WO2001068936A1 - Matiere composite et son procede de production - Google Patents

Matiere composite et son procede de production Download PDF

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Publication number
WO2001068936A1
WO2001068936A1 PCT/JP2001/001712 JP0101712W WO0168936A1 WO 2001068936 A1 WO2001068936 A1 WO 2001068936A1 JP 0101712 W JP0101712 W JP 0101712W WO 0168936 A1 WO0168936 A1 WO 0168936A1
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WO
WIPO (PCT)
Prior art keywords
metal
composite material
base material
substrate
compound
Prior art date
Application number
PCT/JP2001/001712
Other languages
English (en)
Japanese (ja)
Inventor
Takashi Kubota
Hiroshi Watanabe
Original Assignee
Mitsui Mining & Smelting Co.,Ltd.
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 Mitsui Mining & Smelting Co.,Ltd. filed Critical Mitsui Mining & Smelting Co.,Ltd.
Priority to JP2001567413A priority Critical patent/JP4060595B2/ja
Publication of WO2001068936A1 publication Critical patent/WO2001068936A1/fr

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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
    • 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 method for producing a composite material comprising two or more metals or non-metals and a compound thereof, and in particular, it is possible to disperse a dispersant very uniformly in a matrix of a composite material regardless of the composition of the composite material. Manufacturing technology. Background art
  • composite materials composed of metals, nonmetals, or compounds thereof have been used in various fields as structural materials for automobile parts and aircraft parts, electrode materials, target materials for thin film formation, and the like.
  • This composite material is manufactured by dispersing a metal or a non-metal or a compound thereof different from the base material in the base material so as to adjust the material properties so as to be suitable for each use.
  • nonmetal refers to hydrogen, boron, carbon, silicon, nitrogen, phosphorus, and the like, and is used as a broad concept including so-called semimetals such as antimony and bismuth. are doing.
  • This semi-solid agitation method is a method in which a metal serving as a base material is made into a semi-molten state, non-metal particles as a dispersing material are introduced into the metal, and strong stirring is performed to forcibly disperse the non-metal particles in the base metal. is there.
  • This method is effective when manufacturing a composite material using the molten metal of the base metal and non-metal particles with poor wettability.
  • the method uses a semi-molten state to prevent separation of the base metal and non-metal particles. It manufactures composite materials.
  • a metal powder as a base material and a non-metal powder as a dispersing material are mixed at a predetermined ratio, and the mixture is formed. It is manufactured by sintering.
  • HIP hot isostatic pressing
  • a metal powder as a base material and a non-metal powder as a dispersing material are mixed at a predetermined ratio, and the mixture is formed. It is manufactured by sintering.
  • the metal is easily oxidized, since the starting material is a powder, the oxygen concentration in the obtained composite material becomes high, and it may be difficult to control the physical properties of the composite material.
  • the base material and the dispersing material are both metals, and have properties of a low melting point metal and a high melting point metal, respectively.
  • a vacuum melting method it is very difficult to produce such a metal-metal composite material by, for example, a vacuum melting method.
  • the composite material according to the conventional manufacturing method will be described in more detail by taking a sputtering target material as an example.
  • a sputtering target material As an example, when forming wirings for liquid crystal displays and semiconductor integrated circuits, wiring technology by a sputtering method using an evening get material of a composite material has been used.
  • an aluminum thin film having excellent heat resistance and low resistance is typically used.
  • a target of a composite material using aluminum as a base material is used. Materials are used.
  • the aluminum thin film used for wiring of a liquid crystal display or a semiconductor integrated circuit for example, a target material of a composite material in which aluminum is used as a base material and a group IVa metal such as carbon and titanium is dispersed is used.
  • a target material made of an aluminum composite material makes it possible to form wiring having excellent heat resistance and low resistance, and to prevent disconnection of wiring due to stress. Therefore, it is naturally required that the target material of the aluminum composite material has a composition capable of forming a thin film satisfying the wiring characteristics, and further, the target material itself has few defects such as voids and voids. It is required to have a high density and a small amount of gas that becomes impurities.
  • the aluminum alloy described above is manufactured by the semi-melting stirring method, powder metallurgy method, or melting method. Even if a target material is manufactured, there is a limit in uniformly dispersing carbon and Group IVa metal in the aluminum base material, and a target that can stably form wiring satisfying practical wiring characteristics The material was insufficient.
