US20150342469A1 - Thin metal membrane with support - Google Patents

Thin metal membrane with support Download PDF

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Publication number
US20150342469A1
US20150342469A1 US14/653,340 US201314653340A US2015342469A1 US 20150342469 A1 US20150342469 A1 US 20150342469A1 US 201314653340 A US201314653340 A US 201314653340A US 2015342469 A1 US2015342469 A1 US 2015342469A1
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Prior art keywords
layer
component
metal
composite
layers
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Inventor
Nicholas Baltos
Oliver Keitel
Lena WEBER
Andreas Reisinger
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Heraeus Deutschland GmbH and Co KG
Heraeus Medical Components LLC
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Heraeus Deutschland GmbH and Co KG
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Assigned to Heraeus Deutschland GmbH & Co. KG reassignment Heraeus Deutschland GmbH & Co. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HERAEUS MEDICAL COMPONENTS LLC
Publication of US20150342469A1 publication Critical patent/US20150342469A1/en
Assigned to HERAEUS MEDICAL COMPONENTS LLC reassignment HERAEUS MEDICAL COMPONENTS LLC ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BALTOS, Nicholas
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
    • A61B5/021—Measuring pressure in heart or blood vessels
    • A61B5/0215—Measuring pressure in heart or blood vessels by means inserted into the body
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B1/00—Layered products having a non-planar shape
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
    • B81C1/00158—Diaphragms, membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/02—Details of sensors specially adapted for in-vivo measurements
    • A61B2562/0247—Pressure sensors
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/12—Manufacturing methods specially adapted for producing sensors for in-vivo measurements
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
    • A61B5/024—Detecting, measuring or recording pulse rate or heart rate
    • A61B5/02444—Details of sensor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00—Specific applications of microelectromechanical systems
    • B81B2201/02—Sensors
    • B81B2201/0264—Pressure sensors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2203/00—Basic microelectromechanical structures
    • B81B2203/01—Suspended structures, i.e. structures allowing a movement
    • B81B2203/0127—Diaphragms, i.e. structures separating two media that can control the passage from one medium to another; Membranes, i.e. diaphragms with filtering function
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12361—All metal or with adjacent metals having aperture or cut
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component

Definitions

  • Membranes having a low membrane thickness maybe used as transmission media for pressure sensors in implantable devices or in medical instruments to be inserted into the human body for measurements and other activities.
  • the pressure differences encountered inside the body are relatively low. For this reason, it is necessary to use membranes that are as thin as possible. This enables the transmission of pressure, and therefore the pressure measurement, to be accurate.
  • all materials that are used in this context and contact body fluids must be biocompatible.
  • Membranes of this type are known. Both metallic and plastic-based membranes are currently in use as materials. Conventionally, very thin metallic membranes are produced by abrading production methods, for example by milling or erosion. However, such membranes are not as thin as needed. Further, if membrane thicknesses of less than 50 ⁇ m are to be attained with these methods, a substantial effort is required in order to achieve homogeneous quality.
  • a thin sheet of metal or metal foil of the desired thickness is used via a weld connection. It is feasible in this way to produce metal sheets and metal foils with low layer thicknesses.
  • a base body that would guarantee an airtight weld connection and homogeneous quality at acceptable prices.
  • a soldering procedure as an alternative to welding would be conceivable. However, this is disadvantageous in that further metals and alloys would need to be incorporated in addition to the participating metals. These alloys often have very limited biocompatibility. Moreover, this procedure bears the risk of forming local elements, which is associated with corrosion.
  • a production method for silicon membranes is known from micro system technology, a field that is distant from the production of biocompatible objects. Such silicon membranes are used as flow sensors. The membranes are produced by selective etching of the silicon wafer.
  • the following documents are cited as pertinent examples: DE 10 2005 023 699 A1, EP 1 114 985 A1, and WO 1997/21986 A1.
  • the cited methods apply dry etching with hydrogen chloride gas, which is common in the semiconductor industry. This approach is limited to silicon wafers and cannot be applied to the production of implantable membranes.
  • the present invention is based on the object to provide an implantable component comprising a preferably metallic substrate and a metallic membrane, wherein the layer thickness of the membrane is as low as possible.
