorsinterns eine Temperatur zwischen 8800C und 9800C gewählt. Nach dem Vorsintern und vor dem Sintern wird die Oberfläche des Keramikbauteils mit einem Strahlgut behan- delt. Zur Herstellung von Keramikbauteilen wird zunächst ein pul- verförmiges Keramikausgangsmaterial in eine Form gefüllt, die die Gestalt des Keramikbauteils vorgibt. Da sich das Volumen des Keramikbauteils durch nachfolgende Bearbeitungsschritte verringert, ist die Form größer als das fertige Keramikbauteil. Eine stabile innere Struktur des Keramikbauteils wird durch nachfolgendes Sintern erreicht. Durch das Sintern entstehen feste Verbindungen zwischen den Partikeln des Pulvers .The invention is based on the object to present a method for producing a ceramic component, in which a ceramic component produced according to the invention provides a better starting base for applying a coating. Based on the above-mentioned prior art, the object is achieved by the features of the independent claims. Advantageous embodiments can be found in the subclaims. According to the invention, a temperature between 880 0 C and 980 0 C is selected for the step of presintering. After presintering and before sintering, the surface of the ceramic component is treated with a blasting material. For the production of ceramic components, first a powder-shaped ceramic starting material is filled into a mold which predetermines the shape of the ceramic component. Since the volume of the ceramic component is reduced by subsequent processing steps, the shape is larger than the finished ceramic component. A stable internal structure of the ceramic component is achieved by subsequent sintering. The sintering creates solid bonds between the particles of the powder.
Das Sintern wird in mehreren Schritten durchgeführt. In einem ersten Schritt wird das Keramikbauteil bei einer niedrigeren Temperatur vorgesintert, so dass sich lediglich schmale Brücken zwischen den Körnern des Pulvers herausbilden. Für das erfindungsgemäße Verfahren soll die Stabilität der schmalen Brücken gerade derart sein, dass die Behandlung der Oberfläche mit einem Strahlgut zu einer erhöhten Oberflächenrauigkeit führt. Ist die Stabilität der Brücken zu gering, kann das Keramikbauteil in mehrere Bestandteile zerbersten, ist die Stabilität der Brücken zu hoch, reicht die Behandlung mit dem Strahlgut nicht aus, um die Oberflächenstruktur des Keramikbauteils zu verändern. Versuche haben gezeigt, dass die gewünschte Veränderung der Oberflä- chenstruktur durch das Strahlgut dann eintritt, wenn für das Vorsintern eine Temperatur zwischen 8800C und 9800C gewählt wird. Die innere Struktur des Keramikbauteils ist dann gerade derart, dass mit dem Strahlgut Bruchstücke der gewünschten Größe aus dem Bauteil herausgebrochen werden können .The sintering is carried out in several steps. In a first step, the ceramic component is pre-sintered at a lower temperature, so that only narrow bridges between the grains of the powder are formed. For the inventive method, the stability of the narrow bridges should be just such that the treatment of the surface with a blasting material leads to an increased surface roughness. If the stability of the bridges is too low, the ceramic component can break into several components, if the stability of the bridges is too high, the treatment with the abrasive material is insufficient to change the surface structure of the ceramic component. Experiments have shown that the desired change in the surface structure by the blasting material occurs when a temperature between 880 0 C and 980 0 C is selected for pre-sintering. The inner structure of the ceramic component is then just such that fragments of the desired size can be broken out of the component with the blasting material.
