DE19809932C1 - Method for coloring surgical instruments made of steel or heat resistant plastic - Google Patents

Method for coloring surgical instruments made of steel or heat resistant plastic

Info

Publication number
DE19809932C1
DE19809932C1 DE1998109932 DE19809932A DE19809932C1 DE 19809932 C1 DE19809932 C1 DE 19809932C1 DE 1998109932 DE1998109932 DE 1998109932 DE 19809932 A DE19809932 A DE 19809932A DE 19809932 C1 DE19809932 C1 DE 19809932C1
Authority
DE
Germany
Prior art keywords
surgical instruments
coloring
anodic oxidation
steel
resistant plastic
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
Application number
DE1998109932
Other languages
German (de)
Inventor
Richard Zeller
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Aesculap AG
Original Assignee
Aesculap AG
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 Aesculap AG filed Critical Aesculap AG
Priority to DE1998109932 priority Critical patent/DE19809932C1/en
Application granted granted Critical
Publication of DE19809932C1 publication Critical patent/DE19809932C1/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
    • A61L27/30—Inorganic materials
    • A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A61L31/082—Inorganic materials
    • A61L31/088—Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon

Abstract

The surgical instruments are coated with a layer of titanium between 2 and 10 micro m thick. Subsequently, an oxide layer with a thickness in the nanometer range is produced on this coating by anodic oxidation.

Description

Die Erfindung betrifft ein Verfahren zum Einfärben von chirurgischen Instrumenten, die aus einem vakuumbestän­ digen, hochtemperaturfesten Kunststoff oder aus Stahl bestehen.The invention relates to a method for coloring surgical instruments made from a vacuum high-temperature-resistant plastic or steel consist.

Chirurgische Instrumente werden aus Gründen der Körper­ verträglichkeit häufig aus Titan hergestellt. Aller­ dings ergeben sich dabei Schwierigkeiten, wenn kompli­ zierte Formen notwendig sind, da Titan schwer zu bear­ beiten ist.Surgical instruments are made for the sake of the body Compatibility often made from titanium. Everything Difficulties arise when compli graceful shapes are necessary because titanium is difficult to bear is working.

Andererseits gibt es chirurgische Instrumente aus ande­ ren verformbaren Substraten, beispielsweise aus Stahl, die wesentlich leichter herstellbar sind. Diese haben jedoch den Nachteil, daß sie an ihrer Oberfläche nicht dauerhaft einfärbbar sind. Eine solche Einfärbbarkeit wird jedoch bei chirurgischen Instrumenten häufig ge­ wünscht, um diese Instrumente identifizieren zu können, beispielsweise um eine klare Zuordnung zwischen einem handhabbaren Instrumente und einem Implantat zu gewähr­ leisten.On the other hand, there are surgical instruments from others ren deformable substrates, for example made of steel, which are much easier to manufacture. Have this however, the disadvantage that they are not on their surface can be colored permanently. Such colorability is however often used with surgical instruments wishes to be able to identify these instruments for example, a clear assignment between one to handle manageable instruments and an implant Afford.

Es ist Aufgabe der Erfindung, ein Verfahren zum Einfär­ ben von chirurgischen Instrumenten vorzuschlagen, die aus hochtemperaturfestem Kunststoff oder aus Stahl be­ stehen.It is an object of the invention to provide a method for coloring propose surgical instruments that  made of high temperature resistant plastic or steel stand.

Diese Aufgabe wird bei einem Verfahren der eingangs be­ schriebenen Art erfindungsgemäß dadurch gelöst, daß man die Instrumente mit einer dünnen Titanschicht mit einer Dicke zwischen 2 und 10 µm beschichtet und diese durch anodische Oxidation an ihrer Oberfläche in einer Schichtdicke im Nanometerbereich oxidiert.This task is in a process of the beginning Written type solved according to the invention in that the instruments with a thin layer of titanium with a Coated thickness between 2 and 10 microns and this through anodic oxidation on their surface in one Layer thickness in the nanometer range oxidized.

Es hat sich überraschend herausgestellt, daß durch die­ ses Verfahren auch bei den genannten Substraten durch die Erzeugung einer Sandwichbauweise an der Oberfläche eine Oberflächeneinfärbung erzielt werden kann, die dauerhaft ist, die also auch eine größere Anzahl von Sterilisationszyklen gut übersteht.It has surprisingly been found that the ses procedure for the substrates mentioned the creation of a sandwich construction on the surface a surface coloring can be achieved that is permanent, which is also a larger number of Sterilization cycles survived well.

