EP1286644A1 - Produit ceramique pour applications dentaires et son procede de fabrication - Google Patents

Produit ceramique pour applications dentaires et son procede de fabrication

Info

Publication number
EP1286644A1
EP1286644A1 EP01940551A EP01940551A EP1286644A1 EP 1286644 A1 EP1286644 A1 EP 1286644A1 EP 01940551 A EP01940551 A EP 01940551A EP 01940551 A EP01940551 A EP 01940551A EP 1286644 A1 EP1286644 A1 EP 1286644A1
Authority
EP
European Patent Office
Prior art keywords
dental
dental ceramic
bar
sintered body
precipitate
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Withdrawn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
EP01940551A
Other languages
German (de)
English (en)
Inventor
Wolfgang Wiedemann
Original Assignee
Heraeus Kulzer 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 Heraeus Kulzer GmbH filed Critical Heraeus Kulzer GmbH
Publication of EP1286644A1 publication Critical patent/EP1286644A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/15—Compositions characterised by their physical properties
    • A61K6/17—Particle size
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
    • A61K6/838—Phosphorus compounds, e.g. apatite
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/849—Preparations for artificial teeth, for filling teeth or for capping teeth comprising inorganic cements
    • A61K6/864—Phosphate cements

Definitions

  • the present invention relates to a ceramic material for dental applications, in particular for dental fillings and dentures.
  • the invention further relates to a method for producing such a material and the use of a starting material of the manufacturing method for dental applications.
  • US 4,097,935 is known as the closest prior art, in which an essentially pure hydroxyapatite is proposed as dental ceramic.
  • the physical properties of the hydroxyapatite ceramic disclosed there are isotropic and, in particular, are not optically birefringent.
  • This object is achieved by a ceramic having the features of claim 1.
  • the object is also achieved by a method having the features of claim 7.
  • the sintered body is anisotropic, the lattice planes of the crystallites forming the sintered body are aligned with a preferred direction. This results in a reduction in the internal reflections in the sintered body.
  • the sintered body itself becomes translucent to an extent that comes close to natural tooth enamel.
  • the refractive index in the visible light range is anisotropic, in particular if the sintered body has birefringence, the optical properties of the sintered body are in the preferred range. This gives a particularly natural appearance with a difference in the refractive indices ⁇ n> 1 10 "4 , in particular ⁇ n> 2 10 ⁇ 3.
  • the sintered body is preferably also anisotropic with respect to X-ray diffraction, the intensity of reflections being changed as a result of the texture, that is to say of preferred directions in the sintered body , eg air-filled ellipsoidal cavities) in favor of an intrinsic birefringence due to texture effects can be excluded This improves optical properties.
  • the anisotropy is oriented to a given axis, for example the axis of symmetry of a cylindrical ceramic body.
  • the properties of the sintered body are thus also better defined, for example in terms of mechanical machinability.
  • a sintered body in which the content of tricalcium phosphate (TCP) and / or another poorly soluble phosphate is ⁇ 4% is advantageous. This also promotes the low opacity and mouth resistance of the material.
  • the calcium phosphate compound which is precipitated in the process according to the invention is advantageously essentially stoichiometric hydroxylapatite.