  • FIG. 1 shows a process for producing a composite according to one embodiment of the invention
  • FIG. 2 shows a process for producing a composite according to a second embodiment of the invention
  • FIG. 3 shows a process for producing a component comprising a support layer and a membrane according to a further embodiment of the invention
  • FIG. 4 is a flowchart corresponding to the process depicted in FIG. 3 ;
  • FIG. 5 shows another process for producing a component comprising a support layer and a membrane
  • FIG. 6 is a flowchart corresponding to the process depicted in FIG. 5 ;
  • FIG. 7 shows examples of components according to embodiments of the invention, each comprising a composite made of two layers.
  • FIG. 8 shows a schematic of a device 10 according to an embodiment of the invention.
  • the present invention generally relates to a component comprising a composite of at least two layers that are connected to each other.
  • the first layer comprises a hole and the second layer has a thickness in the range of 1 to 50 ⁇ m.
  • the first and second layers each comprise at least one metal and the compositions of the first and second layers are different.
  • the present invention is also directed to a method for producing a component comprising at least two layers that are connected to each other and have the aforementioned features, a method for producing a component comprising at least three layers that are connected to each other and have the aforementioned features, as well as a component that is obtained by one of the aforementioned methods and the use of at least one of the aforementioned components in a living body or for producing an implant for use in a living body.
  • a component in particular a membrane, comprising a composite of at least two layers that are connected to each other.
  • the first layer comprises at least one hole
  • the second layer has a thickness in the range of 1 to 50 ⁇ m, preferably of 1 to 40 ⁇ m, or of 1 to 30 ⁇ m, or of 1 to 15 ⁇ m
  • the first layer and the second layer each comprises at least one metal
  • the compositions of the first and second layers are different.
  • a hole may be understood to be a region of a layer where the layer is discontinuous throughout its entire thickness.
  • the hole is bordered in the plane of the layer by a margin made of layer.
  • continuous may be understood to mean that the object thus specified or the region of a layer thus specified does not contain a hole, a gap of materials or the like.
  • An object specified as being continuous may comprise variations in thickness if the thickness is always larger than zero.
  • the thickness of the layer is the extension of that layer perpendicular to a plane that may be placed in the layer at the measuring location. If the measurement of the thickness of a layer at multiple locations yields different values, the thickness is the arithmetic mean of the measured values. If the layer forms a tube, the tangential plane at the measuring location on the tube may be understood to be the plane in the layer.
  • impervious may be understood to mean that a liquid, in particular water, or a gas, in particular helium, cannot pass through the object specified as being impervious at a pressure applied to the object in the range of 0 to 30,000 Pa.
  • the imperviousness is measured by means of a tightness test of the object with helium (so-called “helium leakage test”) according to the MIL-STD-883H standard, method 1014.13, test condition A 4 .
  • the term resistant may be understood to mean that a mass of an object specified as being resistant that is in contact with a substance does not decrease during the time of contact. In the spirit of the present invention, this is the case if the mass of the object after contact with the substance is less than 0.1% less than before contact with the liquid. Preferably, the mass increases or takes when it is in contact with another substance.
  • biocompatible may be understood to mean that the object referred to as being biocompatible meets the pertinent biocompatibility requirements according to the ISO 10993 part 1-20 standard.
  • the at least two layers of the component according to the invention that are connected to each other form a membrane.
  • a membrane of this type is used, for example, in devices for measuring a pressure difference, for example of a blood pressure in a human or in an animal.
  • the two layers that are connected to each other and the component according to the invention are suitable for determining a pressure difference of up to 25,000 Pa.
  • a pressure difference may be understood to mean that a relative pressure or pressure change, rather than an absolute pressure, is being measured.
  • the first layer according to the invention may comprise any shape that is suitable for connecting to the second layer and may consist of any material that is suitable for connecting to the second layer.
  • the first layer and the second layer form a 2-dimensional composite, whereby the first layer contains one hole or multiple holes in the region of the surface superimposed by the second layer.
  • the first layer is preferably provided as a substrate and the second layer is preferably provided as a membrane.
