EP4118252A1 - Procédé de fabrication d'un revêtement pour une pièce principale, et élément fonctionnel comprenant une pièce principale avec un revêtement - Google Patents

Procédé de fabrication d'un revêtement pour une pièce principale, et élément fonctionnel comprenant une pièce principale avec un revêtement

Info

Publication number
EP4118252A1
EP4118252A1 EP21713587.0A EP21713587A EP4118252A1 EP 4118252 A1 EP4118252 A1 EP 4118252A1 EP 21713587 A EP21713587 A EP 21713587A EP 4118252 A1 EP4118252 A1 EP 4118252A1
Authority
EP
European Patent Office
Prior art keywords
coating
target
base body
sputtering
particles
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.)
Pending
Application number
EP21713587.0A
Other languages
German (de)
English (en)
Inventor
Nils Schäfer
Lambert Alff
Márton MAJOR
Stefan Petzold
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.)
Technische Universitaet Darmstadt
Original Assignee
Technische Universitaet Darmstadt
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 Technische Universitaet Darmstadt filed Critical Technische Universitaet Darmstadt
Publication of EP4118252A1 publication Critical patent/EP4118252A1/fr
Pending 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/046—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/541—Heating or cooling of the substrates
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/548—Controlling the composition
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/01—Manufacture or treatment
    • H10N60/0184—Manufacture or treatment of devices comprising intermetallic compounds of type A-15, e.g. Nb3Sn

Definitions

  • the invention relates to a method for producing a coating of a base body with a coating made of a first material and a second material, a first target made of the first material and a second target made of the second material being arranged in a vacuum chamber, one to be coated
  • the base body is arranged in the vacuum chamber, a sputtering gas being introduced into the vacuum chamber and wherein, during a sputtering process with sputtering gas ions, first target particles are detached from the first target and attached to the base body as coating particles, and second target particles are detached from the second target and applied as coating particles are attached to the base body.
  • a base body Numerous different methods are known from practice with which an often comparatively thin coating can be produced on a base body.
  • a process known as sputtering atoms are released from a solid body known as a target by bombarding them with high-energy ions, so that the released target atoms pass into the gas phase and are deposited on nearby surfaces.
  • the base body to be coated is arranged in the vicinity of a target during a sputtering process, so that the target atoms released from the target are preferably deposited on a surface of the base body and form the desired coating on the base body.
  • A15 phase group of substances two or three different metals usually form an intermetallic phase with an A15 structure. Some of the A15 phases have advantageous superconducting properties, so that these A15 phases are suitable for numerous areas of application in which superconducting properties are advantageous or necessary.
  • the A15 phases usually have a composition with the empirical formula A3B, where A is a transition metal and B is a metallic main group element of the periodic table. Component B can also be a mixture of different metallic main group elements.
  • A15 phases such as NbsGe or NbsSn enable the construction of superconducting magnets or cables with magnetic flux densities of more than 10T.
  • a functional element with superconducting properties from a base body which is coated with a suitable coating of an A15 phase, such as NbsSn.
  • a superconducting cavity of a particle accelerator which is usually made of high-purity niobium
  • a functional element with a base body made of copper and a coating made of NbsSn could be replaced by a functional element with a base body made of copper and a coating made of NbsSn.
  • the base body can be made of copper, for example.
  • Such a functional element with a base body made of copper could be significantly more cost-effective than a corresponding functional element made of high-purity niobium.
  • the production of the coating of the base body from NbsSn is complex and leads to restrictions in the use of such a functional element.
  • such a coating can be produced on a base body, for example made of copper, by a number of successive sputtering processes, with thin layers, for example of niobium and tin, being applied to the base body alternately with the aid of sputtering . Subsequently, the base body with the layer sequence of niobium and tin applied to it must be heated so that the heating of the layers caused diffusion of the individual atoms of the layers and the desired material NbsSn is formed.
  • NbsSn requires heat treatment at high temperatures of about one thousand Degrees Celsius and more is required, with the resulting coating often being inhomogeneous even under advantageous process conditions and also various compounds and phases being created, so that the superconducting properties of the coating produced in this way are impaired.
