US20030056928A1 - Method for producing composite material and composite material produced thereby - Google Patents

Method for producing composite material and composite material produced thereby Download PDF

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US20030056928A1
US20030056928A1 US09/926,486 US92648601A US2003056928A1 US 20030056928 A1 US20030056928 A1 US 20030056928A1 US 92648601 A US92648601 A US 92648601A US 2003056928 A1 US2003056928 A1 US 2003056928A1
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composite material
base material
bulk body
dispersion
metal
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Takashi Kubota
Hiroshi Watanabe
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Mitsui Mining and Smelting Co Ltd
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Assigned to MITSUI MINING & SMELTING CO., LTD. reassignment MITSUI MINING & SMELTING CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KUBOTA, TAKASHI, WATANABE, HIROSHI
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    • 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
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • C23C14/0005—Separation of the coating from 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
    • 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
    • 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
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • 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
    • 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
    • C23C14/3464—Sputtering using more than one target

Definitions

  • the present invention relates to a manufacturing method for a composite material comprising two or more metals or nonmetals and compounds thereof and, more particularly, to a manufacturing method in which a dispersion material can be dispersed very homogeneously into a base material of the composite material independently of the composition of the composite material.
  • composite materials comprising metals or nonmetals or compounds thereof have been used in a wide variety of applications as structural materials for automobile parts, aircraft parts, etc., electrode materials, target materials for film formation, and the like.
  • the composite material is manufactured by dispersing metals or nonmetals or compounds thereof different from a base material into the base material to control material properties so that material properties suitable for each application can be realized.
  • nonmetal used in this specification includes hydrogen, boron, carbon, silicon, nitrogen, phosphorous, and the like, and is used as a wide concept including antimony, bismuth, etc. which are what we call a semimetal.
  • the compo-casting process and the powder metallurgy process are known.
  • a metal which is used as a base material
  • nonmetal particles which are used as a dispersion material
  • This process is effective in the case where the composite material is manufactured by using nonmetal particles having poor wettability with respect to the melted metal of base material.
  • the composite material is manufactured in a semi-melting state so as to prevent separation of nonmetal particles from base metal.
  • the fusion-casting process is generally used.
  • both of a base material and a dispersion material are metals, and they have properties of a low melting point metal and a high melting point metal, respectively, it is very difficult to manufacture such a metal-metal composite material by, for example, the vacuum fusion process.
  • a composite material obtained by the conventional manufacturing method is described in more detail by taking a sputtering target material as an example.
  • a sputtering target material As an example, when the wiring for a liquid crystal display or a semiconductor integrated circuit is formed, the wiring technology using a sputtering method using a target material of composite material has been employed.
  • an aluminum film which has high heat resistance and low electrical resistance, is typically used, and a target material of composite material using aluminum as a base material is used to form the aluminum film.
  • the aluminum film used as the wiring for a liquid crystal display or a semiconductor integrated circuit for example, a target material of composite material in which aluminum is used as a base material and carbon and a group IVa metal such as titanium are dispersed is used.
  • a target material of composite material made of aluminum is used, the wiring having high heat resistance and low electrical resistance can be formed, so that breakage of wiring caused by stress can be prevented.
  • the target material of composite material made of aluminum is naturally required to have a composition capable of forming a film meeting the requirements for the wiring characteristics.
  • the target material is required to have less defects such as a cavity and a void, to have a high density, and to entrain less gas that forms impurities.
  • a dispersion material can be dispersed into a base material in the conventional manufacturing method for a composite material, however the dispersibility is insufficient, and an internal defect and entrance of impurities occur in the bulk body.
  • the conventional composite material has many drawbacks to be improved.
  • the target material considering the case where a composite material used for other applications as a structural material for an automobile part, aircraft part, etc. or an electrode material is manufactured, in the conventional manufacturing method, it is very difficult to manufacture a composite material having various compositions generally by one manufacturing method.
  • the present invention has been made in view of the above situation, and accordingly an object thereof is to provide a manufacturing method for a composite material comprising two or more metals or nonmetals and compounds thereof, in which a dispersion material can be dispersed very homogeneously into a base material of the composite material, and which method can be used generally independently of the composition of the composite material as compared with the conventional manufacturing method.
  • the present invention provides, as a first invention, a manufacturing method for a composite material in which a metal or a nonmetal or a compound thereof is used as abase material, and at least one kind of metals or nonmetals or compounds thereof different from the base material is dispersed as a dispersion material, wherein a raw material for base material comprising a metal or a nonmetal or a compound thereof for forming the base material and at least one of raw materials for dispersion material comprising metals or nonmetals or compounds thereof for forming the dispersion material are evaporated simultaneously or alternately, and the evaporated particles are deposited on a substrate to form a bulk body.