  • the composite of first and second layers is impervious with respect to gases or liquids, and is preferably impervious with respect to gases and liquids.
  • a combination of a hole in the first layer and a superimposed continuous second layer forms a membrane in which the first and second layers are connected in a continuous manner at the boundaries of the hole with respect to the first layer.
  • the first layer forms a support for the membrane. This support may be shaped, for example, as a frame or as a grid.
  • the second layer has no holes, at least in those regions that are superimposed over one or more holes in the first layer.
  • regions of the component may, for example, serve for assembly of the composite of the first layer and second layer in the component.
  • the first layer of the component has a thickness in the range of 50 to 500 ⁇ m, preferably of 70 to 350 ⁇ m, or of 90 to 200 ⁇ m.
  • the thickness of this layer may be determined by common measuring methods, in particular with a micrometer measuring screw.
  • the second layer of the component has a thickness in the range of 2.0 to 25 ⁇ m, preferably of 3 to 15 ⁇ m.
  • the thickness of this layer may also be determined by common measuring methods, in particular on a transverse section of the layer by scanning electron microscopy.
  • the material of the first layer comprises at least one metal.
  • all metals that are known to and are deemed well-suited for the intended purpose by a person skilled in the art are conceivable.
  • the composition of the first layer differs from the composition of the second layer.
  • the compositions of the first layer and of the second layer are selected appropriately such that the composition of the first layer may be chemically removed by treatment with a liquid CA, whereas the composition of the second layer is resistant to this liquid CA at least for the duration of treatment of the first layer with the liquid CA.
  • the liquid CA may be appropriately selected such that the electrochemical potential of the liquid CA is larger than the electrochemical potential of the composition of the first layer at the surface of contact to the liquid CA. Moreover, the liquid CA is selected appropriately such that the electrochemical potential of the liquid CA is smaller than the electrochemical potential of the composition of the second layer at the surface of contact to the liquid CA.
  • the electrochemical potentials of the compositions of the first, second and, if applicable, further layers and of the liquid CA during the treatment may be calculated by means of the Nernst equation (Roempp-Lexikon Chemie, 10th ed. (1998), volume 4, page 2869, entry “Nernstsche Gleichung” (Nernst equation)).
  • a non-noble metal is included in a composition of a layer, the electrochemical potential of the metal and of the composition containing the metal may deviate from the aforementioned theoretical values.
  • the non-noble metal behaves like a metal with a more positive E value than would be expected from its electrochemical potential. This phenomenon is called passivation.
  • the potential of the passivated metal is called passivation potential.
  • a passivation potential may arise in the case of a non-noble metal if a non-noble metal contacts water, air, liquid CA or a combination of two or more thereof.
  • a continuous firmly-adhering passive layer made of an oxide or hydroxide of the non-noble metal is then formed at the contact surface.
  • the passive layer at the surface of contact to a liquid CA affects the passivation potential.
  • This passivation potential must be attained in order to be able to chemically remove the layer of metal situated underneath the passive layer in order to first remove the passive layer and then the metal of the metal layer.
  • parts of the metal are preferably dissolved and abraded by oxidation from the metal body, for example a metal layer.
  • a contact surface is the surface of a layer that contacts the liquid CA when this layer is treated with a liquid CA.
  • the passivation potential is the electrochemical potential of a layer at the contact surface. Accordingly, a composite of at least two layers that are connected to each other is preferred, in which the electrochemical potential of the first layer at its surface of contact to a liquid CA is smaller than the electrochemical potential of the second layer at its surface of contact to the liquid CA.
  • a suitable liquid CA for a given composite of first and second layers is to perform dissolution experiments.
  • a liquid in consideration for the liquid CA is applied to weighed samples of the first and second layers and allowed to act for a period of time at treatment conditions (temperature, applied electrical voltage). Subsequently, the liquid is removed and the samples are weighed again.
  • the liquid is deemed suitable as liquid CA if a decrease in weight due to the treatment with a liquid is noted in the sample of the first layer, whereas no decrease in weight is noted in the sample of the second layer.