  • atoms from the base body also diffuse into the coating and accumulate in the coating. Diffusion of atoms from the base body into the coating can be reduced with a diffusion barrier made of a suitable material, the diffusion barrier being designed as a thin layer and arranged between the base body and the coating made of NbsSn.
  • this diffusion barrier usually hampers heat removal from the coating into the base body, which is advantageous or even necessary for many applications, and thereby impairs the properties and possible uses of such a functional element.
  • this object is achieved in that a first sputter rate for the first target and a second sputter rate for the second target are specified during the sputtering process in such a way that the Coating is produced with a desired stoichiometric ratio of the first target particles to the second target particles, and that the base body is heated to a coating temperature of less than six hundred degrees Celsius during the sputtering process with a heating device.
  • the first target particles and the second target particles initially accumulate randomly on the base body at the respective location where they hit the surface of the base body. It has been shown that by heating the base body to a coating temperature of less than six hundred degrees Celsius, the first target particles and second target particles deposited on the surface of the base body have sufficient mobility due to the thermal energy to form the desired A15 phase and in the The result is a homogeneous coating with a phase-pure crystal lattice to grow on the base body. Since the first target particles and the second target particles impinging on the base body are comparatively mobile on the surface, heating to less than six hundred degrees Celsius is sufficient to form the desired A15 phase from the first target particles and the second target particles on the surface.
  • the base body can consist of different materials which are advantageous for different functional elements or areas of application of the relevant functional elements.
  • a material of the base body which is advantageous for many areas of application is, for example, copper. If the base body made of copper is heated to less than six hundred degrees Celsius, there is no significant diffusion of the copper material into the coating that is deposited on the surface of the base body. If the base body is heated to less than six hundred degrees Celsius, it is therefore not necessary to arrange a diffusion barrier made of a suitable material between the base body and the coating applied to it, with which the undesired diffusion of copper into the coating is reduced or, if possible, largely suppressed can.
  • the first material is a first metal and that the second material is a second metal or a mixture of metals.
  • the metal mixture can contain, for example, two or more different metals which each form a compound with the first metal.
  • the respective connections can then be combined with one another and combine to form a homogeneous crystal lattice according to the respective proportions.
  • the second material is a second metal, by suitably specifying the process parameters, it can be achieved that only a single compound of the first metal with the second metal is created, so that a phase-pure crystal lattice is formed.
  • the first target particles from the first material and the second target particles from the second material form an A15 phase.
  • the material of the first target and the material of the second target can be selected so that the first target particles and second target particles released from the first target and from the second target form an A15 phase which has particularly advantageous properties for certain areas of application.
  • the first sputter rate and the second sputter rate are specified so that the stoichiometric ratio required for the formation of the A15 phase of the first target particle is given to the second target particle.
  • a stoichiometric ratio of 75% to 25% is advantageous.
  • Functional elements with a base body for example made of copper or a material with comparable thermal conductivity, can thus be provided with a superconducting coating, so that the functional element produced in this way can be used advantageously for numerous applications because of the superconducting properties of the coating.
  • At least one further third target is arranged in the vacuum chamber during the sputtering process, and that for each further third target a third sputter rate for the accumulation of third target particles in the coating is specified so that the coating is generated with a desired stoichiometric ratio of the third target particles to the first and second target particles.
  • a second target with a metal mixture instead of a second target with a metal mixture, a second target with a second metal and additionally a third target with a further third material can be used, so that all three targets consist of pure metals or elements.
  • An individual sputter rate can be specified for all three targets, so that complex stoichiometric ratios can also be specified and achieved for the desired coating.
  • a coating can be produced in which NbsSn and NbsGe are combined to form a homogeneous crystal lattice. It is preferably provided that the base body is heated to a coating temperature between two hundred degrees Celsius and six hundred degrees Celsius and particularly preferably to a coating temperature between four hundred degrees Celsius and five hundred degrees Celsius during the sputtering process. It has been shown that for many material combinations of two metals that form an A15 phase, a coating temperature between two hundred degrees Celsius and six hundred degrees Celsius, or in many cases between four hundred degrees Celsius and five hundred degrees Celsius, is sufficient to achieve that on the surface of the base body impinging first target particles and second target particles to allow sufficient mobility to form the desired A15 phase with a phase-pure crystal lattice.