  • the raw material for base material for forming the base material and the raw material for dispersion material for forming the dispersion material are made evaporated particles by what we call the physical vapor deposition process (PVD process), and the evaporated particles are deposited on the substrate to form the bulk body.
  • PVD process physical vapor deposition process
  • the dispersion material is dispersed very homogeneously into the base material, so that various composite materials can be manufactured easily independently of the properties of each raw material. That is to say, even a composite material of a combination of a high melting point metal and a low melting point metal can also be manufactured easily.
  • the sputtering method or the vacuum deposition method in the physical vapor deposition process is preferably used.
  • the reason for this is that in these methods, evaporated particles are produced from each raw material at relatively high rate, so that a bulk body having a predetermined volume can be formed easily.
  • the sputtering method or the vacuum deposition method is applied in the first invention, since the raw material is evaporated in an atmosphere of inert gas such as argon or in a vacuum atmosphere, even an easily oxidizable raw material can be used. Therefore, the quantity of oxygen entering into the manufactured bulk body can be controlled, and the entrance of gas and other impurities can be avoided to the utmost. Further, a bulk body of composite material having far less internal defects can be manufactured.
  • the raw material for base material and the raw material for dispersion material can be evaporated simultaneously or alternately.
  • the evaporated particles of the raw material for base material and the raw material for dispersion material are deposited at random.
  • a composite material in which the dispersion material is dispersed homogeneously into the base material is manufactured by controlling the deposit layer of the base material and the dispersion material on the order of angstrom.
  • the sputtering method is preferably used for the evaporation of raw materials
  • the inventors invented a manufacturing method for a composite material in which a metal or a nonmetal or a compound thereof is used as a base material, and at least one kind of metals or nonmetals or compounds thereof different from the base material is dispersed as a dispersion material, wherein a raw material for evaporation comprising a metal or a nonmetal or a compound thereof for forming the base material or a metal or a nonmetal or a compound thereof for forming the dispersion material is evaporated in an atmosphere of any one of a hydrocarbon gas, oxygen gas, and nitrogen gas, and the evaporated particles are deposited on a substrate to form a bulk body.
  • This second invention is based on the physical vapor deposition process (PVD process) or the chemical vapor deposition process (CVD process).
  • PVD process physical vapor deposition process
  • CVD process chemical vapor deposition process
  • any one of a hydrocarbon gas, oxygen gas, and nitrogen gas is selected, so that a composite material in which carbides, nitrides, or oxides are dispersed as a dispersion material very homogeneously into the base material can be manufactured.
  • the sputtering method and the vacuum deposition method in the physical vapor deposition process or an activated deposition method in the chemical vapor deposition process is preferably used.
  • the hydrocarbon gas used in the second invention is not subject to any special restriction as to the composition thereof if it can be decomposed into carbon and hydrogen at the time of sputtering or deposition.
  • methane, ethane, and acetylene gas can be cited.
  • an inert gas such as argon, the evaporation efficiency of raw material can be controlled.
  • a raw material for evaporation comprising a metal or a nonmetal or a compound thereof for forming the base material
  • a raw material for evaporation containing a metal or a nonmetal or a compound thereof for forming the dispersion material in addition to the base material may be used.
  • a raw material for evaporation comprising copper for forming the base material and silicon for forming the dispersion material is used to produce evaporated particles in nitrogen gas by using the sputtering method, and the particles are deposited on the substrate, so that silicon and nitrogen react with each other to yield stable silicon nitride.
  • a composite material in which silicon nitride, which is a dispersion material, is dispersed very homogeneously into copper, which is a base material can be manufactured.
  • a raw material for evaporation comprising copper as the base material and aluminum as the dispersion material are used to produce evaporated particles in oxygen gas by using the sputtering method, and the particles are deposited on the substrate, so that aluminum and oxygen react with each other to yield stable aluminum oxide. Therefore, a composite material in which aluminum oxide, which is a dispersion material, is dispersed very homogeneously into copper, which is a base material, can be manufactured.
  • a composite material that has not been realized by the conventional manufacturing method that is, a composite material in which even a dispersion material having poor wettability with respect to the base material is dispersed very homogeneously into the base material can be manufactured.