  • a bulk material with a certain volume is required.
  • a bulk material composite material is formed by a conventional manufacturing method, internal defects such as nests are generated and the bulk material is Density tends to be low, and impurities such as gas are often mixed. Therefore, even if a bulk body manufactured by the conventional manufacturing method is used as a target material, it is difficult to realize stable wiring formation by sputtering.
  • the conventional method for producing a composite material can disperse the dispersing material in the base material, but its dispersibility is insufficient, and it is difficult to produce a norc body. There are many points to be improved due to internal defects that occur and contamination of impurities.
  • the conventional production methods require composite materials of various compositions. It can be said that it is very difficult to produce a single product by a single method.
  • the present invention has been made in view of the above-described circumstances, and a method of manufacturing a composite material including two or more metals or nonmetals and a compound thereof is more effective than a conventional manufacturing method in a base material of a composite material. It is an object of the present invention to provide a production method capable of dispersing a dispersion material in a very uniform manner, and to provide a production method of a composite material which can be applied for general purposes regardless of the composition of the composite material. Disclosure of the invention
  • the present inventors focused on a vapor phase growth technique used for forming a thin film, and as a result of intensive research, a technique capable of manufacturing a composite material that could not be realized by a conventional manufacturing method. was completed.
  • a metal or a non-metal or a compound thereof is used as a base material, and as a dispersant, at least one kind of a metal or a non-metal or a compound thereof different from the base material is dispersed.
  • a method for producing a composite material comprising: a base material made of a metal or a non-metal or a compound thereof constituting the base material; At least one or more materials for the dispersing material, which are composed of a metal or a non-metal or a compound thereof, constituting the dispersing material are simultaneously or alternately evaporated, and these evaporated particles are deposited on a substrate to form a bulk body. Things.
  • the evaporating particles are formed by a so-called physical vapor deposition method (PVD method) by using a raw material for the base material for forming the base material and a raw material for the dispersion material for forming the dispersion material. This is deposited on a substrate to form a bulk body.
  • the raw materials constituting the base material and the dispersing material are deposited as vaporized particles, respectively, so that unlike the conventional manufacturing method, the dispersing material is extremely uniform in the base material.
  • Various composite materials can be easily produced without being affected by the properties of each raw material. That is, even a composite material of a combination of a high melting point metal and a low melting point metal can be easily manufactured.
  • the first invention it is preferable to use a sputtering method or a vacuum evaporation method in a physical vapor deposition method. This is because these methods generate evaporated particles from each raw material at a relatively high speed, so that it is easy to form a bulk body having a predetermined volume.
  • the sputtering method or the vacuum evaporation method when the sputtering method or the vacuum evaporation method is applied, the evaporation of the raw material is performed in an inert gas atmosphere such as argon or a vacuum atmosphere. It can be applied, the amount of oxygen mixed in the manufactured bulk body can be controlled, impurities such as gas are mixed as much as possible, and the bulk body of the composite material with very few internal defects can be manufactured.
  • the evaporation of the raw material in the first invention can be performed simultaneously or alternately with the raw material for the base material and the raw material for the dispersing material. In the case of evaporating and depositing at the same time, the vaporized particles of the base material and the dispersing material are randomly deposited. In addition, even when the materials are alternately evaporated, controlling the deposited layer of the base material and the dispersing material on the order of Angstroms enables a composite material in which the dispersing material is uniformly dispersed in the base material to be macroscopically. Become. Further, the evaporation of the raw material in the first invention is preferably performed by a sputtering method in consideration of forming a bulk body in a relatively short time.
  • the present inventors use a metal or non-metal or a compound thereof as a base material, and use a different type of non-metal or these
  • a metal or nonmetal constituting the base material or a compound thereof, or a metal or nonmetal constituting the dispersant or a raw material for evaporation comprising the metal or a compound thereof was evaporated in an atmosphere of a hydrocarbon gas, an oxygen gas, or a nitrogen gas, and evaporated particles were deposited on a substrate to form a bulk body.
  • This second invention is based on physical vapor deposition (PVD) or chemical vapor deposition (CVD), and uses a hydrocarbon-based gas to evaporate the raw material for evaporation.
  • PVD physical vapor deposition
  • CVD chemical vapor deposition
  • the evaporation source is preferably evaporated by a sputtering method or a vacuum evaporation method in a physical vapor phase method or an activated evaporation method in a chemical vapor deposition method.
