JP5535212B2 - Manufacturing method of ceramic member - Google Patents
Manufacturing method of ceramic member Download PDFInfo
- Publication number
- JP5535212B2 JP5535212B2 JP2011521487A JP2011521487A JP5535212B2 JP 5535212 B2 JP5535212 B2 JP 5535212B2 JP 2011521487 A JP2011521487 A JP 2011521487A JP 2011521487 A JP2011521487 A JP 2011521487A JP 5535212 B2 JP5535212 B2 JP 5535212B2
- Authority
- JP
- Japan
- Prior art keywords
- ceramic member
- ceramic
- sintering
- temperature
- starting material
- 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.)
- Expired - Fee Related
Links
- 239000000919 ceramic Substances 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000463 material Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 239000007858 starting material Substances 0.000 claims description 11
- 238000005422 blasting Methods 0.000 claims description 6
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- 230000003746 surface roughness Effects 0.000 description 9
- 210000000988 bone and bone Anatomy 0.000 description 6
- 230000007423 decrease Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
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- 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
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- 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
- A61F2310/00005—The prosthesis being constructed from a particular material
- A61F2310/00179—Ceramics or ceramic-like structures
- A61F2310/00185—Ceramics or ceramic-like structures based on metal oxides
- A61F2310/00239—Ceramics or ceramic-like structures based on metal oxides containing zirconia or zirconium oxide ZrO2
-
- 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
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Description
本発明は、セラミック部材の製造方法に関する。その方法では、粉末状のセラミック出発材料を利用可能にし、セラミック部材の形状を予め規定するモールドに導入する。セラミック部材を、予備焼結させ、モールドから取り出し、次に、予備焼結の温度よりも高い温度で焼結させる。 The present invention relates to a method for manufacturing a ceramic member. In that method, a powdered ceramic starting material is made available and the shape of the ceramic member is introduced into a pre-defined mold. The ceramic member is pre-sintered and removed from the mold and then sintered at a temperature higher than the pre-sintering temperature.
セラミック部材のそのような製造方法は、例えば欧州特許第0421085号により知られている。このようにして製造されたセラミック部材は、低い表面粗さを有し、それゆえ、セラミック部材にコーティングをしっかりと適用することは難しいことが分かっている。 Such a method for producing a ceramic member is known, for example, from EP 0421085. Ceramic members produced in this way have a low surface roughness and it has therefore proved difficult to apply a coating firmly to the ceramic member.
本発明の目的は、セラミック部材の製造方法を提供することであり、その方法において、本発明に基づいて製造されたセラミック部材は、コーティングの適用にとってより良い出発基盤を提供する。先に記載の先行技術から進めて、その目的は、独立請求項の特徴によって達成される。有利な実施形態は、従属請求項に明記されている。本発明に基づいて、予備焼結工程のために、880℃〜980℃の間の温度を選択する。予備焼結後かつ焼結前に、セラミック部材の表面をブラスト材料で処理する。 The object of the present invention is to provide a method of manufacturing a ceramic member, in which the ceramic member manufactured according to the present invention provides a better starting basis for coating applications. Proceeding from the prior art described above, the object is achieved by the features of the independent claims. Advantageous embodiments are specified in the dependent claims. Based on the present invention, a temperature between 880 ° C. and 980 ° C. is selected for the pre-sintering step. After the pre-sintering and before sintering, the surface of the ceramic member is treated with a blast material.
セラミック部材を製造するために、まず、粉末状のセラミック出発材料を、セラミック部材の形状を予め規定するモールドに導入する。セラミック部材の体積は、その後に続く加工工程の結果として減少するため、モールドは完成したセラミック部材よりも大きい。セラミック部材の安定な内部構造は、その後に続く焼結によって達成される。焼結は、粉末の粒子同士の確固とした接続をもたらす。 In order to produce a ceramic member, first a powdery ceramic starting material is introduced into a mold that predefines the shape of the ceramic member. Because the volume of the ceramic member decreases as a result of subsequent processing steps, the mold is larger than the finished ceramic member. A stable internal structure of the ceramic member is achieved by subsequent sintering. Sintering provides a firm connection between the powder particles.