  • the atmosphere in which the raw material is evaporated By controlling the atmosphere in which the raw material is evaporated, the entrance of impurities can be restrained to the utmost, and a bulk body having far less internal defects can be manufactured.
  • the sputtering method is preferably used for the evaporation of raw material.
  • the composite material obtained by the manufacturing methods of the first and second inventions of the present invention described above is a bulk body deposited and formed on the substrate. It is not difficult for this bulk body to be handled as a simple body, unlike what we call a film. By separating the bulk body from the substrate, the bulk body has a volume of a degree such that the bulk body itself can be handled as it is.
  • the bulk body separated from the substrate by the manufacturing methods of the first and second inventions can be used as it is for each application, for example, as a target material.
  • the bulk body obtained by the manufacturing methods of the first and second inventions is melted, mixed, and formed by casting together with the raw material for base material comprising a metal or a nonmetal or a compound thereof for forming the base material, by which the concentration of dispersion material can be controlled.
  • the obtained composite material of bulk body is structurally ideal in that the dispersion material is dispersed very homogeneously into the base material.
  • these two manufacturing methods are based on the vapor phase epitaxy method, so that in the case of the bulk body having a larger volume, manufacturing must be performed for a long period of time, and also it is difficult to obtain a complicated bulk body.
  • the bulk body obtained by these two methods is melted, mixed, and formed by casting together with the raw material for base material to control the concentration of dispersion material, by which a composite material of a larger bulk body is manufactured. If a mold of a predetermined shape is used at the time of casting, a composite material of a complex shape can be obtained easily.
  • the bulk body obtained by the first and second inventions and the raw material for base material are melted, mixed, and formed by casting, a phenomenon that the dispersion material is separated from the base material may possibly be caused as in the conventional manufacturing method.
  • the bulk body is formed in a state in which the base material and the dispersion material are dispersed into each other very finely, that is, the bulk body is formed in a state in which the dispersion material has high wettability with respect to the base material. Therefore, even if the bulk body is melted together with the raw material for base material, the dispersion material is not separated from the base material.
  • the composite material obtained by melting, mixing, and casting the bulk body and the raw material for base material is in a state in which the dispersion material is dispersed very homogeneously into the base material.
  • a composite material is manufactured by melting the bulk body and the raw material for base material in this way, when the bulk body is formed, the quantity of dispersion material or the quantity of raw material for base material to be added is controlled in advance, by which the composition of the finally obtained composite material can be controlled easily.
  • the temperature for melting the bulk body and the raw material for base material may be determined appropriately according to the composition of composite material. Basically, the melting may be performed at a temperature in the range from the melting point to the evaporating temperature of the bulk body. In effect, the temperature may be controlled so that the bulk body becomes in a fully flowing state and the raw material for base material and the bulk body can be mixed homogeneously with each other.
  • the atmosphere when the melting is performed is not subject to any special restriction.
  • the melting is performed preferably in a vacuum atmosphere or in an atmosphere of inert gas such as argon gas.
  • the casting is preferably performed under a rapid solidification condition. This is because if the casting is performed under a rapid solidification condition, the crystal structure of composite material is made fine, and the dispersion material is dispersed into the base material homogeneously and finely.
  • the crystal structure thereof can be controlled by rolling or heat treatment.
  • the finally manufactured composite material must have properties suitable for each application.
  • a composite material having properties suitable for each application, for example, high strength properties can be realized by controlling the crystal structure thereof by means of rolling or heat treatment. In this case, both of rolling and heat treatment may be applied, or only either of them may be applied.
  • the evaporated particles be deposited while the substrate is rotated.
  • the deposition of evaporated particles proceeds homogeneously at all locations on the surface of the rotating substrate, so that as compared with the case where the evaporated particles are deposited on the stationary substrate, a bulk body with a more uniform composition and a uniform thickness can be formed.
  • the substrate on which the evaporated particles are deposited is preferably made of the same material as the base material.
  • deposited particles deposit in conformity with the substrate, so that a homogeneous crystal structure can be obtained easily.
  • the material of the substrate is the same as the base material, the formed bulk body can be melted without being peeled off from the substrate, so that the manufacturing process can be simplified.
  • a composite material suitable for each application can be manufactured generally independently of the composition thereof, the dispersion material is dispersed very homogeneously into the base material, the entrance of impurities is restrained, and a composite material of bulk body having no internal defect such as a cavity can be obtained. Therefore, the composite material obtained by the manufacturing method in accordance with the present invention can be practically used appropriately for each application, and can be used very suitably as a structural material for an automobile part, aircraft part, etc., an electrode material, or a target material for film formation.