  • magnetron sputtering In order to improve the efficiency of the sputtering process, provision is optionally made for magnetron sputtering to be carried out during the sputtering process.
  • an additional magnetic field is generated in the vicinity of the first target and in the vicinity of the second target, through which the electron density in an area above that for the dissolving out of target surfaces provided for target particles is increased and, due to the increased ionization of the sputtering gas in this area, the sputtering rate of the target material in question and thus the layer growth of the coating are increased.
  • a person skilled in the art is aware of the options available for effectively carrying out magnetron sputtering and optimizing individual process parameters.
  • the base body to be treated in an adhesion increase step preceding the sputtering process in order to strengthen the adhesion of the coating to a surface of the base body to be coated.
  • the surface of the base body can be treated chemically or physically, for example by an etching process or by irradiation with ion beams or with laser light.
  • a region of the base body adjoining the surface of the base body can be changed or partially or completely removed.
  • chemical or physical properties of the surface can be changed in such a way that the subsequently applied coating adheres much more strongly to the surface. It is also possible to apply an adhesive layer that enhances the adhesive effect on the surface of the base body.
  • the adhesive layer can serve as an adhesion promoter.
  • the base body can also be cooled during the adhesion increase step or heated to an adhesion step temperature that corresponds to the coating temperature or is lower, but is higher than room temperature. If necessary, the liability increase step can be used for
  • the surface of a base body provided for the coating can be changed in such a way that a coating is possible in the first place.
  • a simple control of the individual components that are used and operated during a sputtering process to carry out the method according to the invention can be achieved according to one embodiment of the inventive concept in that a predetermined sputtering power ratio is specified for the first sputter rate and the sputter rate.
  • the sputtering power ratio can, for example, be determined in advance by means of separate examinations as a function of the target materials used.
  • the sputtering power ratio as the ratio of the first sputtering rate to the second sputtering rate can also be determined in advance as a function of the coating temperature specified in an individual case and specified for carrying out the sputtering process.
  • the first sputtering rate and the second sputtering rate can be changed during a coating process in order, for example, to accelerate or slow down the layer growth as a function of the increasing distance from the surface of the base body, with the fixedly specified sputtering power ratio the stoichiometric ratio of the first target particles relative to the second target particles is kept constant and a homogeneous formation of an A15 phase with a phase-pure crystal lattice is promoted.
  • the first metal is niobium and the second metal is tin or a mixture of two or more elements with more than 50 mol percent tin.
  • an intermetallic chemical compound and particularly advantageously also the A15 phase NbsSn can be produced during the coating process.
  • the coating material NbsSn produced in this way has very advantageous superconducting properties and is also suitable for applications that require large currents and magnetic fields, as is the case, for example, with particle accelerators.
  • niobium instead of a combination of exclusively niobium and tin, or instead of an A15 phase NbsSn, a coating of niobium on the one hand and a mixture of tin and another element such as gallium or aluminum on the other hand is produced .
  • the respective proportions can be predetermined by the mixture used for the second material in such a way that a coating with advantageous properties is formed.
  • a coating described above with a layer thickness between 200 nm and 5 ⁇ m is advantageous.
  • the layer thickness can be precisely specified with the described sputtering process as a function of the respective requirements.
  • the coating is produced with a layer sequence of at least two layers of a coating material, with a separating layer of a different and non-superconducting material being arranged between adjacent layers of a superconducting coating material.
  • the separating layer allows two layers of the Coating material are separated from one another in order to enable or strengthen particularly advantageous properties of the coating by such a layer sequence.
  • a sequence of two or more thin layers of a superconducting coating material, which are separated from one another by a separating layer made of a non-superconducting material, can improve the practical electrical conduction properties and thus the use of the base body coated in this way as a functional element, for example in particle accelerators or made possible or favored in the case of superconducting cables.
  • the separating layer can consist of an insulator material such as, for example, plastic and can be applied using conventional coating processes to a layer made of a superconducting coating material, which in turn has been applied by sputtering. It is also conceivable that the separating layer is made of an electrically conductive material such as a metal or a metallic compound, which, however, at least under conditions in which the
  • Coating material has superconducting properties, has no superconducting properties.