  • composition of the hydrocarbon gas in the second invention is not particularly limited as long as it can be decomposed into carbon and hydrogen at the time of sputtering or vapor deposition, preferably methane, ethane or acetylene gas.
  • vaporization atmosphere of the raw material according to the second aspect of the present invention can be adjusted by including an inert gas such as argon to adjust the vaporization efficiency of the raw material.
  • a metal or a non-metal constituting the base material or a raw material for evaporation composed of these compounds may be used, or a metal or a non-metal constituting the dispersing material in addition to the base material or the same may be used.
  • a raw material for evaporation containing a compound may be used. For example, when an evaporating material consisting of copper as a base material and silicon as a dispersing material is vaporized by a sputtering method in a nitrogen gas and deposited on a substrate, silicon and nitrogen react with each other and are stable.
  • a composite material can be produced in which silicon nitride is produced and the silicon nitride is dispersed as a dispersant in the base metal copper in a very uniform manner.
  • silicon nitride is produced and the silicon nitride is dispersed as a dispersant in the base metal copper in a very uniform manner.
  • evaporating particles consisting of copper as a base material and aluminum as a dispersing material are dispersed in oxygen gas and vaporized particles are generated by a sputtering method and deposited on a substrate, aluminum and oxygen react with each other to form a stable material.
  • a composite material can be produced in which aluminum oxide is formed and the aluminum oxide is dispersed as a dispersant in the copper base material in a very uniform manner.
  • the dispersant is very uniformly dispersed in the base material. It is possible to manufacture a composite material that has been mixed, and by adjusting the atmosphere in which the raw materials evaporate, the contamination of impurities can be suppressed as much as possible, and a bulk body with very few internal defects can be manufactured. It becomes possible.
  • the evaporation of the raw material in the second invention is preferably carried out by a sputtering method in consideration of the fact that the bulge is formed in a relatively short time.
  • the composite material obtained by the production methods of the first and second inventions of the present invention described above is a pulp body formed by being deposited on a base material. It is not difficult to handle as a single unit like a so-called thin film, but it has a volume enough to handle the bulk itself as it is by peeling it off the substrate.
  • the bulk material separated from the substrate by the manufacturing method according to the first and second inventions can be used as it is for various uses such as a target material.
  • the bulk body obtained by the production method according to the first and second inventions is melted together with a metal or nonmetal constituting the base material or a base material raw material made of these compounds, and , Mixed, forged and molded, and the dispersant concentration can be adjusted.
  • the obtained composite material of the bulk body is structurally very ideal in that the dispersing material is extremely uniformly dispersed in the base material.
  • these two manufacturing methods are based on the vapor phase growth method, if a bulk body having a larger volume needs to be manufactured for a long time, it is necessary to obtain a complicated shape. Is also difficult.
  • the bulk material obtained by these two methods and the raw material for the base material are combined, melted, mixed, and formed to adjust the concentration of the dispersing material to form a larger bulk material. It produces composite materials. If a mold having a predetermined shape is used during the molding, it is easy to obtain a composite material having a complicated shape.
  • the base material and the dispersion Since the bulk material is formed in a state in which the material is very finely dispersed with each other, that is, since the dispersed material forms the bulk body in a state in which the base material has high wettability, Even when the melt is dissolved together with the base material, the dispersant does not separate from the base material.
  • the composite material obtained by dissolving and mixing the bulk body and the raw material for the base material and forging and molding is in a state where the dispersing material is extremely uniformly dispersed in the base material.
  • the amount of the dispersing material is adjusted beforehand when forming the norm body, or the amount of the base material to be added is increased.
  • the composition of the finally obtained composite material can be easily controlled.
  • the temperature at which the bulk body and the base material are melted may be appropriately determined according to the composition of the composite material. Basically, the temperature is determined within the range from the melting point temperature to the evaporation temperature of the bulk body. In other words, it is only necessary to adjust the temperature so that the bulk body is in a sufficiently fluid state and the raw materials for the base material to be charged and the bulk body can be uniformly mixed.
  • the atmosphere in which the dissolution treatment is performed but it is preferable to perform the dissolution treatment in a vacuum atmosphere or an inert gas atmosphere such as argon for a composite material in which the base material or the dispersant is easily oxidized.