  • the composite material obtained by the manufacturing method in accordance with the present invention in which aluminum is used as the base material and carbon is used as the dispersion material, is very suitable as a target material.
  • an aluminum film is effectively used for the wiring for a liquid crystal display or a semiconductor integrated circuit.
  • a so-called mosaic-like target material in which when an aluminum film containing carbon is formed by the sputtering method, a chip etc. comprising carbon or silicon is embedded directly in an aluminum metal material has been known (Japanese Patent Laid-Open No. 2-292821).
  • FIG. 1 is a schematic view showing a case where a bulk body is formed on a stationary substrate by the sputtering method
  • FIG. 2 is a schematic view showing a case where a bulk body is formed on a stationary substrate by the vacuum deposition method
  • FIG. 3 is a schematic view showing a case where a bulk body is formed on a rotating substrate by the sputtering method
  • FIG. 4 is a schematic view showing a case where a bulk body is formed on a rotating substrate by using both of the sputtering method and the vacuum deposition method;
  • FIG. 5 is a micrograph of a cross section of a composite material having been subjected to water-cooled casting in Example 1;
  • FIG. 6 is a schematic view showing a case where a bulk body is formed on a stationary substrate by introducing hydrocarbon gas using the sputtering method.
  • FIG. 7 is a schematic view showing a case where a bulk body is formed on a stationary substrate by introducing hydrocarbon gas using the deposition method.
  • a first embodiment described below relates to a manufacturing method of the before-mentioned first invention, and a second embodiment relates to a manufacturing method of the before-mentioned second invention.
  • the first embodiment relates to a manufacturing method in which a bulk body is formed by evaporating a raw material for base material and a raw material for dispersion material using the sputtering method or the vacuum deposition method.
  • FIGS. 1 to 4 are schematic views showing various manufacturing methods of the first embodiment.
  • FIG. 1 shows a method in which a metal raw material used as a base material and a nonmetal raw material used as a dispersion material are evaporated by the sputtering method and are deposited on a plate-shaped stationary substrate.
  • a plate-shaped stationary substrate 2 is installed in a chamber 1 , and a metal target 4 for base material and a nonmetal target 5 for dispersion material are provided on a respective substrate 3 so as to face the stationary substrate 2 .
  • the stationary substrate 2 and the targets 4 and 5 are connected to a not-shown electric power source.
  • the stationary substrate 2 is formed of a metal for base material.
  • FIG. 1 shows a case where two targets of the metal target 4 for base material and the target 5 for dispersion material are used, a plurality of targets can be provided appropriately according to the composition of the intended composite material.
  • An inert gas for example, argon gas is introduced in the chamber 1 , and the pressure of the gas is controlled to a predetermined value. Thereafter, a predetermined voltage is applied between the metal target 4 for base material and the stationary substrate 2 and between the nonmetal target 5 for dispersion material and the stationary substrate 2 to cause a sputtering phenomenon, by which a metal for base material and a nonmetal for dispersion material are evaporated and deposited on the stationary substrate 2 .
  • the voltage may be applied to cause the sputtering phenomenon simultaneously on both of the targets 4 and 5 , or maybe applied to cause the sputtering phenomenon alternately.
  • a DC 2-pole sputtering system is shown in FIG. 1, what we call a high-frequency sputtering system or what we call a magnetron sputtering system may be used.
  • a composite material of a bulk body 6 is formed on the stationary substrate 2 .
  • the bulk body 6 is removed from the stationary substrate 2 by grinding or etching the stationary substrate 2 .
  • the simple bulk body 6 can be used in a variety of applications as a structural material, electrode material, or target material.
  • this bulk body 6 can be used without being subjected to treatment, it can also be used by being subjected to rolling or heat treatment if necessary to control the crystal structure.
  • the bulk body 6 and the stationary substrate 2 are heated and melted together with a base material metal having been prepared separately.
  • the composition of the finally obtained composite material that is, the concentration of the dispersion material can be determined arbitrarily.
  • the materials are heated to a predetermined temperature and are melted into a flowable state to some degree, they are agitated sufficiently to be mixed homogeneously, and then are formed by casting under a rapid solidification condition, by which a composite material having the intended composition and shape can be obtained. Further, if necessary, the composite material can be rolled or heat-treated to control the crystal structure.
  • FIG. 2 shows a method in which a metal raw material used as a base material and a nonmetal raw material used as a dispersion material are evaporated by the vacuum deposition method and are deposited on a plate-shaped stationary substrate.
