WO2003012887A1 - Procede de formation de film multicouche - Google Patents

Procede de formation de film multicouche Download PDF

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Publication number
WO2003012887A1
WO2003012887A1 PCT/JP2002/006806 JP0206806W WO03012887A1 WO 2003012887 A1 WO2003012887 A1 WO 2003012887A1 JP 0206806 W JP0206806 W JP 0206806W WO 03012887 A1 WO03012887 A1 WO 03012887A1
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WO
WIPO (PCT)
Prior art keywords
film
forming
conductive
multilayer film
multilayer
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.)
Ceased
Application number
PCT/JP2002/006806
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English (en)
Japanese (ja)
Inventor
Masaharu Kawachi
Masahito Yoshizawa
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Japan Science and Technology Agency
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Japan Science and Technology Corp
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Filing date
Publication date
Application filed by Japan Science and Technology Corp filed Critical Japan Science and Technology Corp
Publication of WO2003012887A1 publication Critical patent/WO2003012887A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • 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
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • C23C28/3455—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
    • 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
    • H10N60/0268—Manufacture or treatment of devices comprising copper oxide
    • H10N60/0296—Processes for depositing or forming copper oxide superconductor layers
    • H10N60/0324—Processes for depositing or forming copper oxide superconductor layers from a solution

Definitions

  • the present invention relates to a method for forming a multilayer film, and more particularly to a method for forming a superconducting film having excellent superconducting properties.
  • the superconducting paste is printed on the substrate surface by a method such as screen printing, and then the obtained superconducting paste layer is heat-treated.
  • the present inventors As a method for forming a superconducting film on the surface of a substrate having an arbitrary shape other than a planar shape such as a curved surface, the present inventors have previously proposed a method using electrophoretic deposition. We proposed a method of coating conductor particles and heat-treating them.
  • the superconducting film is formed on a relatively inexpensive ceramic substrate such as an aluminum substrate or a quartz glass tube by the electrophoretic deposition method.
  • the superconducting film is formed by the electrophoretic deposition.
  • the atoms constituting the base and the atoms constituting the superconductor fine particles are separated. There was a problem that they would interdiffuse, thereby deteriorating the superconducting properties of the superconducting film.
  • the present invention has been made under such circumstances, and has as its object to provide a method for forming a multilayer film that does not cause mutual diffusion with a substrate.
  • a step of forming a diffusion prevention film on a substrate surface a step of electrophoretically depositing or electrodepositing a metal on the diffusion prevention film, and a heat treatment of the substrate to sinter the metal,
  • a method for forming a multilayer film including a step of forming a metal film is provided.
  • a step of forming a diffusion prevention film on the surface of the substrate and a step of electrophoretically depositing or depositing a high-temperature superconductor and a high-temperature superconductor precursor on the diffusion prevention film , And a heat treatment of the substrate to sinter the high-temperature superconductor and the high-temperature superconductor precursor to form a superconducting film.
  • one selected from the group consisting of zirconium stabilized zirconia and ceramic oxide can be used as the diffusion preventing film.
  • the particle diameter of the fine particles constituting the diffusion prevention film is preferably about 0.2 ⁇ m to 5 ⁇ m.
  • the diffusion preventing film can be formed by the electrophoretic deposition method or the coating method.
  • a first conductive film is formed on a substrate surface, and the diffusion prevention film is formed on the first conductive film. It can be formed by electrophoresis.
  • a second conductive film can be formed on the diffusion prevention film, and a superconductive film can be formed on the second conductive film.
  • the conductive film can be formed by forming a conductive paste layer on the surface of the substrate and heat-treating the conductive paste layer.
  • the conductive film can be formed by plating a conductive material or by vacuum deposition of a conductive material.
  • the conductive film can contain silver as a main component.
  • the superconducting film can be formed in a pattern.
  • a superconducting wiring can be formed.
  • the method for forming a multilayer film of the present invention configured as described above, mutual diffusion between the substrate and the superconducting film is prevented, and the superconducting film having excellent superconducting properties is obtained.
  • the film can be easily formed.