Allgemein steigt die Festigkeit der Verbindung zwischen den Partikeln des Pulvermaterials an, wenn die Temperatur des Vorsinterns erhöht wird. Gute Ergebnisse mit dem erfindungsgemäßen Verfahren wurden erzielt, wenn die Temperatur des Vorsinterns größer war als 9000C bzw. kleiner war als 95O0C.In general, the strength of the bond between the particles of the powder material increases when the temperature of the Pre-sintering is increased. Good results were achieved with the inventive method, if the presintering temperature was greater than 900 0 C and 95O 0 C. was less than
Um das Keramikbauteil mit einer Titanlegierung beschichten zu können, sollte die Oberflächenrauigkeit Ra größer sein als 2,5 μm (WO 2009/036845) . Die Rauigkeitsangaben im Rahmen der Erfindung beziehen sich auf die mittlere Rauigkeit Ra gemäß DIN EN ISO 4288 und 3274 und auf das fertige Keramikbauteil nach dem Sintern. Die mit dem erfindungsgemäßen Verfahren erzielte Oberflächenrauigkeit hängt von den bei der Behandlung mit dem Strahlgut gewählten Parametern ab, wie beispielsweise Partikelgröße des Strahlguts und Ge- schwindigkeit, mit der die Partikel auf das Keramikbauteil auftreffen. Vorzugsweise werden diese Parameter bei dem erfindungsgemäßen Verfahren so eingestellt, dass die Oberflächenrauigkeit Ra des fertigen Keramikbauteils größer ist als 2,5 μm. Damit die Beschichtung in einem Arbeitsgang de- ckend aufgetragen werden kann, sollte die Oberflächenrauigkeit R3 des fertigen Keramikbauteils nicht größer sein als 7 μm.In order to be able to coat the ceramic component with a titanium alloy, the surface roughness R a should be greater than 2.5 μm (WO 2009/036845). The roughness data in the context of the invention relate to the mean roughness R a according to DIN EN ISO 4288 and 3274 and to the finished ceramic component after sintering. The surface roughness achieved with the method according to the invention depends on the parameters selected during the treatment with the blasting material, such as, for example, the particle size of the blasting material and the speed at which the particles impinge on the ceramic component. Preferably, these parameters are adjusted in the inventive method so that the surface roughness R a of the finished ceramic component is greater than 2.5 microns. In order to be able to apply the coating in one operation, the surface roughness R 3 of the finished ceramic component should not be greater than 7 μm.
Im Rahmen der Erfindung kann die gesamte Oberfläche des Ke- ramikbauteils mit dem Strahlgut behandelt werden. Dies ist dann sinnvoll, wenn die gesamte Oberfläche des Keramikbauteils mit einer Beschichtung versehen werden soll. Häufig soll aber nur ein Teil der Oberfläche beschichtet werden, während ein anderer Teil der Oberfläche frei von Beschich- tungen sein soll. Dies gilt beispielsweise für Endoprothe- senkomponenten, deren Oberfläche zum Teil eine Verbindung mit Knochenmaterial eingehen soll, während ein anderer Teil als Gleitfläche zum Zusammenwirken mit einer anderen Pro- thesenkomponente bestimmt ist. Für die Gleitfläche ist eine erhöhte Oberflächenrauigkeit nicht gewünscht. Bei dem erfindungsgemäßen Verfahren kann deswegen vorgesehen sein, dass nur ein Teil der Oberfläche des Keramikbauteils mit dem Strahlgut behandelt wird, während ein anderer Teil der Oberfläche von der Behandlung mit dem Strahlgut ausgespart bleibt. Wird im Rahmen der Erfindung von einer Behandlung der Oberfläche des Keramikbauteils gesprochen, so kann damit die gesamte Oberfläche oder ein Teil der Oberfläche ge- meint sein.In the context of the invention, the entire surface of the ceramic component can be treated with the blasting material. This is useful if the entire surface of the ceramic component is to be provided with a coating. Often, however, only part of the surface should be coated, while another part of the surface should be free from coatings. This applies, for example, to endoprothesis components whose surface is intended to form part of a connection with bone material, while another part serves as a sliding surface for interaction with another prosthesis. thesenkomponente is determined. For the sliding surface increased surface roughness is not desired. In the method according to the invention, it can therefore be provided that only a part of the surface of the ceramic component is treated with the blasting material, while another part of the surface remains recessed from the treatment with the blasting material. If, in the context of the invention, a treatment of the surface of the ceramic component is used, then the entire surface or a part of the surface may be meant.