An sich ist es bereits bekannt, chirurgische Instrumen­ te mit einer Zwischenschicht zu versehen und auf diese einen Überzug aus unterstöchiometrischem TiO2-x, aufzu­ bringen (DE 39 02 250 C1).It is known per se to provide surgical instruments with an intermediate layer and to apply a coating of substoichiometric TiO 2-x thereon (DE 39 02 250 C1).

Weiterhin ist es bekannt, chirurgische Instrumente und Implantate mit Titan zu beschichten und eine weitere Beschichtung aus TiO2 vorzunehmen. Diese weitere Be­ schichtung wird aber sowohl mittels CVD als auch mit­ tels PVD Verfahren vorgenommen, also nicht durch anodi­ sche Oxidationen, außerdem werden andere Dicken der Oxidschicht verwandt (DE 195 06 188). Im Rahmen der DE 40 05 692 A1 wird ein Verfahren beschrieben, bei dem durch Hochvakuum-Plasma-Beschichtung Oxidschichten auf ein Substrat aufgebracht werden, jedoch mit Schichtdic­ ken im Mikrometerbereich, also in einem wesentlich hö­ heren Bereich als bei dem hier beschriebenen Verfahren.Furthermore, it is known to coat surgical instruments and implants with titanium and to carry out a further coating of TiO 2 . However, this further coating is carried out both by means of CVD and by means of PVD processes, that is to say not by anodic oxidation, and other thicknesses of the oxide layer are also used (DE 195 06 188). DE 40 05 692 A1 describes a method in which oxide layers are applied to a substrate by high vacuum plasma coating, but with layer thicknesses in the micrometer range, that is to say in a much higher range than in the method described here.

Es ist dabei vorteilhaft, wenn man die anodische Oxida­ tion mit einer Gleichspannung bis maximal 130 Volt aus­ führt, insbesondere bei einer Gleichspannung zwischen 30 und 80 Volt.It is advantageous if the anodic oxide tion with a DC voltage of up to 130 volts leads, especially with a DC voltage between 30 and 80 volts.

Es ist günstig, wenn man die anodische Oxidation mit einer Stromdichte zwischen 100 und 200 mA/cm2 durch­ führt.It is advantageous if the anodic oxidation is carried out with a current density between 100 and 200 mA / cm 2 .

Insbesondere kann man die anodische Oxidation in einem Elektrolyten ausführen, der Zitronensäure enthält.In particular, the anodic oxidation can be carried out in one Run electrolytes that contain citric acid.

Günstig ist es weiterhin, wenn man die Titanschicht durch eine Vakuumbeschichtung aufbringt. Beispielsweise kann die Titanschicht eine Vakuumprüferbeschichtungs­ schicht sein.It is also favorable if you have the titanium layer by applying a vacuum coating. For example the titanium layer can be a vacuum tester coating be a shift.

Die nachfolgende Beschreibung einer bevorzugten Ausfüh­ rungsform der Erfindung dient im Zusammenhang mit der beiliegenden Zeichnung der näheren Erläuterung. Es zei­ gen:The following description of a preferred embodiment tion form of the invention serves in connection with the enclosed drawing of the detailed explanation. It shows gene:

Fig. 1: einen chirurgischen Clip mit einer oberflächlich oxidierten Titanbeschich­ tung und Fig. 1: a surgical clip with a surface oxidized titanium coating and device

Fig. 2: eine Schnittansicht längs Linie 2-2 in Fig. 1. Fig. 2 is a sectional view taken along line 2-2 in Fig. 1.

Die vorliegende Erfindung bezieht sich auf chirurgische Instrumente im weitesten Sinne, darunter werden alle Handhabungswerkzeuge, Implantate und sonstigen in der Chirurgie Verwendung findenden Teile verstanden, die aus einem verformbaren Substrat bestehen und bei denen der Wunsch besteht, daß sie oberflächlich eingefärbt werden. Nachfolgend wird die Erfindung am Beispiel ei­ nes in der Zeichnung nur schematisch dargestellten Ge­ fäßclips 1 erörtert. Ein solcher Gefäßclip 1 mit zwei elastisch gegeneinander biegbaren Branchen 2, 3 weist eine relativ komplizierte Außenkontur auf, er besteht beispielsweise aus einem Substrat aus Stahl, dieses Ma­ terial ist günstig zu verformen und zu bearbeiten, so daß die komplizierte Außenkontur des Gefäßclips 1 leicht zu erreichen ist.The present invention relates to surgical instruments in the broadest sense, including all handling tools, implants and other parts used in surgery, which consist of a deformable substrate and for which there is a desire that they be colored on the surface. In the following, the invention is discussed using the example of egg nes in the drawing, only schematically illustrated vessel clips 1 . Such a vessel clip 1 with two elastically bendable branches 2 , 3 has a relatively complicated outer contour, it consists for example of a substrate made of steel, this material is inexpensive to deform and edit, so that the complicated outer contour of the vessel clip 1 easily to achieve.