  • a metal in particular, a high-temperature superconductor and a high-temperature superconductor precursor are deposited on a substrate surface by electrophoretic deposition or electrodeposition via a diffusion prevention film, It is characterized in that a multilayer film is formed by heat treatment.
  • a ceramic substrate As a substrate on which a multilayer film is formed, a ceramic substrate can be used. Since this ceramic base material is subjected to heat treatment, it has heat resistance up to about 100 ° C. and is relatively stable with respect to the multilayer film. Many This and Do which Joukenwomitasuko and is rather desirable close to the thermal expansion coefficient of the layer film, Anore Mi Na (A 1 2 O 3), and the this to use such oxide Ma Gune Shi U beam (M g O) I can do it. Among them, aluminum can be used favorably in terms of availability.
  • the thickness of the diffusion prevention film formed on the substrate is preferably from 10111 to 100111. If it is less than 10 ⁇ , it is difficult to prevent interdiffusion, and if it exceeds 20 ⁇ , the superconducting film may be peeled off.
  • the diffusion prevention film has not only a diffusion prevention effect but also a buffer film effect of preventing peeling due to a difference in the coefficient of thermal expansion between the substrate and a film formed thereon.
  • the diffusion prevention film can be formed by the electrophoretic deposition method or the coating method.However, when the anti-diffusion film is formed by the electrophoretic deposition method, the underlayer must be conductive, and therefore, the diffusion prevention film must A conductive material must be applied. Silver is preferred as the conductive material.
  • Examples of the method for applying a conductive material to the substrate surface include a method in which a conductive paste is applied and heat-treated, and a method in which the conductive material is deposited or deposited by vapor deposition. Can be listed.
  • silver paste examples include 904 T, FSP-306 ⁇ , and ⁇ -106 D (trade name: manufactured by Tanaka Kikinzoku Co., Ltd.).
  • examples of the film formed on the substrate via the diffusion preventing film include a semiconductor, a semiconductor precursor, a high-temperature superconductor, and a high-temperature superconductor precursor.
  • the conductor precursor is not particularly limited, for example, YB a 2 C u 3 0 7 particles, YB a 2 C u 4 ⁇ 8 particles or the like Yore, Ru this and can.
  • the base since the high-temperature superconductor and / or the high-temperature superconductor precursor are deposited by electrophoretic deposition or electrodeposition, the base must be conductive. Therefore, it is necessary to apply a conductive material to the surface of the diffusion prevention film.
  • a conductive material silver is preferable as a metal that does not react with the superconductor.
  • the method of depositing the conductive material on the surface of the base is as described above.
  • the thickness of the conductive material is preferably about 0.3 ⁇ m to about 10 ⁇ m.
  • electrophoretic deposition is used to deposit high-temperature superconductors
  • electrodeposition is used to deposit high-temperature superconductor precursors.
  • a substrate is placed in a solvent in which high-temperature superconducting fine particles are dispersed, an anode is placed in opposition to the applied conductive material, and a voltage is applied between the electrodes using the conductive material as a cathode.
  • a solvent in which high-temperature superconducting fine particles are dispersed
  • an anode is placed in opposition to the applied conductive material
  • a voltage is applied between the electrodes using the conductive material as a cathode.
  • concentration of the fine particles in the solvent is usually 30 mg to 40 mg / cm 3, and the concentration of iodine is 0.4 mg / cm ⁇ ”.
  • Electrophoretic electrodeposition conditions can be the same as those commonly used.
  • the voltage is 40 to 500 V
  • the time is 10 to 60 seconds.
  • Electrophoretic deposition involves applying a magnetic field parallel to the electrophoresis direction. It is desirable to carry out in a state where it was done.
  • the substrate is cylindrical
  • the magnetic field may be rotated about the axis of the cylindrical substrate.
  • the magnetic field is desirably about 1 T to about 10 T.
  • a substrate is placed in a solution in which a high-temperature superconductor precursor is deposited by electrolysis, an anode is placed in opposition to the deposited conductive material, and the conductive material is used as a cathode. This is done by applying a voltage between the electrodes.
  • a solution in which dimethyl sulfoxide (DMS 0) is used as a solvent and a nitrate or the like of an element constituting the high-temperature superconductor precursor is dissolved may be used. I can do it.
  • the conditions for electrodeposition may be those used for normal use.
  • the voltage is -2.5 to 14 V and the time is 3 to 5 minutes with respect to the reference electrode.
  • the electrophoretically or electrodeposited high-temperature superconductor and Z or high-temperature superconductor precursor are then heat-treated and sintered.
  • the high-temperature superconductor precursor fine particles become high-temperature superconductive fine particles.
  • the heat treatment temperature is preferably 880-920 ° C, and the heat treatment atmosphere is preferably oxygen.
  • the superconducting film in pattern and form superconducting wiring You can do this.