Die Teilchengröße des Strahlguts liegt vorzugsweise in derselben Größenordnung wie die Teilchengröße des Keramikausgangsmaterials . Das Strahlgut kann dann besonders wirksam auf das Keramikbauteil einwirken. Allerdings besteht bei der Verwendung eines solchen Strahlguts die Gefahr, dass sich Partikel des Strahlguts in den Lücken des Keramikmate- rials festsetzen, die durch die herausgeschlagenen Bruchstücke entstehen. Die Partikel stellen dann Verunrei- nigungen im Keramikmaterial dar. Verunreinigungen dieser Art können verhindert werden, indem als Strahlgut ein Pulver verwendet wird, das dem Pulver des Keramikausgangsmaterials entspricht. Setzen sich Partikel dieses Materials in dem Keramikbauteil fest, so ändern sie nichts an der homo- genen Zusammensetzung des Keramikmaterials.The particle size of the blasting material is preferably of the same order of magnitude as the particle size of the ceramic starting material. The blasting material can then act particularly effective on the ceramic component. However, when using such a blasting material, there is the danger that particles of the blasting material settle in the gaps of the ceramic material which are produced by the broken-out fragments. The particles then constitute impurities in the ceramic material. Impurities of this type can be prevented by using as blasting material a powder which corresponds to the powder of the ceramic starting material. If particles of this material become stuck in the ceramic component, they do not change the homogeneous composition of the ceramic material.
Die auf die Oberfläche des Keramikbauteils aufzubringende Beschichtung kann aus einer Titan-Legierung oder reinem Titan bestehen. Als Verfahren zum Aufbringen der Beschichtung kommt Plasmaspritzen in Frage. Das Plasmaspritzen ist ein Verfahren, bei dem ein Gas durch einen Lichtbogen geleitet und dadurch ionisiert wird. Das Beschichtungsmaterial wird in Pulverform in das ionisierte Gas eingebracht und von dem Gasstrom auf das zu beschichtende Werkstück transportiert.The applied to the surface of the ceramic component coating may consist of a titanium alloy or pure titanium. As a method for applying the coating plasma spraying comes into question. Plasma spraying is a process by which a gas is passed through an arc and thereby ionized. The coating material is introduced in powder form in the ionized gas and transported by the gas flow to the workpiece to be coated.
Als geeignete Keramikwerkstoffe für das erfindungsgemäße Verfahren haben sich Zirkoniumoxid, Aluminiumoxid sowie Mischungen aus beiden erwiesen.Zirconium oxide, aluminum oxide and mixtures of both have proved suitable ceramic materials for the process according to the invention.
Die Erfindung wird nachfolgend unter Bezugnahme auf die beigefügten Zeichnung anhand einer vorteilhaften Ausfüh- rungsform beispielhaft beschrieben. Es zeigen:The invention will be described below by way of example with reference to the accompanying drawings with reference to an advantageous embodiment. Show it:
Fig. 1 eine Bandscheibenprothese in Schnittdarstellung;1 shows a disc prosthesis in section;
Fig. 2 einen vergrößerten Ausschnitt aus der Bandscheibenprothese gemäß Fig. 1; Fig. 3 eine schematische Darstellung der inneren Struktur des Keramikmaterials im Ausgangszustand;FIG. 2 shows an enlarged detail of the intervertebral disc prosthesis according to FIG. 1; FIG. Fig. 3 is a schematic representation of the internal structure of the ceramic material in the initial state;
Fig. 4 die Ansicht aus Fig. 3 nach dem Vorsintern; undFIG. 4 shows the view from FIG. 3 after pre-sintering; FIG. and
Fig. 5 die Ansicht aus Fig. 3 nach dem Sintern.Fig. 5 is the view of Fig. 3 after sintering.
In Fig. 1 ist eine als Bandscheibenprothese ausgebildeteIn Fig. 1 is designed as a disc prosthesis
Endoprothese in einen Zwischenwirbelraum zwischen zwei Wirbelkörpern 6, 7 eingesetzt. Die Bandscheibenprothese um- fasst eine erste Anschlussplatte 1 und eine zweite Anschlussplatte 2. Die erste Anschlussplatte 1 ist eine zur Verbindung mit einem ersten Wirbelkörper 6 ausgebildete En- doprothesenkomponente, die zweite Anschlussplatte 2 ist eine zur Verbindung mit einem zweiten Wirbelkörper 7 ausgebildete Endoprothesenkomponente.Endoprosthesis inserted into an intervertebral space between two vertebral bodies 6, 7. The intervertebral disc prosthesis comprises a first connecting plate 1 and a second connecting plate 2. The first connecting plate 1 is an endoprosthesis component designed for connection to a first vertebral body 6; the second connecting plate 2 is an endoprosthesis component designed for connection to a second vertebral body 7.