  • a separating layer made of a metallic material can also be applied by a sputtering process.
  • a separating layer made of a metallic material usually has a high thermal conductivity, as a result of which a very advantageous thermal conductivity of the coated base body can be achieved in some applications.
  • Refractory metals such as tantalum, Molybdenum or tungsten are also viewed as advantageous materials for a separating layer due to their high thermal conductivity. It is also conceivable that the material of the separating layer corresponds to the material from which the base body is made.
  • a ceramic layer and preferably a layer of aluminum nitride ceramic is applied as the separating layer.
  • Aluminum nitride ceramics have a particularly high thermal conductivity and, in contrast to metals, are poorly electrically conductive.
  • a layer of aluminum nitride ceramic can also be applied by a sputtering process to a base body previously coated with a superconducting coating material. Since only the targets have to be exchanged for this purpose, a coating consisting of several layers with several layers of superconducting coating material and with one or more layers of aluminum nitride ceramic can be produced with the sputtering method according to the invention almost without interruption and without major changeover times.
  • the first target and the second target are arranged in a recess or in an externally accessible cavity of a base body and that an inner wall of the base body delimiting the recess or the cavity is coated in the sputtering process . Since the inner wall of the recess or cavity to be coated surrounds the target, almost all of the target particles released from the target during the sputtering process are deposited on the inner surface of the base body to be coated and form the desired coating. As a result, the sputtering process can be carried out particularly effectively and economically.
  • the base body on the one hand and the first and second target on the other hand are displaced relative to one another during the sputtering process.
  • the base body surrounding the targets can be set in a rotational movement while the sputtering process is being carried out.
  • the targets are fixed to a rotatably or movably mounted target holder and the target holder is displaced relative to the base body.
  • both the base body and the targets can be displaced at the same time in order, for example, to be able to implement complex movement sequences relative to one another as simply as possible. This enables a very short process duration for the sputtering process and a very uniform formation of the sputtered coating. Areas of the inner wall of the recess or of the not intended for a coating Cavities can be covered before the sputtering process is carried out.
  • the invention also relates to a functional element with a base body with a coating of an A15 phase.
  • a functional element can have a base body and a coating made of an A15 phase, such as NbsSn, applied to it.
  • a functional element of this type could serve, for example, as a replacement for a functional element which is manufactured entirely from a uniform, but cost-intensive material.
  • a practical example of such a functional element is a cavity of a particle accelerator. Such cavities are usually made of high-purity niobium, which results in high material and manufacturing costs. It has been shown that for many applications and in particular for cavities of a particle accelerator, functional elements are also suitable in which a base body with a coating of a superconducting A15 phase and in particular with a coating NbsSn are suitable. However, the previously known manufacturing processes for such functional elements are costly and unsatisfactory as a result.
  • this object is achieved in that the coating is produced directly on a surface of the base body using a previously described sputtering method.
  • the arrangement of a diffusion barrier between the base body and the coating can be dispensed with.
  • a suitable diffusion barrier not only has the desired property of preventing the undesired diffusion of particles from the base body into the coating during the production of the coating or during any subsequent heat treatment that may be required, but also provides a comparatively effective, but represent an undesirable barrier for heat transport.
  • the base body is made of copper.
  • Copper is a comparatively inexpensive material that has high electrical conductivity and high thermal conductivity, which is advantageous for many areas of application of such functional elements. Copper can also be machined in a simple manner, so that inexpensive production of the base body is also favored in the case of complex shapes.
  • an inner wall of a recess or a cavity in the base body it can be advantageous for an inner wall of a recess or a cavity in the base body to be coated with a superconducting coating. It is therefore optionally provided that the coating partially or completely covers an inner wall of a recess or a cavity in the base body.
  • the functional element has a cavity for an accelerator.
  • a cavity that can be used as a functional element in a particle accelerator usually has a rotationally symmetrical shape with a continuous cavity.
  • This cavity can be coated with a superconducting coating according to the invention.
  • Such a cavity can be produced particularly inexpensively and has the superconducting or electrically conductive and heat-conductive properties required for use in a particle accelerator.