  • the bulk body according to the first and second inventions and the composite material obtained by melting, mixing and forging the bulk body and the raw material for the base material are subjected to rolling or heat treatment to obtain the composite body.
  • the crystal structure can be controlled.
  • the final composite material must have properties that can be adapted to each application.However, if a composite material with excellent properties, such as excellent strength properties, should be rolled or heat treated, By doing so, it can be realized by adjusting the crystal structure.
  • rolling and heat treatment may be used in combination, or rolling or heat treatment alone may be used.
  • the substrate is rotated to deposit the evaporated particles. When a rotating substrate maintained at a predetermined rotation speed is used, the deposition of the evaporated particles proceeds uniformly at various points on the surface of the rotating substrate. This is because a bulk body having a more uniform composition and a uniform thickness can be formed.
  • the substrate on which the evaporated particles are deposited is made of the same material as the base material. This is because the deposited particles are deposited consistently with the substrate, and a uniform crystal structure is easily obtained.
  • a composite material is manufactured by dissolving, mixing, and molding the above-mentioned bulk body and the raw material for the base material, if the material of the substrate is the same as the base material, the formed bulk body is removed from the substrate. It can be dissolved without peeling, so that the manufacturing process can be simplified.
  • a composite material tailored to each application can be produced for general use regardless of the composition, and the dispersing material is dispersed in a very uniform state in the base material, and impurities Is suppressed, and a bulk composite material having no internal defects such as nests can be obtained. Therefore, the composite material obtained by the production method of the present invention can be applied to various applications as appropriate, and is very suitable as a structural material for automobile parts and aircraft parts, an electrode material, a target material for forming a thin film, and the like. It is something. Furthermore, a composite material obtained by the production method of the present invention, in which the base material is aluminum and the dispersing material is carbon, is very suitable as the target material.
  • FIG. 1 is a schematic view showing a case where a bulk body is formed on a stationary substrate by a sputtering method.
  • FIG. 2 is a schematic diagram showing a case where a bulk body is formed on a stationary substrate by a vacuum evaporation method.
  • FIG. 3 is a schematic view showing a case where a bulk body is formed on a rotating substrate by a sputtering method.
  • FIG. 4 is a schematic view showing a case where a bulk body on a rotating substrate is formed by using both a sputtering method and a vacuum evaporation method.
  • FIG. 5 is a cross-sectional observation photograph of the composite material after water cooling in Example 1.
  • FIG. 6 is a schematic diagram showing a case where a hydrocarbon body is introduced by a sputtering method to form a bulk body on a stationary substrate.
  • FIG. 7 is a schematic view showing a case where a bulk body is formed on a stationary substrate by introducing a hydrocarbon gas by a vapor deposition method.
  • the first embodiment relates to a manufacturing method in which a base material and a dispersant material are evaporated by a sputtering method or a vacuum evaporation method to form a bulk body.
  • a sputtering method or a vacuum evaporation method to form a bulk body.
  • FIG. 1 shows a method of evaporating a metal raw material serving as a base material and a nonmetal raw material serving as a dispersing material by a sputtering method and depositing them on a plate-shaped stationary substrate.
  • a plate-shaped stationary substrate 2 is installed in the chamber 1, and a metal target 4 for base material and a non-metallic getter 5 for dispersing material 5 are placed on a substrate 3 so as to face the stationary substrate 2.
  • Each one has its own equipment.
  • the stationary substrate 2 and each of the targets 4 and 5 are connected to a power source (not shown).
  • the stationary substrate 2 is made of a base metal. You.
  • FIG. 1 shows the case where two targets, ie, the base metal target 4 and the dispersing material target 5 are used, more targets are used in accordance with the composition of the target composite material. It can also be installed as appropriate.
  • FIG. 1 shows an example of a DC two-pole sputtering method, a so-called high-frequency sputtering method or a magnetron sputtering method may be applied.
  • a composite material of the 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, and the bulk body 6 is made into a single body, and the structural material, the electrode material, and the target material are removed. Can be used for various purposes.
  • the bulk body 6 can be used as it is, it can be used after adjusting the crystal structure by performing rolling or heat treatment as necessary.