Dieser Gefäßclip 1 wird in einer an sich bekannten Va­ kuumbeschichtungsanlage mit einer dünnen Schicht 4 aus Reintitan beschichtet, die Schichtdicke liegt dabei zwischen 2 und 10 µm.This vessel clip 1 is coated in a known vacuum coating system with a thin layer 4 of pure titanium, the layer thickness is between 2 and 10 microns.

Das in dieser Weise mit einer Titanschicht 4 versehene Instrument wird anschließend in einer geeigneten Anlage anodisch oxidiert, dazu wird das Instrument in einen Elektrolyten gehalten, der beispielsweise 1,8% Zitro­ nensäure enthält, das zu oxidierende Teil wird als An­ ode geschaltet, als Kathode kann ein Titanblech dienen. The instrument provided in this way with a titanium layer 4 is then anodically oxidized in a suitable system, for this purpose the instrument is held in an electrolyte which contains, for example, 1.8% citric acid, the part to be oxidized is connected as an anode, as a cathode can be used a titanium sheet.

Zwischen den Elektroden wird eine Gleichspannung von maximal 130 Volt, insbesondere in der Größenordnung zwischen 30 und 80 Volt angelegt, wobei die Größe der Gleichspannung einen Einfluß auf die erzielbare Farbe hat. Mit einer Stromdichte in der Größenordnung zwi­ schen 100 und 200 mA/cm2 wird dann die Titanschicht oberflächlich anodisch oxidiert, und zwar mit einer Schichtdicke in der Größenordnung von 50 nm und 250 nm.A maximum DC voltage of 130 volts, in particular in the range between 30 and 80 volts, is applied between the electrodes, the magnitude of the DC voltage having an influence on the color that can be achieved. With a current density in the order of between 100 and 200 mA / cm 2 , the titanium layer is then surface anodically oxidized, with a layer thickness in the order of 50 nm and 250 nm.

Das in dieser Weise mit einer doppelten Beschichtung versehene Instrument weist eine deutlich erkennbare, leuchtende Farbgebung auf und ist durch die Beschich­ tung mit Titan in hohem Maße körperverträglich.This is done with a double coating provided instrument has a clearly recognizable, bright coloring and is due to the coating treatment with titanium to a high degree.

Claims (6)

1. Verfahren zum Einfärben von chirurgischen Instru­ menten, die aus einem vakuumbeständigen, hochtem­ peraturfesten Kunststoff oder aus Stahl bestehen, dadurch gekennzeichnet, daß man die Instrumente mit einer dünnen Titanschicht mit einer Dicke zwischen 2 und 10 µm beschichtet und diese durch anodische Oxidation an ihrer Oberfläche in einer Schichtdicke im Nanometerbereich oxidiert.1. A method for coloring surgical instru ments, which consist of a vacuum-resistant, high temperature resistant plastic or steel, characterized in that the instruments are coated with a thin titanium layer with a thickness between 2 and 10 microns and this by anodic oxidation on them Surface oxidized in a layer thickness in the nanometer range. 2. Verfahren nach Anspruch 1, dadurch gekennzeich­ net, daß man die anodische Oxidation mit einer Gleichspannung bis maximal 130 Volt ausführt.2. The method according to claim 1, characterized in net that the anodic oxidation with a DC voltage up to a maximum of 130 volts. 3. Verfahren nach Anspruch 2, dadurch gekennzeich­ net, daß man die anodische Oxidation mit einer Gleichspannung zwischen 30 und 80 Volt ausführt.3. The method according to claim 2, characterized in net that the anodic oxidation with a DC voltage between 30 and 80 volts. 4. Verfahren nach einem der voranstehenden Ansprü­ che, dadurch gekennzeichnet, daß man die anodi­ sche Oxidation mit einer Stromdichte zwischen 100 und 200 mA/cm2 durchführt. 4. The method according to any one of the preceding Ansprü surface, characterized in that one carries out the anodic oxidation with a current density between 100 and 200 mA / cm 2 . 5. Verfahren nach einem der voranstehenden Ansprü­ che, dadurch gekennzeichnet, daß man die anodi­ sche Oxidation in einem Elektrolyten ausführt, der Zitronensäure enthält.5. Method according to one of the preceding claims che, characterized in that the anodi performs oxidation in an electrolyte, which contains citric acid. 6. Verfahren nach einem der voranstehenden Ansprü­ che, dadurch gekennzeichnet, daß man die Titan­ schicht durch eine Vakuumbeschichtung aufbringt.6. Method according to one of the preceding claims che, characterized in that the titanium layer by applying a vacuum coating.
DE1998109932 1998-03-07 1998-03-07 Method for coloring surgical instruments made of steel or heat resistant plastic Expired - Fee Related DE19809932C1 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006013115A1 (en) * 2004-08-06 2006-02-09 Politecnico Di Milano Method for the protection/selective colouring of an end­product
DE102011107787A1 (en) 2011-07-15 2013-01-17 Oerlikon Trading Ag, Trübbach Method for improving the wear resistance of colored surgical instruments
DE102012003851A1 (en) 2012-02-29 2013-08-29 Oerlikon Trading Ag, Trübbach Component with temperature-sensitive appearance of the surface
WO2018220002A1 (en) * 2017-05-30 2018-12-06 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein Coated substrate having a titanium-containing coating and a modified titanium oxide coating