Die erste Anschlussplatte 1 und die zweite Anschlussplatte 2 liegen über zueinander passende Gleitflächen 3 aneinander an. Die Gleitflächen 3 bilden ein Gelenk für Bewegungen zwischen der oberen Anschlussplatte 1 und der unteren Anschlussplatte 2.The first connection plate 1 and the second connection plate 2 abut each other via matching sliding surfaces 3. The sliding surfaces 3 form a joint for movements between the upper terminal plate 1 and the lower terminal plate 2.
In Bereichen 13 der Oberflächen der Anschlussplatten 1, 2, mit denen die Anschlussplatten 1, 2 an dem Knochenmaterial der Wirbelkörper 6, 7 anliegen, sind Vorsprünge 12 ausgebildet. Die Vorsprünge 12 haben eine flachere Flanke in der Richtung, in der die Anschlussplatten 1, 2 in den Zwischenwirbelraum eingeschoben werden, und eine steilere Flanke in entgegengesetzter Richtung. Durch die flachere Flanke wird das Einschieben der Anschlussplatten 1, 2 in den Zwischenwirbelraum erleichtert. Die steilere Flanke bietet den Anschlussplatten 1, 2 Halt, wenn die Vorsprünge 12 in das Knochenmaterial der Wirbelkörper 6, 7 eingedrungen sind. Die steileren Flanken verhindern, dass die Anschlussplatten 1, 2 in entgegengesetzter Richtung wieder aus dem Zwischenwirbelräum herausgezogen werden können.In regions 13 of the surfaces of the connection plates 1, 2, with which the connection plates 1, 2 bear against the bone material of the vertebral bodies 6, 7, projections 12 are formed. The projections 12 have a flatter edge in the direction in which the connection plates 1, 2 are inserted into the intervertebral space, and a steeper flank in the opposite direction. Due to the flatter edge, the insertion of the connection plates 1, 2 is facilitated in the intervertebral space. The steeper flank offers the connection plates 1, 2 stop when the projections 12 have penetrated into the bone material of the vertebral bodies 6, 7. The steeper flanks prevent the connection plates 1, 2 from being pulled out of the intervertebral space in the opposite direction.
Flansche 4, 5 der Anschlussplatten 1, 2 sind dazu bestimmt, an der ventralen Seite der Wirbelkörper 6, 7 anzuliegen.Flanges 4, 5 of the connection plates 1, 2 are intended to abut against the ventral side of the vertebral bodies 6, 7.
Wegen der Flansche 4, 5 können die Anschlussplatten 1 , 2 in dorsaler Richtung nicht über die gewünschte Position hinaus in den Zwischenwirbelräum eingeschoben werden.Because of the flanges 4, 5, the connection plates 1, 2 in the dorsal direction can not be inserted beyond the desired position in the Zwischenwirbelräum.
Die Anschlussplatte 1 und die Anschlussplatte 2 sind aus einem Keramikwerkstoff 9 geformt. Die Gleitflächen 3 an den Anschlussplatten 1, 2 sind an einer Oberfläche des Keramikwerkstoffs 9 ausgebildet. Die Bereiche 13, über die eine Verbindung zu dem Knochenmaterial hergestellt wird, sind mit einer Beschichtung 10 aus einer Titan-Legierung belegt.The terminal plate 1 and the terminal plate 2 are formed of a ceramic material 9. The sliding surfaces 3 on the connection plates 1, 2 are formed on a surface of the ceramic material 9. The regions 13, via which a connection to the bone material is produced, are covered with a coating 10 made of a titanium alloy.