焼結を複数の工程で行なう。第1工程において、セラミック部材をより低温で予備焼結させ、粉末の粒子間に狭いブリッジのみを形成する。本発明に基づく方法にとっての狭いブリッジの安定性は、ちょうど、ブラスト材料による表面の処理が表面粗さの増加をもたらすようなものである必要がある。ブリッジの安定性が低すぎる場合、セラミック部材は、破砕して幾つかの部分に分かれてしまい、ブリッジの安定性が高すぎる場合、ブラスト材料による処理は、セラミック部材の表面構造を変化させるのに十分でない。予備焼結のために、880℃〜980℃の間の温度を選択する場合、ブラスト材料により表面構造の所望の変化が起きることを、試験は示した。そして、セラミック部材の内部構造は、ちょうど、ブラスト材料によってその部材から所望のサイズの断片が割れて取り出されることができるようなものである。 Sintering is performed in multiple steps. In the first step, the ceramic member is pre-sintered at a lower temperature to form only narrow bridges between the powder particles. The narrow bridge stability for the method according to the invention just needs to be such that the treatment of the surface with the blast material results in an increase of the surface roughness. If the bridge stability is too low, the ceramic member will break into several parts, and if the bridge stability is too high, the treatment with blasting material will change the surface structure of the ceramic member. not enough. Tests have shown that when a temperature between 880 ° C. and 980 ° C. is selected for presintering, the blast material causes the desired change in surface structure. And the internal structure of the ceramic member is just such that a piece of the desired size can be broken out of the member by the blast material.
予備焼結の温度が上がると、粉末材料の粒子同士の接続の強さは一般的に増加する。予備焼結の温度は、900℃よりも高い、あるいは950℃よりも低い場合、本発明に基づく方法によって、良好な結果が得られた。 As the presintering temperature increases, the strength of the connection between the particles of the powder material generally increases. Good results have been obtained with the method according to the invention when the presintering temperature is higher than 900 ° C. or lower than 950 ° C.
セラミック部材をチタン合金で被覆することができるようにするために、表面粗さRaは2.5μmよりも大きい必要がある(国際公開第2009/036845号)。本発明の文脈における粗さの値は、DIN EN ISO 4288および3274に基づく平均粗さRaに関わっており、ならびに焼結後の完成したセラミック部材に関わる。本発明に基づく方法によって達成される表面粗さは、ブラスト材料による処理にて選択されたパラメータによって決まり、例えば、ブラスト材料の粒子サイズおよび粒子がセラミック部材に衝突するスピードである。本発明に基づく方法において、完成したセラミック部材の表面粗さRaが2.5μmよりも大きくなるように、これらのパラメータを適応させることが好ましい。1つの作業工程で、表面を覆うようにコーティングを適用することができることを、確実にするために、完成したセラミック部材の表面粗さRaは、7μm以下であるべきである。 The ceramic member in order to be able to coat a titanium alloy, the surface roughness R a must be greater than 2.5 [mu] m (WO 2009/036845). Roughness values in the context of the present invention is concerned with an average roughness R a that is based on DIN EN ISO 4288 and 3274, and related to the finished ceramic component after sintering. The surface roughness achieved by the method according to the invention depends on the parameters selected in the treatment with the blast material, for example the particle size of the blast material and the speed at which the particles impinge on the ceramic member. In the process according to the invention, so that the surface roughness R a of the finished ceramic member is greater than 2.5 [mu] m, it is preferable to adapt these parameters. In one working step, that can be applied coating so as to cover the surface, in order to ensure a surface roughness R a of the finished ceramic component, should be 7μm or less.