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6092761A (en) * 1983-10-28 1985-05-24 京セラ株式会社 Metal member for living body implant
WO1986006617A1 (en) * 1985-05-07 1986-11-20 Plasmainvent Ag Coating of an implant body
DE3902250C1 (en) * 1989-01-26 1990-02-01 Aesculap Ag, 7200 Tuttlingen, De Surgical instrument for laser surgery
DE4005692A1 (en) * 1990-02-23 1991-08-29 Omt Oberflaechen Materialtech METHOD FOR PRODUCING PHYSIOLOGICALLY COMPATIBLE OXIDE LAYERS ON SKELETON IMPLANTS
DE4311772A1 (en) * 1992-04-10 1993-10-14 Tavkoezlesi Kutato Intezet Bud Biocompatible implants comprising titanium@ for bone surgery - are prepd. by anodic oxidation of etched surface treated with phosphate-contg. soln., and then heat treating
JPH06315489A (en) * 1993-05-10 1994-11-15 Nikon Corp In-bone implant
EP0700685A2 (en) * 1994-09-12 1996-03-13 Japan Energy Corporation Titanium implantation materials for the living body
DE19506188A1 (en) * 1995-02-22 1996-08-29 Miladin Dr Lazarov Implant

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6092761A (en) * 1983-10-28 1985-05-24 京セラ株式会社 Metal member for living body implant
WO1986006617A1 (en) * 1985-05-07 1986-11-20 Plasmainvent Ag Coating of an implant body
DE3902250C1 (en) * 1989-01-26 1990-02-01 Aesculap Ag, 7200 Tuttlingen, De Surgical instrument for laser surgery
DE4005692A1 (en) * 1990-02-23 1991-08-29 Omt Oberflaechen Materialtech METHOD FOR PRODUCING PHYSIOLOGICALLY COMPATIBLE OXIDE LAYERS ON SKELETON IMPLANTS
DE4311772A1 (en) * 1992-04-10 1993-10-14 Tavkoezlesi Kutato Intezet Bud Biocompatible implants comprising titanium@ for bone surgery - are prepd. by anodic oxidation of etched surface treated with phosphate-contg. soln., and then heat treating
JPH06315489A (en) * 1993-05-10 1994-11-15 Nikon Corp In-bone implant
EP0700685A2 (en) * 1994-09-12 1996-03-13 Japan Energy Corporation Titanium implantation materials for the living body
DE19506188A1 (en) * 1995-02-22 1996-08-29 Miladin Dr Lazarov Implant

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006013115A1 (en) * 2004-08-06 2006-02-09 Politecnico Di Milano Method for the protection/selective colouring of an end­product
DE102011107787A1 (en) 2011-07-15 2013-01-17 Oerlikon Trading Ag, Trübbach Method for improving the wear resistance of colored surgical instruments
WO2013010647A1 (en) 2011-07-15 2013-01-24 Oerlikon Trading Ag, Trübbach Method for improving the wear resistance of dyed surgical instruments
CN103649363A (en) * 2011-07-15 2014-03-19 欧瑞康贸易股份公司(特吕巴赫) Method for improving the wear resistance of dyed surgical instruments
US20140171924A1 (en) * 2011-07-15 2014-06-19 Oerlikon Trading Ag, Trubbach Method for improving the wear resistance of dyed surgical instruments
US9175378B2 (en) * 2011-07-15 2015-11-03 Oerlikon Surface Solutions Ag, Trubbach Method for improving the wear resistance of dyed surgical instruments
DE102012003851A1 (en) 2012-02-29 2013-08-29 Oerlikon Trading Ag, Trübbach Component with temperature-sensitive appearance of the surface
WO2013127506A2 (en) 2012-02-29 2013-09-06 Oerlikon Trading Ag, Trübbach Unit having temperature-sensitive appearance of the surface thereof
WO2018220002A1 (en) * 2017-05-30 2018-12-06 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein Coated substrate having a titanium-containing coating and a modified titanium oxide coating

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