EP1286644A1 - Keramisches material für dentalanwendungen sowie verfahren zu dessen herstellung - Google Patents
Keramisches material für dentalanwendungen sowie verfahren zu dessen herstellungInfo
- 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- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 229910010293 ceramic material Inorganic materials 0.000 title description 4
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 19
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 18
- 239000011351 dental ceramic Substances 0.000 claims abstract description 14
- 239000000919 ceramic Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000011575 calcium Substances 0.000 claims description 13
- 239000001506 calcium phosphate Substances 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 11
- 238000002441 X-ray diffraction Methods 0.000 claims description 10
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 9
- 235000011010 calcium phosphates Nutrition 0.000 claims description 8
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 235000019731 tricalcium phosphate Nutrition 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 4
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 4
- -1 Calcium phosphate compound Chemical class 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 5
- 239000005445 natural material Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 12
- 230000011514 reflex Effects 0.000 description 9
- 210000003298 dental enamel Anatomy 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 2
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 208000014151 Stomatognathic disease Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- XAAHAAMILDNBPS-UHFFFAOYSA-L calcium hydrogenphosphate dihydrate Chemical compound O.O.[Ca+2].OP([O-])([O-])=O XAAHAAMILDNBPS-UHFFFAOYSA-L 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005115 demineralization Methods 0.000 description 1
- 230000002328 demineralizing effect Effects 0.000 description 1
- 239000001177 diphosphate Substances 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 239000012154 double-distilled water Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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)
- Life Sciences & Earth Sciences (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Inorganic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Dental Preparations (AREA)
- Materials For Medical Uses (AREA)
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 (de) | 2000-06-08 | 2001-06-06 | Keramisches material für dentalanwendungen sowie verfahren zu dessen herstellung |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1286644A1 true EP1286644A1 (de) | 2003-03-05 |
Family
ID=7644842
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01940551A Withdrawn EP1286644A1 (de) | 2000-06-08 | 2001-06-06 | Keramisches material für dentalanwendungen sowie verfahren zu dessen herstellung |
Country Status (15)
Country | Link |
---|---|
US (1) | US20030183963A1 (no) |
EP (1) | EP1286644A1 (no) |
JP (1) | JP2003535114A (no) |
CN (1) | CN1433294A (no) |
AU (1) | AU2001274087A1 (no) |
BR (1) | BR0111442A (no) |
CA (1) | CA2410448A1 (no) |
DE (1) | DE10027946A1 (no) |
EE (1) | EE200200679A (no) |
IL (1) | IL152749A0 (no) |
MX (1) | MXPA02011703A (no) |
NO (1) | NO20025347D0 (no) |
RU (1) | RU2002134904A (no) |
WO (1) | WO2001093808A1 (no) |
ZA (1) | ZA200209915B (no) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004538228A (ja) | 2001-06-22 | 2004-12-24 | ビーエーエスエフ アクチェンゲゼルシャフト | 特定の長さ幅比を有する棒状アパタイト結晶 |
WO2010106668A1 (ja) * | 2009-03-19 | 2010-09-23 | サウスコーストデンタル株式会社 | 歯面修復材 |
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)
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 |
AU5320496A (en) * | 1995-03-20 | 1996-10-08 | Penn State Research Foundation, The | Hydroxyapatite forming dry particulate agglomerate and methods therefor |
DE19725553A1 (de) * | 1997-06-12 | 1998-12-24 | Ivoclar Ag | Chemisch stabile transluzente Apatit-Glaskeramik |
DE19725555A1 (de) * | 1997-06-12 | 1998-12-24 | Ivoclar Ag | Transluzente Apatit-Glaskeramik |
-
2000
- 2000-06-08 DE DE10027946A patent/DE10027946A1/de not_active Withdrawn
-
2001
- 2001-06-06 RU RU2002134904/15A patent/RU2002134904A/ru not_active Application Discontinuation
- 2001-06-06 IL IL15274901A patent/IL152749A0/xx unknown
- 2001-06-06 CN CN01810712A patent/CN1433294A/zh active Pending
- 2001-06-06 CA CA002410448A patent/CA2410448A1/en not_active Abandoned
- 2001-06-06 AU AU2001274087A patent/AU2001274087A1/en not_active Abandoned
- 2001-06-06 EP EP01940551A patent/EP1286644A1/de not_active Withdrawn
- 2001-06-06 EE EEP200200679A patent/EE200200679A/xx unknown
- 2001-06-06 US US10/297,419 patent/US20030183963A1/en not_active Abandoned
- 2001-06-06 BR BR0111442-5A patent/BR0111442A/pt not_active Application Discontinuation
- 2001-06-06 JP JP2002501382A patent/JP2003535114A/ja not_active Withdrawn
- 2001-06-06 MX MXPA02011703A patent/MXPA02011703A/es unknown
- 2001-06-06 WO PCT/EP2001/006401 patent/WO2001093808A1/de active Application Filing
-
2002
- 2002-11-07 NO NO20025347A patent/NO20025347D0/no not_active Application Discontinuation
- 2002-12-06 ZA ZA200209915A patent/ZA200209915B/xx unknown
Non-Patent Citations (1)
Title |
---|
See references of WO0193808A1 * |
Also Published As
Publication number | Publication date |
---|---|
DE10027946A1 (de) | 2001-12-13 |
MXPA02011703A (es) | 2003-03-27 |
US20030183963A1 (en) | 2003-10-02 |
AU2001274087A1 (en) | 2001-12-17 |
CA2410448A1 (en) | 2002-11-26 |
CN1433294A (zh) | 2003-07-30 |
IL152749A0 (en) | 2003-06-24 |
NO20025347L (no) | 2002-11-07 |
BR0111442A (pt) | 2003-06-03 |
JP2003535114A (ja) | 2003-11-25 |
NO20025347D0 (no) | 2002-11-07 |
RU2002134904A (ru) | 2004-06-27 |
WO2001093808A1 (de) | 2001-12-13 |
EE200200679A (et) | 2004-06-15 |
ZA200209915B (en) | 2003-08-25 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 20021122 |
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