  • the at least one metal of the first layer of the component is selected from the group consisting of silver, gold, platinum, titanium, iridium, niobium, tantalum, tungsten, palladium, copper, iron, steel, and stainless steel, in as far as suitable for medical implants, such as, e.g., 316L and 304, or a combination of at least two thereof. If multiple metals are present in the first layer as a combination, the combination is preferred to be an alloy.
  • Preferred alloys for the first layer are alloys including niobium and tantalum; nickel and titanium; or platinum and iridium.
  • one or more further metals may be present in the aforementioned alloys. These further metals may be those from the list specified above or others that have not been specified above.
  • the at least one metal of the second layer is selected from the same metals from the same group, except for copper and iron, as the at least one metal of the first layer. If multiple metals are present as a combination, the combination is preferred to be an alloy; the alloys specified for the first layer are also preferred in this case. It is also preferred that this alloy contains one or more further metals. These further metals may be those from the list specified above or others that have not been specified above.
  • the metal or metals of the first layer differ from the metal or metals of the second layer.
  • liquid CA any and all liquids known to a person skilled in the art and deemed to be suitable for chemical removal of the first layer without removing the second layer may be used as liquid CA.
  • liquid pure substances, mixtures of multiple pure substances or mixtures of one or more pure substances and one or more inorganic or organic solvents are conceivable as liquid CA.
  • a person skilled in the art is aware of suitable liquids CA for combinations of first layer and second layer selected by the person skilled in the art.
  • compositions of the first layer compositions of the second layer, and the liquid CA are as follows:
  • Composition Composition of the of the first layer second layer Ingredients of the liquid CA (a) Niobium Platinum HF/HNO 3 /H 2 O at a volume ratio of 1:1:3; or NaOH conc. (b) Gold Platinum KCN/H 2 O (10 wt.-% KCN); or HCl/HNO 3 at a molar ratio of 3:1; or KI/I 2 /H 2 O at a molar ratio of 4:1:40 (c) Gold Niobium KCN/H 2 O (10 wt.-% KCN); or HCl/HNO 3 at a molar ratio of 3:1; or KI/I 2 /H 2 O at a molar ratio of 4:1:40 (d) Titanium Platinum HF/H 2 O 2 /H 2 O at a molar ratio of 1:1:20
  • the aforementioned ingredients of the liquid CA are present, for example, as follows: HF: 48 wt.-%, water added up to 100 wt.-%; HNO 3 : 69 wt.-%, water added up to 100 wt.-%; HCl: 36 wt.-%, water added up to 100 wt.-%; H 2 O 2 : 30 wt.-%, water added up to 100 wt.-%.
  • the chemicals specified in the table maybe procured, for example, from Merck KGaA, D-64293 Darmstadt, Germany.
  • compositions of the first layer and second layer are biocompatible.
  • the side of the second layer facing away from the first layer is provided with a material that is biocompatible.
  • the first layer may be made, at least in part, from one or more non-biocompatible materials; the same applies to coatings or devices that are arranged on the side of the first layer facing away from the second layer.
  • the side of the second layer facing away from the first layer is often referred to as the external side of the membrane or of the component.
  • a diffusion layer is arranged in the composite, between the first and second layers of the component.
  • a diffusion layer may be understood to be a region between the first and second layers that comprises metals, in particular metal atoms, of the composition of the first layer as well as metals, in particular metal atoms, of the composition of the second layer.
  • the diffusion layer has a gradient of each of the ingredients that are present in the diffusion layer.
  • the diffusion layer between the first and second layers in the composite is considered to be the region in which the concentration comprises less than 98 wt.-%, relative to the sample, of metal, in particular metal atoms, of the composition of the first layer or of metal, in particular metal atoms, of the composition of the second layer or both.
  • the presence of a diffusion layer may be tested, for example, by preparing a transverse section through the composite and by analyzing the surface of the transverse section by a combination of scanning electron microscopy and energy-dispersive x-ray analysis (also referred to as: SEM/EDX).
  • SEM/EDX scanning electron microscopy and energy-dispersive x-ray analysis
  • the first and second layers maybe connected to each other by their entire surfaces by any techniques that are known to a person skilled in the art and deemed to be suitable.