本発明の文脈において、セラミック部材の表面全体を、ブラスト材料で処理することができる。このことは、セラミック部材の表面全体にコーティングを提供すべき場合には、都合が良い。しかしながら、表面の一部のみが被覆されるべきで、一方、表面の別の部分はコーティングがないままにすべきであることが多い。これは、例えば内部人工器官部材に当て嵌まり、その表面は一部で、骨質との接続を形成するように意図され、一方、別の部分は、別の人工器官部材との相互作用のためにスライド表面として機能するように意図される。スライド表面にとって、大きな表面粗さは望ましくない。従って、本発明に基づく方法において、セラミック部材の表面の一部のみがブラスト材料で処理され、一方、表面の別の部分はブラスト材料による処理から除外されたままであるという条件を付けることができる。本発明の文脈において、セラミック部材の表面の処理について言及する場合、これは、表面全体または表面の一部を意味することができる。 In the context of the present invention, the entire surface of the ceramic member can be treated with a blast material. This is advantageous when a coating should be provided over the entire surface of the ceramic member. However, often only a portion of the surface should be coated, while another portion of the surface should be left uncoated. This applies for example to an endoprosthesis member, whose surface is partly intended to form a connection with the bone quality, while another part is for interaction with another prosthesis member It is intended to function as a slide surface. A large surface roughness is undesirable for the slide surface. Thus, in the method according to the invention, it can be provided that only a part of the surface of the ceramic member is treated with the blast material, while another part of the surface remains excluded from the treatment with the blast material. In the context of the present invention, when referring to the treatment of the surface of a ceramic member, this can mean the entire surface or a part of the surface.
ブラスト材料の粒子サイズは、セラミック出発材料の粒子サイズと同じオーダーであることが好ましい。その場合、ブラスト材料は、セラミック部材に特に効果的に作用することができる。しかしながら、そのようなブラスト材料を用いる場合、取り出される断片の結果としてセラミック材料に生じる隙間に、ブラスト材料の粒子が付着するという危険がある。その場合、粒子は、セラミック材料において不純物を意味する。この種の不純物は、セラミック出発材料の粉末と一致する(corresponds)粉末を、ブラスト材料として用いることによって防ぐことができる。この材料の粒子がセラミック部材内に付着しても、それらは、セラミック材料の同質な組成を変えない。
The particle size of the blast material is preferably in the same order as the particle size of the ceramic starting material. In that case, the blasting material can act particularly effectively on the ceramic member. However, when using such a blast material, there is a risk that the particles of the blast material will adhere to the gaps created in the ceramic material as a result of the fragments being removed. In that case, the particles mean impurities in the ceramic material. This type of impurity can be prevented by using a powder that corresponds to the ceramic starting material powder as the blasting material. Even if particles of this material are deposited in the ceramic member, they do not change the homogeneous composition of the ceramic material.
セラミック部材の表面に適用されるコーティングは、チタン合金または純チタンでできていてよい。コーティングを適用するための可能な方法は、プラズマ溶射である。プラズマ溶射は、ガスが電気アークを通って導かれ、それによって電離される方法である。コーティング材料は、粉末状で電離ガスに導入され、そのガスのストリームによって被覆すべき加工物に運ばれる。 The coating applied to the surface of the ceramic member may be made of a titanium alloy or pure titanium. A possible method for applying the coating is plasma spraying. Plasma spraying is a method in which gas is directed through an electric arc and thereby ionized. The coating material is introduced into the ionizing gas in powder form and is carried by the gas stream to the workpiece to be coated.
ジルコニウム酸化物、アルミニウム酸化物およびこの2つの混合物は、本発明に基づく方法にとって、セラミック材料として適当であることが分かった。 Zirconium oxide, aluminum oxide and a mixture of the two have been found to be suitable as ceramic materials for the process according to the invention.
本発明を、添付図面を参照し、有利な例示的な実施形態に基づいて、以下でより詳細に説明する。図面は以下のとおりである。 The invention is explained in more detail below on the basis of advantageous exemplary embodiments with reference to the attached drawings. The drawings are as follows.