  • the base body coated according to the invention relates to superconducting motors or generators, it being possible for the functional element to be a superconducting cable or a superconducting line element for magnet coils.
  • the functional element for example, copper foils or copper strips with a coating according to the invention can be provided with superconducting properties, for example with NbsSn, in order then to be used as superconducting magnet coils in superconducting motors or generators that can be used very efficiently.
  • the copper foils or copper strips or corresponding functional elements with a base body made of another suitable material can be shaped into the desired shape using conventional methods.
  • the superconducting coating can be applied in a simple manner using the sputtering method according to the invention.
  • FIG. 1 shows a schematic structure of a device with which the method according to the invention for producing a coating can be carried out
  • FIG. 2 shows a schematic representation of measurement results of an X-ray diffraction measurement of a coating with NbsSn produced at a coating temperature of four hundred and thirty-five degrees Celsius, the intensity of the scattered X-rays being shown over the diffraction angle two theta,
  • FIG. 3 Measured values of the electrical resistance of the coating measured in FIG. 2 in a temperature range between twelve degrees Kelvin and twenty degrees Kelvin, normalized to the electrical resistance at twenty degrees Kelvin,
  • FIG. 4 shows a schematic representation of a partial area of a functional element according to the invention with a base body and a coating arranged directly on a surface of the base body
  • FIG. 5 shows a schematic sectional view of a partial area of the coated base body as in FIG. 4, an area of the base body adjoining the surface being treated and modified in an adhesion increase step in order to increase the adhesion effect for the coating applied thereon,
  • FIG. 6 shows a schematic sectional view of a partial area of the coated base body as in FIGS. 4 and 5, the coating consisting of a sequence of layers, and FIG.
  • FIG. 7 shows a schematic sectional view through a cavity of a base body in which two targets are arranged while the sputtering process is being carried out.
  • FIG. 1 shows an example of a device 1 with which a method according to the invention for coating a base body 2 with a coating from an A15 phase can be carried out.
  • a coating chamber 3 in which a vacuum can be generated, a first target 4 made of a first target material and a second target 5 made of a second target material are arranged next to one another.
  • the target material of the first target 4 is a first metal, namely niobium (Nb).
  • the target material of the second target 5 is a second metal, namely tin (Sn).
  • the base body 2 made of copper is arranged opposite the two targets 4, 5, with a surface 6 of the base body 2 facing the two targets 4, 5 being to be coated.
  • the base body 2 can be opened from a rear side 7 with a heating device 8 during a sputtering process a predefinable coating temperature can be heated.
  • the coating temperature specified for the coating process in question is 435 ° C.
  • the coating chamber 3 has an inlet 9 for a suitable sputtering gas, which can be, for example, a noble gas and preferably argon.
  • a suitable sputtering gas which can be, for example, a noble gas and preferably argon.
  • the sputtering gas can already have been ionized beforehand or else in the
  • Coating chamber 3 are ionized.
  • the two targets 4, 5 and the base body 2 can each be brought to an individually specifiable electrical potential, so that an electrical field is formed in the coating chamber 3, which accelerates positively charged sputtering gas ions 16 in the direction of the two targets 4, 5.
  • the sputtering gas ions 16 can be accelerated sufficiently on the way to the first target 4 or to the second target 5 in order to release first target particles 10 when they strike the first target 4, or to detach them when they strike the second target 5 to detach second target particles 11.
  • the respective sputtering rates of the first target 4 and the second target 5 can be influenced and specified by suitably specifying the respective electrical potentials and thus the potential differences which the sputter gas ions 16 pass through on the way to the first or second target 4, 5.
  • the first and second target particles 10, 11 released by the bombardment with sputtering gas ions 16 are deposited on the surface 6 of the base body 2, among other things.
  • Sputter gas ions 16, used sputter gas particles or target particles 10, 11 emanating from the first target 4 or from can pass through an outlet 12 the second target 5 have been dissolved out and are not deposited on a surface, are discharged from the coating chamber 3.
  • a magnetic field is generated in an area between the two targets 4, 5 and the base body 2 in the immediate vicinity of the two targets 4, 5, through which free electrons in an area above a respective surface 14, 15 of the two targets 4, 5 are concentrated.