  • the first and second layers of the component are joined by means of one of the following connecting techniques: cold welding, cladding, in particular roll cladding such as cold roll cladding, warm roll cladding or explosion cladding.
  • the formation of diffusion layers may be effected, in particular, during warm roll cladding.
  • cold roll cladding and explosion cladding the formation of diffusion layers may be effected through a thermal treatment after the cladding step.
  • a combination of two or more of the aforementioned connection techniques is preferred as well.
  • the component comprises a composite made of three connected layers, in which a third layer is arranged on the side of the first layer facing away from the second layer and comprises at least one hole so that each hole of the first layer has a hole of the third layer superimposed on it.
  • the third layer comprises a thickness of more than 1 ⁇ m, of more than 2 ⁇ m, or of more than 5 ⁇ m.
  • the thickness of the third layer is in the range of 1 to 50 ⁇ m, preferably of 1 to 40 ⁇ m, or of 1 to 30 ⁇ m, or of 1 to 15 ⁇ m, or of 2 to 15 ⁇ m, or of 5 to 20 ⁇ m. From a functional point of view, the third layer should be at least thick enough such that the layer does not comprise any through-going gaps due to voids or other defects of the material.
  • the third layer may be used as the third layer.
  • the at least one metal of the third layer is selected from the same group as the at least one metal of the second layer.
  • the at least one metal of the third layer and the at least one metal of the second layer are identical.
  • the compositions of the third layer and the composition of the second layer are identical.
  • a method for producing a component comprising a composite of at least two layers that are connected to each other is a further object of the present invention.
  • the second layer has a thickness in the range of 1 to 50 ⁇ m; the first and second layers each comprises at least one metal; the third layer has a thickness of at least 1 ⁇ m; and the compositions of the first and second layers are different.
  • the method comprises at least the following process steps:
  • the component obtained according to the inventive method may contain a diffusion layer or further preferred features that have been described above with respect to the inventive component.
  • a component obtained according to the inventive method may preferably contain more than one of the preferred features described above.
  • the first and second layers are each provided, superimposed, and connected to each other while forming a composite.
  • the inventive method may be run as a continuous or as a discontinuous process.
  • the first layer and the second layer are preferably provided from a stock, e.g., a roll each, and fed to the superimposing and then to the connecting.
  • the superimposing and the connecting may proceed simultaneously in this context.
  • a discontinuous process for example, a plate of the first layer and a plate of the second layer are each first taken from a stock. Subsequently, the surfaces of the two plates are superimposed, at least partially, and the plates are then fed to the connecting.
  • the first and second layers may be connected to each other by any techniques that are known and are deemed to be suitable by a person skilled in the art.
  • the connecting is effected on the entire surface in the region in which the two layers are superimposed.
  • the connecting of the first and second layers to form a composite is effected through one of the following connecting techniques: cold welding, cladding, in particular explosion cladding or roll cladding, such as cold roll cladding or warm cladding.
  • the formation of diffusion layers may be effected, in particular, during warm roll cladding. In cold roll cladding and explosion cladding, the formation of diffusion layers may be effected through a thermal treatment after the cladding step.
  • a combination of two or more of the aforementioned connecting techniques is preferred as well.
  • step (ii) of the inventive method a coating SL is applied to at least a part of the first layer.
  • the coating SL is resistant to the liquid CA. Any layer-forming agents, which, after forming the coating, are resistant to the selected liquid CA and adhere to the first layer, may be used for the coating SL. All coatings that are known to a person skilled in the art and are deemed suitable are conceivable as coating SL. These coatings SL are often referred to as protective lacquer, covering lacquer or masking agent. A shrinkable tubing is another preferred coating SL.
  • parts of the first layer are covered by a coating SL, for example a lacquer, in particular a covering lacquer or a so-called photoresist, prior to the application of the liquid.
  • a coating SL for example a lacquer, in particular a covering lacquer or a so-called photoresist, prior to the application of the liquid.