  • the plate-shaped stationary substrate 2 is installed in the chamber 1 , and a metal deposition source 8 for base material and a nonmetal deposition source 9 for dispersion material are provided on a respective deposition crucible 7 so as to face the stationary substrate 2 .
  • Both of the deposition sources 8 and 9 are connected to an electric power source, not shown.
  • the deposition source if being configured so that a rod-like source can be supplied continuously, is effective in achieving mass production of composite material.
  • the stationary substrate 2 is formed of a metal for base material. In the case of the vacuum deposition method described with reference to FIG. 2, as in the case of FIG. 1, many deposition sources can be provided appropriately according to the composition of the intended composite material.
  • the chamber 1 is decompressed to a predetermined pressure to produce a vacuum atmosphere.
  • the metal deposition source 8 for base material and the nonmetal deposition source 9 for dispersion material are heated by causing electric current to flow, and thereby a metal for base material and a nonmetal for dispersion material are evaporated from the deposition sources 8 and 9 , respectively, and are deposited on the stationary substrate 2 .
  • a composite material of the bulk body 6 is formed on the stationary substrate 2 .
  • the bulk body 6 is used as a single body, or it can be used as a composite material in which the concentration of dispersion material has been controlled by melting, mixing, and casting the bulk body 6 together with the metal for base material. Also, if necessary, the composite material can be rolled or heat-treated to control the crystal structure.
  • FIG. 3 shows a case where a composite material of a bulk body is manufactured on a rotating substrate by the sputtering method.
  • a cylindrical rotating substrate 10 is installed in the chamber 1 , and the metal target 4 for base material and the nonmetal target 5 for dispersion material are provided on the respective substrate 3 so as to face the rotating substrate 10 and to be at right angles to each other.
  • argon gas is introduced in the chamber 1 , and a predetermined voltage is applied by means of a not-shown electric power source to perform sputtering, by which a metal for base material and a nonmetal for dispersion material are deposited on the side face of the cylindrical rotating substrate 10 being rotated to form a bulk body 6 ′.
  • a metal for base material and a nonmetal for dispersion material are deposited on the side face of the cylindrical rotating substrate 10 being rotated to form a bulk body 6 ′.
  • the microstructure of the bulk body 6 ′ is made such that the metal for base material and the nonmetal for dispersion material are deposited in layers on the order of angstrom.
  • the metal for base material and the nonmetal for dispersion material have a homogeneous composition, and the dispersion material is dispersed very finely into the base material.
  • the bulk body 6 ′ formed on the rotating substrate can be used without being subjected to treatment as a composite material for each application, or it can be used as a composite material in which the concentration of dispersion material has been controlled by melting the bulk body 6 ′ together with the metal for base material. Further, the composite material can be rolled or heat-treated to control the crystal structure.
  • FIG. 3 shows a case where two targets are used, three or more targets can be provided as a matter of course around the rotating substrate according to the composition of the intended composite material. The above description with reference to FIG.
  • FIG. 4 shows a case where a composite material of a bulk body is manufactured on a rotating substrate through use of both the sputtering method and the deposition method.
  • the cylindrical rotating substrate 10 is installed in the chamber 1 , and the metal target 4 for base material is provided on the substrate 3 and the nonmetal deposition source 9 for dispersion material is provided in the deposition crucible 7 so that they face the rotating substrate 10 and are at right angles to each other.
  • a metal for base material is evaporated by sputtering, and on the other hand, a nonmetal for dispersion material is heated by causing an electric current to flow until the temperature thereof reaches a temperature at which the vapor pressure of the nonmetal substance is higher than the pressure in the chamber 1 , whereby the nonmetal for dispersion material is evaporated.
  • the metal for base material and the nonmetal for dispersion material are deposited on the side face of the rotating substrate 10 to form the bulk body 6 ′.
  • a composite material having the same construction as that described with reference to FIG. 3 can be obtained.
  • the bulk body 6 ′ can be handled in the same way as described with reference to FIG. 1, so that the explanation is omitted.
  • Example 1 represents a case where an aluminum-carbon composite material is manufactured by the use of the rotating substrate shown in FIG. 3 by the sputtering method.
  • Two kinds of materials of aluminum (purity: 99.999%) used as a metal target for base material and carbon (purity: 99.9%) used as a nonmetal target for dispersion material were prepared.
  • Each of the targets measures 127 mm long, 279.4 mm wide, and 10 mm thick.