図1において、椎間板人工器官として構成された内部人工器官が、2つの脊椎体6、7の間の椎間腔に挿入されている。椎間板人工器官は、第1コンタクトプレート1および第2コンタクトプレート2を有して成る。第1コンタクトプレート1は、第1脊椎体6に接続するために構成された内部人工器官部材であり、第2コンタクトプレート2は、第2脊椎体7に接続するために構成された内部人工器官である。
In FIG. 1, an endoprosthesis configured as an intervertebral disc prosthesis has been inserted into the intervertebral space between two
第1コンタクトプレート1および第2コンタクトプレート2は、スライド表面3を合わせることによって、互いに圧迫し合う。スライド表面3は、上側コンタクトプレート1と下側コンタクトプレート2との間の動きのためのヒンジを形成する。
The
突出部12は、コンタクトプレート1、2の表面の領域13に形成され、その領域において、コンタクトプレート1、2は脊椎体6、7の骨質上に位置する。突出部12は、より緩やかなフランクをコンタクトプレート1、2が椎間腔に押し込まれる方向に有し、より急なフランクを反対方向に有する。緩やかな方のフランクは、コンタクトプレート1、2を椎間腔に押し込むのをより容易にさせる。突出部12が脊椎体6、7の骨質に侵入した場合、急な方のフランクは、コンタクトプレート1、2を維持させる。急な方のフランクは、コンタクトプレート1、2が椎間腔から反対方向に再び引き戻されるのを防止する。
The
コンタクトプレート1、2のフランジ4、5は、脊椎体6、7の腹側の面上に位置することが意図される。フランジ4、5は、コンタクトプレート1、2が所望の位置よりも遠くへ背側の方向に椎間腔の中へ押し込まれることができないという効果をもたらす。
The
コンタクトプレート1およびコンタクトプレート2は、セラミック材料9から形成される。コンタクトプレート1、2上のスライド表面3は、セラミック材料9の表面に形成される。骨質との接続が確立される領域13は、チタン合金コーティング10で被覆される。
The
図2は、コンタクトプレート1、2の拡大詳細図を示し、そこにおいて、セラミック材料9とコーティング10との間に界面8が図示される。セラミック材料9は、コーティング10との界面8にて、少なくとも2.5μmの粗さRaを有する。界面8におけるこの粗さは、コーティング10との安定な接続を確立するには十分であるが、骨質との安定な接続には十分ではない。コーティング10は、セラミック材料9よりも、より大きな粗さおよびより大きな多孔性を有し、それによって、骨質との安定な接続を形成する。
FIG. 2 shows an enlarged detailed view of the
表面の一部が所望の粗さを有する内部人工器官部材として、セラミック部材を製造するために、まず、粉末状で存在する出発材料を、製造することになっているセラミック部材と形状が対応するモールドに導入する。セラミック部材は、その後の方法工程の結果として体積が減少するため、モールドは、完成したセラミック部材よりも大きな大きさを有する。その粉末を、例えば振動および圧力によって、モールド内で機械的に圧縮し、そうすると、図3にて概略的に図示されるように、粉末の粒子14は互いに隣接する。920℃の温度での予備焼結の結果、(図4に図示される)ブリッジが、粒子14間に生じる。今やセラミック部材をモールドから取り出すことができるほど、材料の内部構造は安定である。
In order to manufacture a ceramic member as an endoprosthetic member having a desired surface roughness, first the starting material present in powder form corresponds to the shape of the ceramic member to be manufactured. Introduce into mold. Since the ceramic member decreases in volume as a result of subsequent method steps, the mold has a larger size than the finished ceramic member. The powder is mechanically compressed in the mold, for example by vibration and pressure, so that the
ブリッジ15によって、セラミック材料は、穿孔またはフライス削りによる機械加工のために選択されるであろうものよりも、その構造に関してより大きな安定性を有する。構造の安定性は、具体的に言うと、出発材料と一致する粉末でブラストすることによって、予備焼成したセラミック材料から断片を切り離すことができるほどである。その断片は、焼成後、完成したセラミック部材が所望の表面粗さを有するほどの大きさである。
With the
所望の表面構造を得て、機械加工が終了したら、セラミック部材を、予備焼結の温度よりも高い温度で焼結させる。以前ブリッジ15によってしか接続されていなかった粒子の界面に、平面的な接続16が生じる。内部から空隙が無くなるため、セラミック部材の体積は更に減少する。ブラスト材料により処理された表面の部分にて、今やその表面は、約4μmの粗さRaを有する。表面のこの部分に適用されるチタン合金でできたコーティングは、表面にしっかりと付着する。
Once the desired surface structure is obtained and machining is complete, the ceramic member is sintered at a temperature higher than the presintering temperature. A
Claims (9)
a.粉末状のセラミック出発材料を利用可能にする工程;
b.セラミック部材の形状を予め規定するモールドを利用可能にする工程;
c.セラミック出発材料をモールドに導入する工程;
d.セラミック出発材料を880℃〜980℃の間の温度で予備焼結させる工程;
e.セラミック部材をモールドから取り出す工程;
f.セラミック部材の表面をブラスト材料で処理する工程;
g.セラミック部材を予備焼結の温度よりも高い温度で焼結させる工程
を含む方法。 A method for producing a ceramic member comprising the following steps:
a. Making powdered ceramic starting material available;
b. Making available a mold that predefines the shape of the ceramic member;
c. Introducing a ceramic starting material into the mold;
d. Pre-sintering the ceramic starting material at a temperature between 880 ° C. and 980 ° C .;
e. Removing the ceramic member from the mold;
f. Treating the surface of the ceramic member with a blast material;
g. A method comprising sintering the ceramic member at a temperature higher than the temperature of the pre-sintering.