  • a photoresist is a coating SL that is resistant to the chemicals used in the method according to the invention at least for a certain period of time, preferably permanently. Initially, a photoresist precursor is applied to the full surface or at least to part of the surface of the first layer and a lacquer is formed. Then, parts of the lacquer are exposed to radiation. The lacquer thus applied is then destroyed at the exposed sites by the irradiation and any residues of the destroyed lacquer are removed. The substrate treated according to the aforementioned alternative method is then subjected to the method according to the invention.
  • a photoresist precursor is being applied.
  • the lacquer is formed only at the sites that are being exposed to radiation. Any non-fixed and/or non-cured photoresist precursor is then removed.
  • the substrate treated according to the aforementioned alternative method is then subjected to the method according to the invention.
  • Preferred examples of a coating SL for the selected liquid CA are shown in the following table. This listing is not limiting.
  • Liquid CA 2 Coating SL a) HF/HNO 3 /H 2 O Etching resist SD 2052AL 1) b) HCl/HNO 3 /H 2 O Etching resist SD 2052AL 1) c) KCN/H 2 O Metal, e.g. platinum d) NaOH conc. Metal, e.g. platinum e) KI/I 2 /H 2 O Etching resist SD 2052AL 1) 1) available from Lackwerke Peters GmbH & Co KG, D-47906 Kempen; 2) ingredients and mixing ratios as above.
  • At least a part of the first layer, or a part of the coating SL, or a part of both is removed by mechanical or electrical processing after step (i) and before step (ii).
  • a part of the first layer or a part of the coating SL or a part of the first layer and of the coating SL applied to it may be removed by any and all methods that are known and are deemed to be suitable by a person skilled in the art.
  • Mechanical abrasion methods such as, for example, milling or spark erosion, are mentioned as methods that are preferred in this context.
  • Irradiation of the coating SL with an energy-rich radiation source, for example a laser or X-rays is a further preferred method for abrasion specifically of the coating SL.
  • step (iii) of the inventive method parts of the first layer not provided with the coating are contacted to the liquid CA in step (iii) of the inventive method so that the contacting causes at least a part of the first layer to be removed and at least one hole to be formed in the first layer.
  • the removal of the first layer at the sites made to contact the liquid CA is usually effected, as described above, by chemical processes, in particular by dissolution or oxidation processes.
  • an electrical potential is applied to the component, or to the liquid CA, or to both, in addition to removing the at least one part of the first layer.
  • a current flow induced by the electric potential may accelerate the removal of the first layer.
  • Step (iii) is completed by removing the liquid CA, for example by wiping off the liquid CA, and, if applicable, by removing the electrical potential.
  • water or an organic solvent may be used for rinsing.
  • the coating SL is removed from the remaining parts of the first layer in a step (iv) This may be done:
  • the removing is preferably effected by dissolving or cutting the shrinkable tubing and then pulling it off.
  • the composite obtained according to either one of the steps (iii) or (iv) is split-up into multiple parts in a step (v), whereby multiple components are thus obtained. If the component is not split-up into multiple parts, one component is obtained.
  • a method for producing a component comprising a composite of at least three layers that are connected to each other is a further object of the present invention, in which the second layer has a thickness in the range of 1 to 50 ⁇ m; the first layer, the second layer, and the third layer each comprise at least one metal; the third layer has a thickness of at least 1 ⁇ m; the compositions of the first and second layers are different; and the compositions of the first and third layers are different.
  • the method comprises at least the following process steps:
  • Objects that have been described above in the context of the inventive component and of the inventive method specified earlier may be used according to the invention and preferably, if applicable, as first and second layers.
  • the component obtained according to the present inventive method may contain one or more diffusion layer(s) or further preferred features that have been described above with respect to the inventive component or with respect to the inventive method specified earlier.
  • a component obtained according to the inventive method may preferably contain more than one of the preferred features described above.
  • the third layer may be used as the third layer.
  • the at least one metal of the third layer is selected from the same group as the at least one metal of the second layer.
  • the at least one metal of the third layer and the at least one metal of the second layer are identical.
  • the composition of the third layer and the composition of the second layer are identical.
  • the third layer, the first layer, and the second layer each are provided, superimposed, and connected to each other while forming a composite.
  • the inventive method may be run as a continuous or as a discontinuous process.