  • a sputtering apparatus a 3-cathode magnetron sputtering type apparatus was used, and two cathodes of the three cathodes were used.
  • an octagonal cylindrical rotating substrate which was produced by connecting the lengthwise sides of eight stainless steel plates each measuring 279 mm long and 80 mm wide to each other, was prepared.
  • Aluminum foil (purity: 99.999%) with a thickness of 12 ⁇ m was wound around the side face of the rotating substrate, and aluminum and carbon were deposited on the aluminum foil.
  • the sputtering conditions were as follows: Argon gas was introduced in the chamber, the sputtering pressure was 0.87 Pa, the applied electric power was 12 kw (24.8 W/cm 2 ) for the aluminum target and 4 kW (8.3 w/cm 2 ) for the carbon target, and the rotational speed of the rotating substrate was 30 rpm. Sputtering was performed for about 30 hours to form a bulk body with a thickness of 0.6 mm on the side face of the rotating substrate.
  • the formed bulk body had a cross-sectional structure in which an aluminum layer with a thickness of about 0.3 ⁇ m and a carbon layer with a thickness of about 0.01 ⁇ m are laminated, the thicknesses being converted from the film forming rate.
  • the carbon concentration in the bulk body was shown to be 2.6% by weight (5.6% by atomic weight) by analysis.
  • FIG. 5 shows an observation result for a dispersed state of Al—C(Al 4 C 3 ) phase for the aluminum-carbon composite material obtained in Example 1.
  • a black portion represents the Al—C(Al 4 C 3 ) phase.
  • the aluminum-carbon (0.7% by weight) composite material formed by casting as described above was formed into a sputtering target material, and an aluminum film was formed by using this target material.
  • the aluminum film forming conditions were as follows: a DC magnetron sputtering apparatus was used, the sputtering pressure was 0.333 Pa (2.5 mTorr), and the applied electric power was 3 Watt/cm 2 . Under these conditions, a film with a thickness of about 3000 angstroms was formed on a glass substrate.
  • the sputtering time required for forming a film with a thickness of about 3000 angstroms was about 100 seconds. After the film of 3000 angstroms was formed, the glass substrate was replaced, and a film was further formed.
  • hillock which represents heat resistance properties, was investigated for the film formed at the first time, the film formed when about 20 hours of sputtering time in total had elapsed, and the film formed when about 40 hours of sputtering time in total had elapsed.
  • a hillock in this specification means a bump-like protrusion produced on the surface of film when the glass substrate with film is heat-treated under vacuum at a temperature of 300° C. for a given period of time. As a result, it was verified that a hillock scarcely occurred on each film independently of the total sputtering time.
  • Comparative Example 1 uses the compo-casting method. Two kilograms of aluminum (purity: 99.999%) was heated to about 700° C. in a carbon crucible. After the aluminum was melted once and was then cooled to about 640° C., by which the aluminum was made in a semi-melted state (solid-liquid coexisting state). In this state, 15 g of carbon powder with an average particle size of 150 ⁇ m was put in the aluminum melt, and was strongly agitated with an agitator. Thereafter, the aluminum was cast in a water-cooled copper mold. The obtained ingot had a plate shape measuring 200 mm long ⁇ 200 mm wide ⁇ 20 mm thick. The concentration of carbon in a portion corresponding to the bottom side of the copper mold was investigated.
  • a second embodiment relates to a manufacturing method in which a raw material for evaporation is evaporated in a mixture atmosphere of a gas of any one of a hydrocarbon gas, oxygen gas, and nitrogen gas and an inert gas such as argon gas, and evaporated particles are deposited on a substrate, by which a bulk body is formed.
  • FIGS. 6 and 7 are schematic views showing various manufacturing methods of the second embodiment. FIG. 6 shows a case where the sputtering method is used, and FIG. 7 shows a case where the deposition method is used.
  • the plate-shaped stationary substrate 2 is installed in the chamber 1 , and a target 11 for evaporation, which is formed of a metal for base material and a nonmetal for dispersion material, is provided on the substrate 3 so as to face the stationary substrate 2 .
  • the stationary substrate 2 and the target 11 for evaporation are connected to an electric power source 12 .
  • the stationary substrate 2 is formed of a metal for base material.
  • a DC 2-pole sputtering system is shown in FIG. 6, what we call a high-frequency sputtering system or what we call a magnetron sputtering system can be used.
  • the chamber 1 is provided with an atmospheric gas inlet 13 and an atmospheric gas outlet 14 . From the atmospheric gas inlet 13 , an atmospheric gas produced by mixing a hydrocarbon gas such as acetylene gas and an inert gas such as argon gas is supplied, and the atmospheric gas is introduced in the chamber 1 .