Fig. 2 zeigt einen vergrößerten Ausschnitt aus einer Anschlussplatte 1, 2, in dem die Grenzfläche 8 zwischen dem Keramikwerkstoff 9 und der Beschichtung 10 gezeigt ist. Der Keramikwerkstoff 9 hat an der Grenzfläche 8 zur Beschichtung 10 eine Rauigkeit Ra, die mindestens 2 , 5 μm beträgt. Diese Rauigkeit an der Grenzfläche 8 reicht aus, um eine stabile Verbindung mit der Beschichtung 10 einzugehen, für eine stabile Verbindung mit Knochenmaterial reicht sie nicht aus. Die Beschichtung 10 hat eine größere Rauigkeit und größere Porosität als der Keramikwerkstoff 9 und geht deswegen eine stabile Verbindung mit dem Knochenmaterial ein.Fig. 2 shows an enlarged section of a connection plate 1, 2, in which the interface 8 between the Ceramic material 9 and the coating 10 is shown. The ceramic material 9 has at the interface 8 to the coating 10 a roughness R a , which is at least 2, 5 microns. This roughness at the interface 8 is sufficient to establish a stable bond with the coating 10, but is not sufficient for a stable bond with bone material. The coating 10 has a greater roughness and greater porosity than the ceramic material 9 and therefore forms a stable connection with the bone material.
Um ein Keramikbauteil in der Gestalt einer Endoprothesen- komponente herzustellen, bei dem ein Teil der Oberfläche die gewünschte Rauigkeit hat, wird zunächst ein in Pulver- form vorliegendes Ausgangsmaterial in eine Form eingebracht, deren Gestalt dem zu erzeugenden Keramikbauteil entspricht. Da das Keramikbauteil durch die nachfolgenden Verfahrensschritte an Volumen verliert, hat die Form größerer Abmessungen als das fertige Keramikbauteil. In der Form wird das Pulver mechanisch verdichtet, beispielsweise durch Schütteln und Druck, die Partikel 14 des Pulvers liegen dann nebeneinander, wie es in Fig. 3 schematisch dargestellt ist. Durch das Vorsintern bei einer Temperatur von 9200C bilden sich in Fig. 4 dargestellte Brücken zwischen den Partikeln 14. Die innere Struktur des Materials ist nun so stabil, dass das Keramikbauteil aus der Form herausgenommen werden kann .In order to produce a ceramic component in the form of an endoprosthesis component in which part of the surface has the desired roughness, a starting material in powder form is first introduced into a mold whose shape corresponds to the ceramic component to be produced. Since the ceramic component loses volume through the subsequent process steps, the mold has larger dimensions than the finished ceramic component. In the mold, the powder is mechanically compressed, for example by shaking and pressure, the particles 14 of the powder are then adjacent to each other, as shown schematically in Fig. 3. By presintering at a temperature of 920 ° C., bridges shown in FIG. 4 form between the particles 14. The internal structure of the material is now so stable that the ceramic component can be removed from the mold.
Mit den Brücken 15 hat das Keramikmaterial eine größere Stabilität in seiner Struktur, als man sie für eine mechanische Bearbeitung durch Bohren oder Fräsen wählen würde. Die Stabilität der Struktur ist gerade so eingestellt, dass durch Bestrahlen mit einem Pulver, das dem Ausgangsmaterial entspricht, Bruchstücke aus dem vorgesinterten Keramikmate- rial herausgelöst werden können. Die Bruchstücke sind so groß, dass sich nach dem Sintern bei dem fertigen Keramikbauteil die gewünschte Oberflächenrauigkeit ausbildet.With the bridges 15, the ceramic material has a greater stability in its structure than would be chosen for mechanical machining by drilling or milling. The stability of the structure is just adjusted so that by irradiating with a powder containing the starting material corresponds, fragments can be removed from the pre-sintered ceramic material. The fragments are so large that forms the desired surface roughness after sintering in the finished ceramic component.
Ist die gewünschte Oberflächenstruktur erreicht und die mechanische Bearbeitung abgeschlossen, wird das Keramikbauteil bei einer Temperatur gesintert, die höher liegt als die Temperatur des Vorsinterns. An den Grenzflächen der bislang nur über die Brücken 15 verbundenen Partikel bilden sich flächige Verbindungen 16. Da die Hohlräume aus dem Inneren verschwinden, nimmt das Volumen des Keramikbauteils weiter ab. Auf dem Teil der Oberfläche, der mit dem Strahlgut behandelt wurde, hat die Oberfläche nun eine Rauigkeit Ra von ungefähr 4 μm. Eine auf diesen Oberflächenanteil aufgebrachte Beschichtung aus einer Titan-Legierung haftet fest auf der Oberfläche. When the desired surface structure has been achieved and the machining is completed, the ceramic component is sintered at a temperature higher than the pre-sintering temperature. At the interfaces of the previously only connected via the bridges 15 particles form planar connections 16. Since the cavities disappear from the interior, the volume of the ceramic component continues to decrease. On the part of the surface which has been treated with the blasting material, the surface now has a roughness R a of approximately 4 μm. A coating of a titanium alloy applied to this surface portion adheres firmly to the surface.