  • the third layer, the first layer, and the second layer are preferably provided from a stock, e.g., a roll each, and fed to the superimposing and then to the connecting.
  • the superimposing and the connecting may proceed simultaneously in this context.
  • a plate of the third layer, a plate of the first layer, and a plate of the second layer each are first taken from a stock. Subsequently, the surfaces of the three plates are superimposed, at least partially, and the plates are then fed to the connecting.
  • the third layer, the first layer, and the second layer may be connected to each other by any and all techniques that are known and deemed to be suitable by a person skilled in the art.
  • the connecting is effected on the entire surface in the region in which at least two of the three layers are superimposed.
  • the connecting of the three layers to form a composite is effected through one of the following connecting techniques: cold welding, cladding, in particular explosion cladding or roll cladding, such as cold roll cladding or warm cladding.
  • the formation of diffusion layers may be effected, in particular, during warm roll cladding. In cold roll cladding and explosion cladding, the formation of diffusion layers may be effected through a thermal treatment after the cladding step.
  • At least a part of the third layer is removed by mechanical or electrical processing after step (i) and before step (ii).
  • the removing of a part of the third layer may be effected according to any and all methods that are known and deemed to be suitable by a person skilled in the art.
  • Mechanical abrasion methods such as, for example, milling or spark erosion, are preferably selected methods.
  • step (iii) of the inventive method parts of the first layer not provided with the third layer are contacted to a liquid CA in step (iii) of the inventive method.
  • the contacting causes at least a part of the first layer to be removed and at least one hole to be formed in the first layer.
  • the removal of the first layer at the sites made to contact the liquid CA is usually effected by chemical processes, in particular by dissolution or oxidation processes.
  • an electrical potential is additionally applied to the component or to the liquid CA or to both.
  • a current flow induced by the electric potential may support the removal of the first layer.
  • Step (iii) is completed by removing the liquid CA, for example, by wiping off the liquid CA, and, if applicable, by removing the electrical potential.
  • water or an organic solvent may be used for rinsing.
  • the third layer is removed from the first layer at least partially, but preferably completely, in a step (iv). This is done mechanically, for example by means of a polishing process, a grinding process or a milling process.
  • step (iv) is not implemented.
  • the third layer remains on the first layer.
  • the composite obtained according to step (iii) or (iv) is split-up into multiple parts in a step (v) to obtain multiple components. If the component is not split-up into multiple parts, one component is obtained.
  • the first layer, the second layer and, if applicable, the third layer are provided in the form of tubes.
  • the superimposing is effected by inserting the tubes into each other in the desired sequence; the tubes may comprise one or more of the features described above with respect to the three layers.
  • the composite made of at least two or at least three layers that are connected to each other is preferably attained by drawing the tubes. Drawing the tubes is associated with a reduction of the cross-section of the tubes, which leads to an intimate composite being obtained. Pertinent details are known to a person skilled in the art.
  • a component comprising a composite that is obtained according to either one of the two inventive methods described above is another object of the present invention.
  • a component comprising a composite as described above that is obtained according to either one of the inventive methods described above is another object of the present invention.
  • a device comprising the inventive component described above comprising a composite is another object of the present invention.
  • this device is selected from an implant, in particular a cardiac pacemaker, a probe, a pressure measuring device, in particular for measuring pressures in a human or animal body, e.g., a blood pressure measuring device.
  • a method for producing a device for use in a living body which comprises the inventive component described above is another object of the present invention.
  • this device is selected from an implant, in particular a cardiac pacemaker, a probe, a pressure measuring device for measuring pressures in a human or animal body, e.g., a blood pressure measuring device.
  • FIG. 1 shows a process for producing a composite 6 from two layers 2 and 3 .
  • This process may be run continuously or discontinuously.
  • step a a first layer 2 and a second layer 3 are provided and superimposed.
  • step b the two layers 2 and 3 are connected intimately by guiding them between rollers 11 . The rolling reduces the thickness of the layers 2 and 3 (not shown here).
  • the resulting composite 6 is shown in c.
  • FIG. 2 shows a process for producing a composite 6 made of three layers 2 , 3 , and 8 .