  • the green body is preferably pressed at an internal pressure of 200 bar to 10,000 bar, in particular in a range from 800 bar to 1,500 bar. In the latter area, there is a good relationship between the optical properties of the sintered body and the economic feasibility of the production process.
  • the pressing is preferably carried out in the case of a cylindrical green body in an axial direction.
  • the optical properties can be further improved if the pressing is carried out with a press ram in the axial direction, the press ram being rotated about its axis.
  • the object is also achieved by a dental ceramic which is produced by a process according to claims 7-11.
  • a fine crystalline hydroxyapatite as a starting material for dental applications enables the production of dental ceramics which have the desired properties if the individual crystallites are rod-shaped and have a length of 10 nm to 1,000 nm and a thickness between 5 nm and 500 nm.
  • Tab. 1 the half widths of the lines of a calcium phosphate precipitated according to Example 1 in the X-ray diffraction diagram;
  • Fig. 1 the precipitation product acc. Example 1 in about 30,000 times magnification
  • Fig. 2 the precipitate according to Example 2 in about 30,000 times magnification; such as
  • Fig. 3 the precipitate according to Example 3 in about 30,000 times magnification.
  • the reaction takes place in an external reaction vessel with a volume of approx. 5 ml with a throughput of approx. 200 ml / s and a stirring speed of 400 / s with high shear forces at constant temperature.
  • the Ca solution is added dropwise at a rate of 0.33 ml / s.
  • the phosphate solution is introduced into the external reaction vessel at a rate of 0.77 ml / s.
  • the precipitate is at room temperature for 18 h on the mother liquor and is then bidistilled with aqua. washed from room temperature to a nitrate content in the wash water ⁇ 5ppm. After filtration and drying at 210 ° C., a yield of 14.12 g of precipitate is obtained.
  • the precipitation is a calcium phosphate with the lattice structure of apatite.
  • the precipitation consists of very loosely lying needle-like particles of approx. 150 nm length and 50 nm thickness, as can be seen in Fig. 1.
  • the precipitate is crushed to particles ⁇ 250 ⁇ m in an agate mortar, axially pressed at 2400 bar and then sintered with the following temperature profile: room temperature to 400 ° C: 13 ° C / min; stationary 400 ° C: 60 min; 400 ° C to 850 ° C: 10 ° C / min; stationary 850 ° C: 120 min; 850 ° C to 1195 ° C: 3 ° C / min; stationary 1195 ° C: 60 min; Cooling to room temperature: approx. 1.5 ° C / min.
  • Sintering gives us a translucent body with a density of 3.15 g / cm 3 .
  • the X-ray diffraction pattern shows the sintered body as pure hydroxyapatite. The anisotropy can also be seen in the X-ray diffractogram.
  • the intensities of the reflexes are given in Table 2.
  • the relative intensity gives the measured intensity of the respective line as a percentage of the intensity of the (211) reflex.
  • the column “isotropic” shows the relative intensities of the reflections for pulverized samples according to the JCPDS.
  • the column “Location” gives the approximate orientation of the corresponding network plane relative to the c-axis.
  • the reaction takes place in an external reaction vessel with a volume of approx. 5 ml with a throughput of approx. 78 ml / s and a stirring speed of 160 / s at constant temperature for a period of 16 min.
  • the Ca solution is added dropwise at a rate of approx. 0.32 ml / s.
  • the phosphate solution is introduced into the external reaction vessel at a rate of 0.63 ml / s.