  • the composition of the composite material that is, the concentration of the dispersant, can be arbitrarily determined. After heating to a predetermined temperature and dissolving it to a certain degree of fluidity, it is mixed by stirring thoroughly to form a uniform mixture and rapidly molded to form a composite material with the desired composition and shape. I can do it. Furthermore, if necessary, the crystal structure can be adjusted by rolling or heat-treating the composite material.
  • FIG. 2 shows a method of evaporating a metal raw material serving as a base material and a non-metallic raw material serving as a dispersing material by a vacuum evaporation method and depositing them on a plate-shaped stationary substrate.
  • a plate-shaped stationary substrate 2 is installed in the par 1.
  • a vapor deposition tube 7 is provided with a base metal vapor deposition source 8 and a non-metallic vapor deposition source 9 for a dispersing material so as to face the stationary substrate 2. Things are installed.
  • These two evaporation sources 8 and 9 are connected to a power source (not shown). If this evaporation source can be supplied continuously in the form of a rod, it will be effective for mass production of composite materials.
  • the stationary substrate 2 is made of a base metal. In the case of the vacuum evaporation method described with reference to FIG. 2, as in the case of FIG. 1, it is also possible to appropriately install more evaporation sources according to the composition of the target composite material. .
  • the chamber 11 is depressurized to a predetermined pressure to form a vacuum atmosphere, and the metal vapor deposition source 8 for the base material and the non-metallic vapor deposition source 9 for the dispersing material are energized and heated.
  • the metal for the material and the non-metal for the dispersing material are evaporated and deposited on the stationary substrate 2.
  • a composite material of the notch body 6 is formed on the stationary substrate 2.
  • the dispersing material is formed by dissolving, mixing, and forming together with the force used as a single bulk body 6 or the base metal. It can be used as a composite material whose concentration has been adjusted. Further, if necessary, rolling or heat treatment can be performed to adjust the crystal structure.
  • FIGS. Figure 3 shows a case where a bulk composite material is manufactured on a rotating substrate by the spattering method.
  • a cylindrical rotating substrate 10 is installed in the chamber 11, and the base metal 3 is placed on the substrate 3 in a direction facing the rotating substrate 10 and orthogonal to each other.
  • those equipped with a non-metallic target 5 for a dispersing material are installed respectively.
  • an argon gas is introduced into the chamber 11 and a predetermined voltage is applied by a power source (not shown) to perform sputtering, so that the base material is placed on the side surface of the rotating cylindrical rotating substrate 10.
  • the bulk metal 6 ' is formed by depositing the metal for dispersing and the nonmetal for dispersing material.
  • the microstructure of the bulk body 6 ′ is such that a metal for the base material and a non-metal for the dispersing material are deposited on the layer in an Angstrom mode. It will be in the state of having done.
  • this bulk body 6 ′ is viewed as a whole as a whole, the base metal and the dispersant nonmetal have a uniform composition, and the dispersant is contained in the base material. It is extremely finely dispersed.
  • the bulk body 6 ′ formed on the rotating substrate can be used as it is as a composite material for each application as described with reference to FIG. 1, and the bulk body 6 ′ and the base metal are combined together. It can be used as a composite material in which the dispersing agent concentration is adjusted by dissolving. Furthermore, the crystal structure can be adjusted by rolling or heat treatment.
  • FIG. 3 shows a case where two targets are used, it is naturally possible to install three or more targets around the rotating substrate according to the composition of the target composite material. is there. Further, in FIG. 3, the case where the sputtering method is used has been described, but the composite material of the bulk body 6 ′ can be similarly manufactured by using the rotating substrate 10 by the vacuum evaporation method.
  • FIG. 4 shows a case where a bulk composite material is manufactured on a rotating substrate by using both sputtering and vapor deposition.
  • a cylindrical rotary substrate 10 is set in the chamber 11, and a base metal target 4 is provided on a substrate 3 in a direction facing the rotary substrate 10 and orthogonal to each other.
  • the metal for the base material is evaporated by sputtering, while the vapor pressure of the non-metallic material for the non-metallic material for the dispersing material is the pressure in the chamber 11. Electric heating is performed until the temperature becomes higher to evaporate the nonmetal for the dispersion material.
  • the metal for the base material and the non-metal for the dispersing material are deposited on the side surface of the rotating substrate 10 to form a bulk body 6 ′.
  • a composite material having a structure similar to that described in FIG. 3 is obtained.
  • the handling of the node 6 ′ is the same as that described with reference to FIG.