  • This process may also be run continuously or discontinuously.
  • step a a third layer 8 , a first layer 2 , a second layer 3 are provided and superimposed.
  • step b the three layers 8 , 2 , and 3 are connected intimately by guiding them between rollers 11 . The rolling reduces the thickness of the layers 8 , 2 , and 3 (not shown here).
  • the resulting composite 6 is shown in c.
  • FIG. 3 shows a process for producing a component comprising a support layer and a membrane.
  • Image a shows a composite 6 made of two layers 2 and 3 (not shown). This is coated with a coating SL 5 .
  • a hole 7 is formed in the coating SL 5 by removing a part of the coating SL 5 .
  • the coating SL 5 now comprises a hole 7 , which is subsequently immersed in a bath 13 of a liquid 12 .
  • Image c shows an arrangement in which the composite 6 with the hole 7 in the coating SL 5 is being treated with a liquid CA 12 in a bath 13 . Afterwards, the liquid CA is removed, e.g., by rinsing.
  • Image d shows the treated composite 6 which comprises a hole 7 that is present both in layer 5 and in layer 6 .
  • Image e shows the composite 6 after the coating SL 5 has been removed.
  • FIG. 4 is a flowchart corresponding to the process depicted in FIG. 3 .
  • FIG. 5 shows another process for producing a component comprising a support layer and a membrane.
  • the composite consists of three layers, whereby the third layer 8 is resistant to the liquid CA.
  • Image a shows the composite 6 made of three layers 2 , 3 (both not shown), and 8 .
  • a hole 7 is formed in the composite 6 .
  • image b the composite 6 comprises a hole 7 , which is subsequently immersed in a bath 13 containing a liquid 12 .
  • Image c shows an arrangement in which the composite 6 with the hole 7 in layer 8 is being treated with a liquid CA 12 in a bath 13 .
  • the liquid CA is removed, e.g., by rinsing.
  • Image d shows the treated composite 6 which comprises a hole 7 that is present both in layer 8 and in layer 6 .
  • layer 8 is removed.
  • Image e shows the composite 6 after layer 8 has been removed.
  • FIG. 6 is a flowchart corresponding to the process depicted in FIG. 5 .
  • FIG. 7 shows examples of components according to embodiments of the invention, each comprising a composite made of two layers.
  • Line 1 represents a cross-section each and line 2 represents a top view onto each component.
  • FIG. 7 a depicts a circular component with a planar membrane (second layer 3 ) and a cylindrical ring made of the first layer 2 .
  • FIG. 7 b depicts a rectangular component with a planar membrane (second layer 3 ) and a rectangular frame made of the first layer 2 .
  • FIG. 7 c shows a cylindrical component with a domed membrane as part of the second layer 3 that forms an internal cylinder and with a ring made of the first layer 2 forming an external cylinder.
  • FIG. 8 is a diagram of a device 10 (shown dashed) comprising a component 1 with a composite made of a first layer 2 and a second layer 3 .
  • a cold-clad Nb/Pt sheet consisting of a niobium layer with a thickness of 194 ⁇ m and a platinum layer with a thickness of 6 ⁇ m (thickness specifications refer to the cold-clad Nb/Pt sheet; Nb/Pt sheet available from Vincent Metal Products, Inc., 33 Plan Way, Unit 3C, Warwick, R.I. 02886, USA) was cut into rectangular plates having a surface area of 8 mm ⁇ 8 mm. The plate was coated appropriately on the niobium surface and on the narrow sides (these correspond to the surfaces along the thickness of the sheet plates) using etch resist SD2052 AL cover lacquer (available from Lackwerke Peters GmbH & Co.
  • the lacquer coating of the plate was removed by immersing the plate in a bath of diluted sodium hydroxide. Then, deionized water was used to rinse again. Subsequently, this was rinsed again with ethanol.
  • the treated plate comprised a continuous platinum layer and a niobium layer, in which the niobium layer had a hole that extended from the niobium surface of the plate to the platinum surface and was situated in the location in which the field with no lacquer coating previously had been.

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SG11201504892RA (en) 2015-07-30
US20200093381A1 (en) 2020-03-26

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