  • the precipitate is at room temperature for 18 h and is then bidistilled with aqua. washed from room temperature to a nitrate content in the wash water ⁇ 5ppm. After filtration and drying at 210 ° C., a yield of 13.25 g of precipitate is obtained.
  • the fairly loose precipitation consists of crystal needles that are approx. 250 nm long and 50 nm thick, see Fig. 2.
  • the precipitate is crushed to particles ⁇ 250 ⁇ m in an agate mortar, axially pressed at 800 bar and then sintered with the following temperature profile: room temperature to 400 ° C: 13 ° C / min; stationary 400 ° C: 60 min; 400 ° C to 850 ° C: 10 ° C / min; stationary 850 ° C: 120 min; 850 ° C to 1195 ° C: 3 ° C / min; stationary 1195 ° C: 60 min; Cooling to room temperature: approx. 1.5 ° C / min.
  • the result of the sintering is a translucent body with a density of 3.14 g / cm 3.
  • the X-ray diffraction diagram shows the sintered body as pure hydroxyapatite. The anisotropy can also be seen in the X-ray diffractogram.
  • the intensities of the reflections are given in Table 3.
  • the relative intensity gives the measured intensity of the respective line as a percentage of the intensity of the (211) reflex.
  • In the column “isotropic” are the relative intensities of the reflexes for pulverized samples according to the JCPDS specified.
  • the "Location” column indicates the approximate orientation of the corresponding network plane
  • the reaction takes place in an external reaction vessel with a volume of approx. 5 ml with a throughput of approx. 78 ml / s and a stirring speed of 160 / s at constant temperature.
  • the Ca solution is added dropwise at a rate of approx. 0.33 ml / s.
  • the phosphate solution is introduced into the external reaction vessel at a rate of 0.83 ml / s.
  • the precipitate is at 60 ° C. for 18 h (with stirring at 100 min -1 ) on the mother liquor and is then bidistilled with aqua. washed from room temperature to a nitrate content in the wash water ⁇ 20 ppm. After filtration and drying at 210 ° C, a yield of about 14 g of precipitate is obtained.
  • the precipitation consists of elongated, blunt crystallites whose length varies between 150 nm and 400 nm and whose thickness varies between 50 nm and 120 nm, see Fig. 3.
  • the precipitate is crushed to particles ⁇ 250 ⁇ m in an agate mortar, axially pressed at 800 bar and then sintered with the following temperature profile: Room temperature to 400 ° C: 13 ° C / min; stationary 400 ° C: 60 min; 400 ° C to 850 ° C: 10 ° C / min; stationary 850 ° C: 120 min; 850 ° C to 1195 ° C: 3 ° C / min; stationary 1195 ° C: 60 min; Cooling to room temperature: approx. 1.5 ° C / min.
  • the result of the sintering is a translucent body with a density of 3.14 g / cm.
  • X-ray diffraction diagram shows the sintered body as pure hydroxyapatite.
  • Fig. 1 shows a scanning electron microscope image of the calcium phosphate precipitated according to the procedure of Example 1 in a magnification of 30,000 times.
  • the individual particles appear here as elongated crystallites with dimensions of approx. 150 nm by 50 nm.
  • the X-ray diffraction diagram shows the acicular character of the precipitated crystallites more clearly.
  • Table 1 shows the full width at half maximum of the lines of precipitation of the calcium phosphate precipitated according to Example 1.
  • the line width of the (002) reflex whose network planes are perpendicular to the c-axis, is smaller by a factor of 2 compared to the (200) - Reflex, whose network planes are parallel to the c-axis, emphasizes the needle-like shape of the crystallites.
  • a denture made from this after sintering is visually similar to nature and mouth-resistant. In terms of demineralization and remineralization, it behaves somewhat like natural tooth enamel.