  • Example 1 is a case where an aluminum-carbon composite material was produced by a sputtering method using the rotating substrate shown in FIG. Two types of materials were prepared: aluminum (purity 99.99.9%) as a metal target for the base material and carbon (purity 99.9%) as a nonmetallic target for the dispersing material. Both targets are 127 mm long, 279.4 mm wide, and 10 mm thick. Spatterin The power unit used was a three force sword / magnetron sputtering type, and two of the three force swords were used. An eight-sided stainless steel plate with a length of 279 mm and a width of 80 mm on one side was prepared by preparing an octagonal cylindrical rotating substrate with the vertical sides connected to each other. A 12 m aluminum foil (purity 99.99.99%) was wrapped around and aluminum and carbon were deposited on the aluminum foil.
  • the sputtering conditions were as follows: argon gas was introduced into the chamber, the sputtering pressure was 0.87 Pa, the input power was 12 kW (24.8 WZcm 2 ) for the aluminum target, and 4 kW (8. 3 W / cm 2 ), and the rotation speed of the rotating substrate was 30 rpm. Sputtering was performed for about 30 hours to form a bulk body having a thickness of 0.6 mm on the side surface of the rotating substrate.
  • the cross-sectional structure of the formed pulp body is a state in which an aluminum layer having a thickness of about 0.3 m and a carbon layer having a thickness of about 0.01 m are laminated, as calculated from the deposition rate.
  • the carbon concentration in the bulk was determined to be 2.6% by weight (5.6 at%).
  • This bulk body is vacuum-melted together with separately prepared aluminum (purity 99.9 9 9%) to adjust the aluminum-carbon composition so that the carbon concentration becomes 0.7% by weight. Fabrication was performed using a mold. The ⁇ molded also the result of the microscopic observation was conducted, while the aluminum of the base material, in the form of carbon A 1 -C (A 1 4 C 3) phases, and social standing with a grain size of about 1mm It was confirmed that.
  • the composite material of aluminum one-carbon obtained in Example 1 shows the result of observation of the dispersion state of A l-C (A 1 4 C 3) Phase in Fig. In FIG. 5, the black portion is the A 1 -C (A 1 4 C 3 ) phase.
  • the aluminum-carbon (0.7% by weight) composite material formed as described above was formed into a sputtering target material, thereby forming an aluminum thin film.
  • Deposition conditions of the aluminum thin film using a DC magnetron sputtering evening device, a sputtering pressure 0. 3 3 3 P a (2. 5mTo rr), charged electricity 3Wa t tZcm 2, thickness 3000 A on a glass substrate Approximately a thin film was formed.
  • the sputtering time required to form a thin film having a thickness of about 300 OA is about 100 seconds. A thin film was formed. By repeating this thin film forming operation, a long time thin film was formed continuously by one sputtering target material.
  • Hillock which is a heat-resistant property, of the thin film formed for the first time, the thin film when the sputtering time has elapsed about 20 hours, and the thin film when the sputtering time has elapsed about 40 hours has occurred.
  • the hillocks are bumps formed on the surface of the thin film when the glass substrate with the thin film is heat-treated in a vacuum at a temperature of 300 ° C. for a predetermined time. As a result, it was confirmed that hillocks hardly occurred in each thin film regardless of the total sputtering time.
  • the electrical specific resistance of each thin film was measured, it was confirmed that the specific resistance was about 5 ⁇ cm under optimum conditions.
  • Comparative Example 1 is based on a semi-solid stirring method. 2 kg of aluminum (purity 99.99.9%) was heated to about 700 ° C in a carbon tube, melted once, and then cooled to 640 to obtain a semi-molten state (solid liquid phase). (Coexistence state).
  • the second embodiment is a method for evaporating a raw material for evaporation in a mixed atmosphere of a hydrocarbon-based gas, oxygen gas, or nitrogen gas and an inert gas such as argon gas.
  • the present invention relates to a method for producing a bulk body by evaporating water and depositing evaporated particles on a substrate.
  • 6 and 7 schematically show various manufacturing methods in the second embodiment. FIG. 6 shows the case by the sputtering method, and FIG. 7 shows the case by the vapor deposition method.
  • FIG. 6 shows an example of DC two-pole sputtering, a method referred to as a so-called high-frequency sputtering or magnetron sputtering can be applied.