  • the density of the sputtering gas ions 16 striking the respective target 4, 5 and thus the sputtering rates for the first target 4 and for the second target 5 can be influenced.
  • the first target particles 10 released from the first target 4 by the sputtering gas ions 16 and the second target particles 11 released from the second target 5 are deposited on the surface 6 of the base body 2 heated with the heating device 8. Due to the thermal energy of the heated base body 2, sufficient energy is transferred to the adhering target particles 10, 11 so that they can migrate along the surface 6 and react to the desired A15 phase.
  • the first target particles 10 made of niobium and deposited on the surface 6 react with the second target particles 11 made of tin to form the intermetallic phase NbsSn. This creates a very homogeneous coating with a phase-pure crystal lattice.
  • X-ray diffraction measurement one with the previous one described method in the exemplified device 1 shown coating produced from NbsSn.
  • the intensity I of the X-ray radiation scattered on the coating is shown in any unit as a function of the respective diffraction angle 2Q over a range of the diffraction angle 2Q between 30 ° and 90 °.
  • NbsSn characteristic diffraction peaks of NbsSn
  • Other possible compounds of niobium and tin, such as NbSn2 or Nb 2 Sn 5 on the other hand, as well as pure niobium or pure tin, could not be detected.
  • the measurement result accordingly confirms that the desired coating of the base body 2 with the superconducting material NbsSn with a very phase-pure crystal lattice could be produced with the method according to the invention.
  • the electrical resistance R is shown as a function of the temperature T, the electrical resistance R being normalized to the measured resistance value R (20K) at a temperature T of 20K. It can be seen that the coating has superconducting properties and a negligibly low normalized resistance R / R (20K) at a temperature T below about 15.3 K. The transition temperature above which the superconducting property disappears is around 16.3 K and is close to the highest transition temperature of 18.3 K ever proven for a bulk material or for a solid body with comparatively large dimensions for this coating material. This measurement also proves that a high-quality coating of NbsSn with a phase-pure crystal lattice could be produced with the method according to the invention.
  • FIG. 4 a section of a functional element 17 according to the invention is shown as an example.
  • a coating 18 made of NbsSn is applied directly to the surface 6 of the base body 2, which in the exemplary embodiment shown consists of copper.
  • no separate diffusion barrier is arranged between the surface 6 of the base body 2 and the coating 18. This promotes very effective heat transfer from the base body 2 into the coating 18 and vice versa, which is advantageous for numerous applications of such functional elements 17.
  • the surface 6 of the base body 2 to be coated was treated by an etching process in an adhesion increase step preceding the sputtering process, and an area 19 of the base body 2 adjoining the surface 6 was thereby changed in such a way that the subsequently applied to the surface 6 Coating 18 adheres more strongly.
  • the coating 18 has a layer sequence which consists of two layers 20, 21 made of a superconducting coating material, between which a separating layer 22 made of a non-superconducting metal is arranged.
  • the two layers 20, 21 have each been applied using the sputtering method according to the invention.
  • the separating layer 22 can also be applied using a sputtering method or using any conventional coating method.
  • the outer surfaces, which are then covered by a layer 20, 21, 22 applied thereon, can each be treated in an adhesion increase step and the adhesion effect for the subsequently applied layer 20, 21, 22 can thereby be improved.
  • FIG. 7 An exemplary embodiment for a base body 2 with a cavity 23 is shown only schematically in FIG. 7, an inner wall 24 of the cavity 23 in the base body 2 being provided with the coating 18 during the sputtering process.
  • the first target 4 and the second target 5 and the associated components of the magnetic field generating device 13 are arranged in the cavity 23 of the base body 2 during the sputtering process.
  • a relative movement indicated only by way of example with an arrow 25, can be brought about between the base body 2 and the first and second targets 4, 5 arranged in the cavity 23 of the base body 2.