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EPPCT/EP2008/006524 | 2008-08-07 | ||
PCT/EP2008/006524 WO2009036845A2 (en) | 2007-09-13 | 2008-08-07 | Endoprosthesis component |
PCT/EP2009/005746 WO2010015414A1 (en) | 2008-08-07 | 2009-08-07 | Method for producing a ceramic component |
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JP2011529850A JP2011529850A (en) | 2011-12-15 |
JP5535212B2 true JP5535212B2 (en) | 2014-07-02 |
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EP2187843B1 (en) | 2007-09-13 | 2015-10-07 | DERU GmbH | Endoprosthesis component |
JP6914335B2 (en) * | 2017-07-28 | 2021-08-04 | 京セラ株式会社 | Parts for plasma processing equipment |
CN112979322B (en) * | 2021-02-20 | 2023-09-08 | 北京北方华创微电子装备有限公司 | Ceramic part and manufacturing method thereof |
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DE3516411A1 (en) * | 1985-05-07 | 1986-11-13 | Plasmainvent AG, Zug | COATING OF AN IMPLANT BODY |
JPS63146407A (en) * | 1986-12-10 | 1988-06-18 | 松下電器産業株式会社 | Manufacture of voltage nonlinear resistor |
JPH0731150B2 (en) * | 1987-02-16 | 1995-04-10 | 日本碍子株式会社 | Oxygen sensor element and manufacturing method thereof |
CH681516A5 (en) * | 1989-09-13 | 1993-04-15 | Asea Brown Boveri | |
DE4322084A1 (en) * | 1993-07-02 | 1995-01-12 | Abb Research Ltd | Process for the production of a setter |
DE4322085A1 (en) * | 1993-07-02 | 1995-01-12 | Abb Research Ltd | Method for the production of a moulding from a powder material |
DE4322083A1 (en) * | 1993-07-02 | 1995-01-12 | Abb Research Ltd | Method for the production of a moulding from a powder material |
US5776408A (en) * | 1996-08-23 | 1998-07-07 | Eastman Kodak Company | Method of engraving green ceramic articles |
DE19755536A1 (en) * | 1997-12-13 | 1999-06-17 | Ceramtec Ag | Acetabular cup |
DE10159683A1 (en) * | 2001-11-30 | 2003-06-18 | Michael Gahlert | Dantalimplantat |
ATE345747T1 (en) * | 2003-01-23 | 2006-12-15 | Dinkelacker Wolfgang | BONE IMPLANT AND METHOD FOR THE PRODUCTION THEREOF |
JP4370817B2 (en) * | 2003-06-09 | 2009-11-25 | Tdk株式会社 | Ferrite substrate manufacturing method |
JP4522117B2 (en) * | 2004-03-23 | 2010-08-11 | 京セラ株式会社 | Method for manufacturing processing container member used in semiconductor or liquid crystal manufacturing apparatus |
JP4543152B2 (en) * | 2004-08-20 | 2010-09-15 | 独立行政法人産業技術総合研究所 | Transparent titanium-coated biocompatible material |
US20090246735A1 (en) * | 2006-08-25 | 2009-10-01 | Dirk Rogowski | Process for producing coloured sintered ceramic bodies, in particular for dental applications |
EP2187843B1 (en) * | 2007-09-13 | 2015-10-07 | DERU GmbH | Endoprosthesis component |
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