  • the chamber 11 is provided with an atmosphere gas inlet 13 and an atmosphere gas outlet 14. From the atmosphere gas inlet 13, a hydrocarbon-based gas such as acetylene gas and an unreacted gas such as argon gas are supplied. An atmosphere gas mixed with an active gas is supplied, and the atmosphere gas is introduced into the chamber 1.
  • a hydrocarbon-based gas such as acetylene gas and an unreacted gas such as argon gas are supplied.
  • An atmosphere gas mixed with an active gas is supplied, and the atmosphere gas is introduced into the chamber 1.
  • the hydrocarbon-based gas such as acetylene gas introduced into the chamber 11 is decomposed into carbon and hydrogen.
  • this carbon is taken into the bulk body 6 formed on the stationary substrate 2 together with the evaporating base metal or the dispersing nonmetal, or reacts with the evaporating base metal or the dispersing nonmetal.
  • the carbon concentration in the composite material formed as the bulk body 6 is appropriately determined by adjusting the amount of the hydrocarbon-based gas in the atmospheric gas introduced into the chamber 11 and the voltage applied during the sputtering. It becomes possible.
  • FIG. 7 a plate-shaped stationary substrate 2 is installed in a chamber 11, and a metal for a base material and a non-metal for a dispersing material are formed in a deposition pipe 7 so as to face the stationary substrate 2.
  • the equipment equipped with the evaporation source 15 is installed.
  • the evaporation source 15 is connected to a power source (not shown). This As described in the first embodiment, if the rod-shaped thing can be continuously supplied as the evaporation source 15, it becomes effective when mass-producing the composite material.
  • the stationary substrate 2 is formed of a base metal.
  • the chamber 1 is provided with an atmosphere gas inlet 13 and an atmosphere gas outlet 14. From the atmosphere gas inlet 13, a hydrocarbon-based gas such as acetylene gas and an inert gas such as argon gas are supplied. An atmosphere gas mixed with an active gas is supplied, and this atmosphere gas is introduced into the chamber 11. Thereafter, the pressure is adjusted to a predetermined value, and the metal for the base material and the non-metal for the dispersing material are evaporated by energizing and heating the evaporation source 15, and the evaporated particles pass through the accelerating probe electrode 16 and move to the stationary substrate 2. Deposited on At that time, the hydrocarbon-based gas such as acetylene gas introduced into the chamber 11 is decomposed into carbon and hydrogen as in the case of FIG.
  • a hydrocarbon-based gas such as acetylene gas and an inert gas such as argon gas
  • the decomposed carbon is used for the evaporating base material.
  • the metal and the non-metal for the dispersing material it is taken into the bulk body 6 formed on the stationary substrate 2 or reacts with the evaporating base metal or the non-metal for the dispersing material to form a stable carbide, and In the state of carbide, it is taken into the bulk body 6 formed on the stationary substrate 2.
  • the carbon concentration in the bulk body 6 can be appropriately determined by adjusting the amount of the hydrocarbon-based gas in the atmospheric gas introduced into the chamber 11 and the heating temperature during the deposition.
  • the bulk material 6 may be used as a single bulk body 6 or may be used as a base metal.
  • it can be used as a composite material in which the concentration of the dispersant is adjusted by dissolving, mixing and forging. Further, if necessary, rolling or heat treatment can be performed to adjust the crystal structure.
  • an example of the second embodiment will be described.
  • Example 2 In this example 2, a case is described in which a composite material of aluminum aluminum carbon is produced by the sputtering method shown in FIG.
  • the apparatus used was a reactive magnetron sputtering apparatus, and a disc-shaped aluminum (purity 99.999%) having a diameter of 203.2 mm and a thickness of 10 mm was used as a sputtering target.
  • a gas mixture 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 is supplied into the chamber, and the sputtering pressure is reduced. It was adjusted to be 0.4 Pa.
  • the input power was 8 kW (24.7 W / cm 2 ) for the aluminum target, and the substrate temperature was 200 ° C.
  • Sputtering was performed for 60 minutes to form a bulk body with a thickness of 80 1 m and a total amount of 6.14 g on a stationary substrate.
  • a gas analysis of the carbon concentration of the formed bulk body revealed that the bulk body contained 2.4 wt% of carbon.