Claims

Patentansprüche claims
1. Verfahren zum Herstellen eines Keramikbauteils mit folgenden Schritten: a. Bereitstellen eines Keramikausgangsmaterials in Pulverform; b. Bereitstellen einer die Gestalt des Keramikbauteils vorgebenden Form; c. Einbringen des Keramikausgangsmaterials in die1. A method of manufacturing a ceramic component, comprising the steps of: a. Providing a ceramic starting material in powder form; b. Providing a shape which predetermines the shape of the ceramic component; c. Introducing the ceramic starting material in the
Form; d. Vorsintern des Keramikbauteils bei einer Temperatur zwischen 8800C und 9800C; e. Herauslösen des Keramikbauteils aus der Form; f. Behandeln der Oberfläche des Keramikbauteils mit einem Strahlgut; g. Sintern des Keramikbauteils bei einer Temperatur, die höher ist als die Temperatur des Vor- sinterns ;Shape; d. Pre-sintering of the ceramic component at a temperature between 880 0 C and 980 0 C; e. Removing the ceramic component from the mold; f. Treating the surface of the ceramic component with a blasting material; G. Sintering the ceramic member at a temperature higher than the pre-sintering temperature;
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Temperatur des Vorsinterns größer ist als 9000C.2. The method according to claim 1, characterized in that the temperature of Vorsinterns is greater than 900 0 C.
3. Verfahren nach Anspruch 1 oder 2 , dadurch gekennzeichnet, dass die Temperatur des Vorsinterns kleiner ist als 95O0C.3. The method according to claim 1 or 2, characterized in that the temperature of Vorsinterns is less than 95O 0 C.
4. Verfahren nach einem der Ansprüche 1 bis 3 , dadurch gekennzeichnet, dass die Rauigkeit Ra des Keramikbauteils auf einem Oberflächenanteil größer ist als 2,5 μm. 4. The method according to any one of claims 1 to 3, characterized in that the roughness R a of the ceramic component is greater than 2.5 microns on a surface portion.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass ein Strahlgut verwendet wird, dessen Partikelgröße der Partikelgröße des Keramikausgangsmaterials entspricht.5. The method according to any one of claims 1 to 4, characterized in that a blasting material is used whose particle size corresponds to the particle size of the ceramic starting material.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass ein dem Keramikausgangsmaterial entsprechendes Material als Strahlgut verwendet wird.6. The method according to any one of claims 1 to 5, characterized in that a material corresponding to the ceramic starting material is used as the blasting material.
7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass eine Beschichtung aus einer Titan-Legierung auf die Oberfläche des Keramikbauteils aufgebracht wird.7. The method according to any one of claims 1 to 6, characterized in that a coating of a titanium alloy is applied to the surface of the ceramic component.
8. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass die gesamte Oberfläche des Keramikbauteils mit dem Strahlgut behandelt wird.8. The method according to any one of claims 1 to 7, characterized in that the entire surface of the ceramic component is treated with the blasting material.
9. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass ein Teil der Oberfläche des Keramikbauteils von der Behandlung mit dem Strahlgut ausgespart bleibt. 9. The method according to any one of claims 1 to 7, characterized in that a part of the surface of the ceramic component is left blank from the treatment with the blasting material.
PCT/EP2009/005746 2008-08-07 2009-08-07 Method for producing a ceramic component WO2010015414A1 (en)

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ES09804525T ES2570975T3 (en) 2008-08-07 2009-08-07 Procedure to produce a ceramic component
CN2009801294353A CN102137827B (en) 2008-08-07 2009-08-07 Method for producing a ceramic component
US13/057,913 US20110127700A1 (en) 2008-08-07 2009-08-07 Method for producing a ceramic component
EP09804525.5A EP2331483B1 (en) 2008-08-07 2009-08-07 Method for producing a ceramic component

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