  • a hydrocarbon gas such as acetylene gas
  • an inert gas such as argon gas
  • a predetermined voltage is applied to cause a sputtering phenomenon, by which the metal for base material and the nonmetal for dispersion material are evaporated from the target 11 for evaporation.
  • the hydrocarbon gas such as acetylene gas introduced in the chamber 1 decomposes into carbon and hydrogen.
  • the carbon is taken into the bulk body 6 formed on the stationary substrate 2 together with the evaporating metal for base material and nonmetal for dispersion material.
  • the carbon reacts with the evaporating metal for base material or nonmetal for dispersion material to yield a stable carbide, and is taken into the bulk body 6 formed on the stationary substrate 2 in the carbide state.
  • the quantity of the hydrocarbon gas in the atmospheric gas introduced in the chamber 1 or the voltage applied at the time of sputtering is controlled, by which the carbon concentration in a composite material formed as the bulk body 6 can be determined appropriately.
  • the plate-shaped, stationary substrate 2 is installed in the chamber 1 , and a deposition source 15 formed of a metal for base material and a nonmetal for dispersion material is provided in the deposition crucible 7 so as to face the stationary substrate 2 .
  • the deposition source 15 is connected to an electric power source, not shown.
  • the deposition source 15 if being configured so that a rod-like source can be supplied continuously, is effective in achieving mass production of composite material.
  • the stationary substrate 2 is formed of a metal for base material.
  • the chamber is provided with the atmospheric gas inlet 13 and the atmospheric gas outlet 14 .
  • an atmospheric gas produced by mixing a hydrocarbon gas such as acetylene gas and an inert gas such as argon gas is supplied, and the atmospheric gas is introduced in the chamber 1 .
  • the pressure in the chamber 1 is controlled to a predetermined value, and the deposition source 15 is heated by causing an electric current to flow.
  • the metal for base material and the nonmetal for dispersion material are evaporated, and the evaporated particles are deposited on the stationary substrate 2 after passing through an acceleration probe electrode 16 .
  • the hydrocarbon gas such as acetylene gas introduced in the chamber 1 decomposes into carbon and hydrogen as in the case shown in FIG. 6, and the carbon yielded by the decomposition is taken into the bulk body 6 formed on the stationary substrate 2 together with the evaporating metal for base material and nonmetal for dispersion material.
  • the carbon reacts with the evaporating metal for base material or nonmetal for dispersion material to yield a stable carbide, and is taken into the bulk body 6 formed on the stationary substrate 2 in the carbide state.
  • the quantity of the hydrocarbon gas in the atmospheric gas introduced in the chamber 1 or the heating temperature at the time of deposition is controlled, by which the carbon concentration in the bulk body 6 can be determined appropriately.
  • the bulk body 6 is used as a single body, or it can be used as a composite material in which the concentration of dispersion material has been controlled by melting, mixing, and casting the bulk body 6 together with the metal for base material. Also, if necessary, the composite material can be rolled or heat-treated to control the crystal structure.
  • Example 2 represents a case where an aluminum-carbon composite material is manufactured by the sputtering method shown in FIG. 6.
  • a reactive magnetron sputtering apparatus was used, and as a sputtering target, a disk-shaped aluminum (purity: 99.999%) with a diameter of 203.2 mm and a thickness of 10 mm was used. Also, as a stationary substrate, an aluminum (purity: 99.999%) foil with a thickness of 10 ⁇ m was used.
  • a mixed gas of argon gas (purity: 99.999%) with a gas flow rate of 40 ccm and acetylene gas (purity: 99.5%) with a gas flow rate of 20 ccm was supplied in the chamber, and the sputtering pressure was controlled so as to be 0.4 Pa. Electric power of 8 kW (24.7 W/cm 2 ) was applied to the aluminum target, and the substrate temperature was set at 200° C.
  • Sputtering was performed for 60 minutes, by which a bulk body with a thickness of 80 ⁇ m and a total weight of 6.14 g was formed on the stationary substrate.
  • the carbon concentration in the formed bulk body was gas-analyzed, and it was found that 2.4 wt % of carbon was contained in the bulk body.
  • Example 1 The aluminum-carbon (0.7% by weight) composite material formed by casting as described above was formed into a sputtering target material, and an aluminum film was formed by using this target material under the same conditions as those in Example 1. The film characteristics of the aluminum film was investigated, and resultantly it was verified that as in the case of Example 1, if the aluminum-carbon composite material obtained in Example 2 is used as a raw material for target material, a film having high hillock resistance and low electrical resistivity can be formed steadily.