  • the base body 2 can rotate around the first and second target 4, 5, which are fixed on a target holder (not shown) that protrudes into the cavity 23 of the base body 2, in order to achieve a coating 18 of the inner wall 24 of the cavity 23 that is as uniform as possible as quickly as possible to be produced in the base body 2.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un revêtement pour une pièce principale (2) avec un revêtement. Une première cible (4) constituée d'un premier métal et une seconde cible (5) constituée d'un second métal sont disposées dans une chambre à vide. Une partie principale (2) à revêtir est disposée dans la chambre à vide et est chauffée à une température de revêtement inférieure à 600 °C par un dispositif de chauffage (8). Pendant un processus de pulvérisation cathodique utilisant des ions de gaz de pulvérisation (16), des premières particules cibles (10) sont libérées de la première cible (4), et des secondes particules cibles (11) sont libérées de la seconde cible (5), lesdites particules se fixant à la pièce principale (2) en tant que particules de revêtement. Pendant le processus de pulvérisation cathodique, un premier taux de pulvérisation est spécifié pour la première cible (4), et un second taux de pulvérisation est spécifié pour la seconde cible (5) de telle sorte que pendant le processus de pulvérisation cathodique, le revêtement est formé en une phase A15 ayant un rapport stœchiométrique voulu des premières particules cibles (10) aux secondes particules cibles (11). Un élément fonctionnel présente une pièce principale (2) et un revêtement en Nb3Sn appliqué directement sur la surface (6) de la pièce principale (2).
EP21713587.0A 2020-03-13 2021-03-12 Procédé de fabrication d'un revêtement pour une pièce principale, et élément fonctionnel comprenant une pièce principale avec un revêtement Pending EP4118252A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102020107059.4A DE102020107059A1 (de) 2020-03-13 2020-03-13 Verfahren zum Herstellen einer Beschichtung eines Grundkörpers und Funktionselement mit einem Grundkörper mit einer Beschichtung
PCT/EP2021/056396 WO2021180953A1 (fr) 2020-03-13 2021-03-12 Procédé de fabrication d'un revêtement pour une pièce principale, et élément fonctionnel comprenant une pièce principale avec un revêtement

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EP4118252A1 true EP4118252A1 (fr) 2023-01-18

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EP21713587.0A Pending EP4118252A1 (fr) 2020-03-13 2021-03-12 Procédé de fabrication d'un revêtement pour une pièce principale, et élément fonctionnel comprenant une pièce principale avec un revêtement

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US (1) US20230100972A1 (fr)
EP (1) EP4118252A1 (fr)
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Publication number Priority date Publication date Assignee Title
US3576670A (en) * 1969-02-19 1971-04-27 Gulf Energy & Environ Systems Method for making a superconducting material
DE2948735C2 (de) 1979-12-04 1982-06-24 Siemens AG, 1000 Berlin und 8000 München Verfahren zu kontinuierlichen Herstellung von Niob-Germanium-Schichten auf einem Trägerkörper
JPS60251198A (ja) 1984-05-28 1985-12-11 Nippon Telegr & Teleph Corp <Ntt> 超伝導膜の製造方法
US5089455A (en) * 1989-08-11 1992-02-18 Corning Incorporated Thin flexible sintered structures
CN101286544B (zh) * 2007-04-10 2013-01-30 中国科学院物理研究所 一种用于超导器件的超导多层膜及其制备方法
US10347473B2 (en) 2009-09-24 2019-07-09 The United States Of America, As Represented By The Secretary Of The Navy Synthesis of high-purity bulk copper indium gallium selenide materials
US9169548B1 (en) 2010-10-19 2015-10-27 Apollo Precision Fujian Limited Photovoltaic cell with copper poor CIGS absorber layer and method of making thereof
PT2791384T (pt) * 2011-12-15 2016-07-15 Council Scient Ind Res Revestimento seletivo solar melhorado tendo elevada estabilidade térmica e um processo para a sua preparação
US20170107636A1 (en) * 2015-07-08 2017-04-20 Fermi Research Alliance, Llc Synthesis of superconducting nb-sn
FR3063675A1 (fr) * 2017-03-10 2018-09-14 Lvmh Swiss Manufactures Sa Materiau comprenant une couche mince d'un alliage comportant du titane et de l'or et procede d'obtention d'un tel materiau

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DE102020107059A1 (de) 2021-09-16
US20230100972A1 (en) 2023-03-30

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