  • an underlying diffusion prevention film or a conductive film is formed in a pattern, and a superconducting film is formed by electrophoresis or electrodeposition on the film. What is necessary is just to form a film pattern.
  • the superconducting film may be etched using a resist pattern or the like formed by photolithography as a mask. .
  • a cylindrical ceramic substrate having an inner diameter of 18 mm, an outer diameter of 21 mm, and a length of 80 mm, made of aluminum having a purity of 97% was prepared.
  • a silver paste was formed to a film thickness of 50 ⁇ on the outer surface of the cylindrical ceramic base material by screen printing.
  • As the silver paste FSP-306 0 (manufactured by Tanaka Kikinzoku Co., Ltd.) was used.
  • this cylindrical ceramic substrate was heat-treated at 600 ° C. for 1 hour in the air.
  • the volatile components of the silver paste evaporated, and the silver components adhered to the outer surface of the cylindrical ceramic substrate.
  • a silver film having a thickness of 10 m was formed.
  • yttrium-stabilized zirconium was electrophoretically deposited on the silver pattern to form a 50 ⁇ -thick diffusion prevention film.
  • a silver paste was formed to a thickness of 100 ⁇ on the diffusion prevention film.
  • As the silver paste FSP-306 0 (manufactured by Tanaka Kikinzoku Co., Ltd.) was used.
  • a heat treatment was performed in the same manner as described above to form a silver film having a thickness of 10 ⁇ m.
  • the high-temperature superconducting fine particles migrate on the silver film formed on the outer surface of the cylindrical ceramic base material. Electrodeposited.
  • the cylindrical ceramic base material was heat-treated with a predetermined heat history, and the high-temperature superconducting fine particles were sintered.
  • the heat treatment atmosphere is oxygen.
  • the heat history was first raised to 300 ° C and maintained for 1 hour, then raised to 800 ° C at a heating rate of 500 ° C / h, then increased to 1 ° C.
  • the temperature was raised to 900 ° C at a temperature increase rate of 00 ° CZh, where it was maintained for 1 hour.
  • the temperature was first lowered to 500 ° C at a temperature reduction rate of 60 ° C / h, maintained for 5 hours, and then cooled to room temperature at a temperature reduction rate of 60 ° C.
  • the conductive film is formed by applying silver paste to the cylindrical ceramic base material.
  • a conductive material may be applied by sticking or vapor deposition.
  • the present invention is not limited to this, and a high-temperature superconducting precursor, which becomes high-temperature superconducting fine particles by heat treatment. On may be electrodeposited. Alternatively, a mixture of high-temperature superconducting fine particles and high-temperature superconducting precursor ion can be electrophoretically deposited.
  • This example shows an example in which high-temperature superconducting fine particles are applied not by electrophoretic deposition but by electrodeposition.
  • a silver film having a thickness of 0.3 ⁇ m is formed on a three-dimensional (for example, an inner diameter of 18 mm, an outer diameter of 21 mm, and a length of 80 mm) alumina base material surface by vacuum evaporation. Formed.
  • a silver film was formed to a thickness of 0.3 ⁇ m on the cerium oxide film by vacuum evaporation, and a high-temperature superconductor was deposited.
  • YBa 2 Cu 3 O 7 was used as the high-temperature superconductor. Electrodeposition was performed as follows.
  • the deposited film is heat-treated at 300 ° C to volatilize organic substances, and inserted into an electric furnace that has been heated to 150 ° C in advance for 1 hour. After heating for 1 minute, the heating of the electric furnace was stopped, and cooling was performed at a cooling speed of 50 ° C / hour. During these heat treatments, oxygen gas was supplied to the electric furnace.
  • the conductive film is formed by vapor deposition on an aluminum base material.
  • the present invention is not limited to this, and the coating method of silver paste is not limited to this.
  • a conductive material may be applied by a key.
  • the method of forming a multilayer film according to the present invention can be applied to various devices using a superconductor.
  • Such devices include, for example, a quantum interference magnetometer using a high-temperature superconducting film, a magnetic detection coil and an input coil of the quantum interference magnetometer, and a high-frequency signal transmission line (story). And my cross-trip line).
  • various substances such as curved surfaces can be obtained by electrophoretically depositing or depositing various substances on the surface of a substrate via a diffusion prevention film.
  • a thin film can be easily and inexpensively formed on the surface of a substrate having such a shape without causing mutual diffusion between the substrate and the substrate.
  • the multilayer film can be formed on a desired substrate, for example, a three-dimensional substrate, the application of the device using the multilayer film, particularly, the superconducting device, is further expanded. As can be expected, the contribution of the present invention in the field of superconductivity is extremely high.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Superconductor Devices And Manufacturing Methods Thereof (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