  • a dispersion material can be dispersed homogeneously into a base material of a composite material, so that various composite materials can be manufactured generally independently of the composition of the composite material as compared with the conventional manufacturing method for a composite material.
  • the composite material obtained by the manufacturing method in accordance with the present invention can meet the requirements for structural materials and electrode materials, and is suitable in each application because the dispersion material is dispersed very homogeneously into the base material and there is no internal defect such as a cavity or a cavity.
  • the composite material is used as a target material when wiring for a liquid crystal display or a semiconductor integrated circuit is formed, the required film characteristics can be realized steadily.

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US20050133121A1 (en) * 2003-12-22 2005-06-23 General Electric Company Metallic alloy nanocomposite for high-temperature structural components and methods of making
EP1614766A1 (en) * 2003-04-16 2006-01-11 Bridgestone Corporation Method for forming porous thin film
US20060057742A1 (en) * 2004-09-08 2006-03-16 Hitachi Cable, Ltd. Method of forming CNT containing wiring material and sputtering target material used for the method
US20060151314A1 (en) * 2002-10-25 2006-07-13 Semiconductor Energy Laboratory Co., Ltd. Sputtering system and manufacturing method of thin film
US20070281419A1 (en) * 2006-06-01 2007-12-06 Alhomoudi Ibrahim Abdullah Ibr Titanium dioxide thin film systems and method of making same
US20080113089A1 (en) * 2006-11-15 2008-05-15 Samsung Electronics Co., Ltd. Method and apparatus for manufacturing electrode for fuel cells
DE102007056678A1 (de) * 2007-11-24 2009-05-28 Bayerische Motoren Werke Aktiengesellschaft Verfahren zur Herstellung eines Bauteils aus einem Metallmatrix-Verbundwerkstoff
US9793099B2 (en) 2012-03-15 2017-10-17 Jx Nippon Mining & Metals Corporation Magnetic material sputtering target and manufacturing method thereof

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US7255757B2 (en) 2003-12-22 2007-08-14 General Electric Company Nano particle-reinforced Mo alloys for x-ray targets and method to make
JP5117357B2 (ja) * 2008-11-26 2013-01-16 株式会社アルバック 永久磁石の製造方法
JP6586618B2 (ja) * 2014-08-07 2019-10-09 国立大学法人豊橋技術科学大学 Ｄｌｃ膜形成方法及びｄｌｃ膜形成装置

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US20060151314A1 (en) * 2002-10-25 2006-07-13 Semiconductor Energy Laboratory Co., Ltd. Sputtering system and manufacturing method of thin film
EP1614766A1 (en) * 2003-04-16 2006-01-11 Bridgestone Corporation Method for forming porous thin film
EP1614766A4 (en) * 2003-04-16 2011-07-06 Bridgestone Corp METHOD FOR PRODUCING A POROUS THIN FILM
US20050133121A1 (en) * 2003-12-22 2005-06-23 General Electric Company Metallic alloy nanocomposite for high-temperature structural components and methods of making
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US20060057742A1 (en) * 2004-09-08 2006-03-16 Hitachi Cable, Ltd. Method of forming CNT containing wiring material and sputtering target material used for the method
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US7632761B2 (en) * 2006-06-01 2009-12-15 Wayne State University Method of making thin film anatase titanium dioxide
US20070281419A1 (en) * 2006-06-01 2007-12-06 Alhomoudi Ibrahim Abdullah Ibr Titanium dioxide thin film systems and method of making same
US7994602B2 (en) 2006-06-01 2011-08-09 Wayne State University Titanium dioxide thin film systems
US20080113089A1 (en) * 2006-11-15 2008-05-15 Samsung Electronics Co., Ltd. Method and apparatus for manufacturing electrode for fuel cells
DE102007056678A1 (de) * 2007-11-24 2009-05-28 Bayerische Motoren Werke Aktiengesellschaft Verfahren zur Herstellung eines Bauteils aus einem Metallmatrix-Verbundwerkstoff
US9793099B2 (en) 2012-03-15 2017-10-17 Jx Nippon Mining & Metals Corporation Magnetic material sputtering target and manufacturing method thereof
US10325761B2 (en) 2012-03-15 2019-06-18 Jx Nippon Mining & Metals Corporation Magnetic material sputtering target and manufacturing method thereof

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