Landscapes

  • Health & Medical Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Plastic & Reconstructive Surgery (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Dental Preparations (AREA)
  • Materials For Medical Uses (AREA)

Abstract

L'invention concerne une céramique dentaire renfermant un corps fritté comprenant une fraction supérieure à 90 % en poids d'hydroxylapatite (HA; Ca5(PO4)3OH). Tout en offrant des possibilités de préparation simples et tout en étant d'une bonne résistance, la céramique selon l'invention permet d'obtenir des propriétés optiques analogues à celles d'un produit naturel grâce au fait que le corps fritté est anisotrope.
EP01940551A 2000-06-08 2001-06-06 Produit ceramique pour applications dentaires et son procede de fabrication Withdrawn EP1286644A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10027946A DE10027946A1 (de) 2000-06-08 2000-06-08 Keramisches Material für Dentalanwendungen sowie Verfahren zu dessen Herstellung und Verwendung eines Ausgangsstoffs des Herstellungsverfahrens für Dentalanwendungen
DE10027946 2000-06-08
PCT/EP2001/006401 WO2001093808A1 (fr) 2000-06-08 2001-06-06 Produit ceramique pour applications dentaires et son procede de fabrication

Publications (1)

Publication Number Publication Date
EP1286644A1 true EP1286644A1 (fr) 2003-03-05

Family

ID=7644842

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01940551A Withdrawn EP1286644A1 (fr) 2000-06-08 2001-06-06 Produit ceramique pour applications dentaires et son procede de fabrication

Country Status (15)

Country Link
US (1) US20030183963A1 (fr)
EP (1) EP1286644A1 (fr)
JP (1) JP2003535114A (fr)
CN (1) CN1433294A (fr)
AU (1) AU2001274087A1 (fr)
BR (1) BR0111442A (fr)
CA (1) CA2410448A1 (fr)
DE (1) DE10027946A1 (fr)
EE (1) EE200200679A (fr)
IL (1) IL152749A0 (fr)
MX (1) MXPA02011703A (fr)
NO (1) NO20025347L (fr)
RU (1) RU2002134904A (fr)
WO (1) WO2001093808A1 (fr)
ZA (1) ZA200209915B (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003000588A1 (fr) 2001-06-22 2003-01-03 Basf Aktiengesellschaft Cristaux d'apatite en forme de baguette a rapport longueur sur largeur determine
US20120064343A1 (en) * 2009-03-19 2012-03-15 Sofsera Corporation Tooth surface repairing material
CN110141523A (zh) * 2019-03-26 2019-08-20 合肥卓越义齿制作有限公司 一种制备义齿用热稳定性能优异的包埋粉
CN113297598B (zh) * 2021-06-11 2024-05-28 上海寻梦信息技术有限公司 快递柜服务端埋点方法、装置、设备及存储介质

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1522182A (en) * 1974-08-02 1978-08-23 Sterling Drug Inc Ceramic material
US4097935A (en) * 1976-07-21 1978-07-04 Sterling Drug Inc. Hydroxylapatite ceramic
US5034352A (en) * 1985-06-25 1991-07-23 Lifecore Biomedical, Inc. Calcium phosphate materials
US5032552A (en) * 1988-07-04 1991-07-16 Tdk Corporation Biomedical material
JPH085712B2 (ja) * 1988-09-15 1996-01-24 旭光学工業株式会社 配向性リン酸カルシウム系化合物成形体及び焼結体並びにそれらの製造方法
DE3935060C2 (de) * 1989-10-20 1996-05-30 Herbst Bremer Goldschlaegerei Verfahren zur Herstellung eines keramischen Materials für den Dentalbereich und eine Verwendung desselben
DE4302072A1 (de) * 1993-01-26 1994-07-28 Herbst Bremer Goldschlaegerei Keramisches Material für Zahnfüllungen und/oder Zahnersatz und Verfahren zur Herstellung desselben
WO1996029144A1 (fr) * 1995-03-20 1996-09-26 The Penn State Research Foundation Agglomerat particulaire sec formant de l'hydroxyapatite et procedes afferents
DE19725555A1 (de) * 1997-06-12 1998-12-24 Ivoclar Ag Transluzente Apatit-Glaskeramik
DE19725553A1 (de) * 1997-06-12 1998-12-24 Ivoclar Ag Chemisch stabile transluzente Apatit-Glaskeramik

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0193808A1 *

Also Published As

Publication number Publication date
CN1433294A (zh) 2003-07-30
DE10027946A1 (de) 2001-12-13
RU2002134904A (ru) 2004-06-27
NO20025347D0 (no) 2002-11-07
MXPA02011703A (es) 2003-03-27
NO20025347L (no) 2002-11-07
CA2410448A1 (fr) 2002-11-26
WO2001093808A1 (fr) 2001-12-13
AU2001274087A1 (en) 2001-12-17
JP2003535114A (ja) 2003-11-25
BR0111442A (pt) 2003-06-03
US20030183963A1 (en) 2003-10-02
EE200200679A (et) 2004-06-15
ZA200209915B (en) 2003-08-25
IL152749A0 (en) 2003-06-24

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