La présente invention concerne un procédé de formation de film multicouche qui consiste à former un film qui empêche la diffusion sur la surface d'un substrat, à électodéposer avec migration ou à électodéposer un supraconducteur haute température et/ou un précurseur de supraconducteur haute température et à thermotraiter le substrat de façon à fritter le supraconducteur haute température et/ou le précurseur de supraconducteur haute température et former ainsi un film à supraconduction.
PCT/JP2002/006806 2001-07-30 2002-07-04 Procede de formation de film multicouche Ceased WO2003012887A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2001228921A JP2003046151A (ja) 2001-07-30 2001-07-30 多層膜の形成方法
JP2001-228921 2001-07-30

Publications (1)

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WO2003012887A1 true WO2003012887A1 (fr) 2003-02-13

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PCT/JP2002/006806 Ceased WO2003012887A1 (fr) 2001-07-30 2002-07-04 Procede de formation de film multicouche

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WO (1) WO2003012887A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01247600A (ja) * 1988-03-30 1989-10-03 Fujikura Ltd 酸化物超電導材の製造方法
EP0631333A1 (fr) * 1993-06-22 1994-12-28 General Atomics Procédé de fabrication bandes multicouches de supraconducteur à haute température et produits fabriqués par ce procédé
WO1999007004A1 (fr) * 1997-07-29 1999-02-11 American Superconductor Corporation Supraconducteurs filamentaires, uniformes, fins

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01247600A (ja) * 1988-03-30 1989-10-03 Fujikura Ltd 酸化物超電導材の製造方法
EP0631333A1 (fr) * 1993-06-22 1994-12-28 General Atomics Procédé de fabrication bandes multicouches de supraconducteur à haute température et produits fabriqués par ce procédé
WO1999007004A1 (fr) * 1997-07-29 1999-02-11 American Superconductor Corporation Supraconducteurs filamentaires, uniformes, fins

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHU C.T. ET AL.: "Fabrication of YBa2Cu2O7-gamma superconducting coatings by electrophoretic deposition", APPL. PHYS. LETT., vol. 55, no. 5, 31 July 1989 (1989-07-31), pages 492 - 494, XP000080841 *

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