  • the aluminum-carbon (0.7% by weight) composite material formed as described above was processed into a sputtering target material, thereby forming an aluminum thin film in the same manner as in Example 1 described above. Under the conditions, the characteristics of the thin film were examined. As a result, when the aluminum-carbon composite material obtained in Example 2 was used as a raw material for an evening get material, a thin film having excellent hillock resistance and low electric resistivity was obtained as in Example 1. Was confirmed to be able to form a stable film.
  • the dispersant can be dispersed more uniformly in the matrix of the composite material than in the conventional method for producing a composite material.
  • various composite materials can be manufactured for general use.
  • the composite material obtained by the production method of the present invention since the dispersing material is extremely uniformly dispersed in the base material and there are no internal defects such as nests, the composite material sufficiently satisfies the required characteristics such as constituent materials and electrode materials. It becomes suitable in each application. In particular, if it is used as a target material when forming wiring for a liquid crystal display or a semiconductor integrated circuit, the required thin film characteristics can be stably realized.

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

Abstract

L'invention concerne un procédé destiné à une matière composite comprenant une matière de base renfermant un métal, un non-métal ou un composé de ces éléments et, dispersé dans cette matière de base, au moins un dispersoïde renfermant un métal, un non-métal ou un composé desdits éléments, et dont la nature est différente de celle de la matière de base. Ce procédé se caractérise en ce qu'une matière brute destinée à la matière de base comprenant un métal, un non-métal ou un composé de ces éléments constituant cette matière de base, et au moins une matière brute destinée au dispersoïde comprenant un métal, un non-métal ou un composé desdits éléments constituant ce dispersoïde, sont vaporisées de manière simultanée ou en alternance, les particules vaporisées étant déposées sur un substrat, d'où l'obtention d'un article en vrac. Ledit procédé permet de produire une matière composite comprenant au moins deux métaux, non-métaux ou composés desdits éléments présentant une dispersion extrêmement uniforme d'un dispersoïde dans une matière de base, indépendamment de la composition de cette matière composite.
PCT/JP2001/001712 2000-03-13 2001-03-06 Matiere composite et son procede de production WO2001068936A1 (fr)

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US7578909B2 (en) 2004-09-08 2009-08-25 Hitachi Cable, Ltd. Method of forming CNT containing wiring material and sputtering target material used for the method
US7731810B2 (en) 2003-12-22 2010-06-08 General Electric Company Nano particle-reinforced Mo alloys for x-ray targets and method to make
JP2010129665A (ja) * 2008-11-26 2010-06-10 Ulvac Japan Ltd 永久磁石の製造方法
WO2013136962A1 (fr) * 2012-03-15 2013-09-19 Jx日鉱日石金属株式会社 Cible de pulvérisation de matériau magnétique et procédé de fabrication de cette dernière
JP2016037637A (ja) * 2014-08-07 2016-03-22 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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US20060189132A1 (en) * 2003-04-16 2006-08-24 Bridgestone Corporation Method for forming 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
US7632761B2 (en) * 2006-06-01 2009-12-15 Wayne State University Method of making thin film anatase titanium dioxide
KR101149408B1 (ko) * 2006-11-15 2012-06-01 삼성전자주식회사 연료 전지용 전극의 제조 방법 및 제조 장치
DE102007056678A1 (de) * 2007-11-24 2009-05-28 Bayerische Motoren Werke Aktiengesellschaft Verfahren zur Herstellung eines Bauteils aus einem Metallmatrix-Verbundwerkstoff

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Publication number Priority date Publication date Assignee Title
US7731810B2 (en) 2003-12-22 2010-06-08 General Electric Company Nano particle-reinforced Mo alloys for x-ray targets and method to make
US7578909B2 (en) 2004-09-08 2009-08-25 Hitachi Cable, Ltd. Method of forming CNT containing wiring material and sputtering target material used for the method
JP2010129665A (ja) * 2008-11-26 2010-06-10 Ulvac Japan Ltd 永久磁石の製造方法
WO2013136962A1 (fr) * 2012-03-15 2013-09-19 Jx日鉱日石金属株式会社 Cible de pulvérisation de matériau magnétique et procédé de fabrication de cette dernière
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JP2016037637A (ja) * 2014-08-07 2016-03-22 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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US20030056928A1 (en) 2003-03-27
KR100446563B1 (ko) 2004-09-04
CN1362998A (zh) 2002-08-07

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