KR100446563B1 - Method for producing composite material and composite material produced thereby - Google Patents

Abstract

The present invention relates to a method for producing a composite material composed of two or more metals or nonmetals and compounds thereof, and is not particularly limited to the composition of the composite material, and to a manufacturing technology capable of dispersing the dispersion material very uniformly in the base material of the composite material. It is about. The present invention is a method for producing a composite material comprising a metal or non-metal or a compound thereof as a base material and dispersing at least one or more kinds of the metal or non-metal or a compound thereof different from the base material as a dispersant. A base material composed of a metal or a nonmetal or a compound thereof, and at least one raw material for a dispersant composed of a metal or a nonmetal or a compound thereof constituting the dispersion material are simultaneously or alternately evaporated so that these vaporized particles are deposited on a substrate. It deposits and makes it bulk.

Description

Method for producing composite material and composite material obtained thereby

Background Art Conventionally, composite materials made of metals or nonmetals or compounds thereof have been widely used in various aspects as structural materials such as automobile parts and aircraft parts, electrode materials, target materials for thin film formation, and the like. The composite material is produced by dispersing the base metal and other metals or nonmetals or compounds thereof in the base material so as to realize material properties for each use. As used herein, the term nonmetal refers to hydrogen, boron, carbon, silicon, nitrogen, phosphorus, and the like, and is used as a broad concept including antimony, bismuth, and the like, called semimetals.

As a manufacturing method of such a composite material, the semi-melt stirring method (compo-casting process) and the powder metallurgy method are known. In this anti-melt stirring method, a metal as a base material is made into a semi-melt state, a nonmetal particle as a dispersant is added thereto, and the steel is agitated to forcibly disperse nonmetal particles in the base metal. This method is effective when manufacturing a composite material from the molten metal and non-wetting nonmetal particles of a base material, and manufacturing a composite material in the semi-melt state so that separation of a base metal and a nonmetal particle may not occur. However, in the semi-melt stirring method, since the metal in the semi-molten state is in the so-called sherbet state, defects such as cavities are likely to occur in the formed article, and gas tends to flow and the material density tends to decrease.

In addition, powder metallurgy represented by hot press, HIP (hot isotropic hydrostatic pressure method) or the like is produced by mixing a metal powder as a base material and a nonmetal powder composed of a dispersant at a predetermined ratio, and molding and sintering it. In this method, in the case of a metal which is easy to oxidize, since the starting material is powder, the oxygen concentration in the obtained composite material becomes high, and it may be difficult to control the composite material properties. Since the powder metallurgy has limitations in powder adjustment, mixing treatment of the powder, and the like, it may be difficult to more uniformly disperse the dispersant in the base material.

In addition to the anti-melt stirring method and the powder metallurgy method, there are also commonly used melt casting methods. However, when the base material and the dispersant are both metals and have properties of low melting point metals and high melting point metals, for example, by vacuum melting method. It is quite difficult to manufacture such a composite material between metals.

Here, the composite material by the conventional manufacturing method is mentioned later in more detail as an example of a sputtering target material. In recent years, the wiring technique by the sputtering method using the target material of a composite material is used, when forming the wiring of a liquid crystal display, a semiconductor integrated circuit, etc. The aluminum thin film which is excellent in heat resistance and low resistance is applied to wiring formation by sputtering, and the target material of the composite material which uses aluminum as a base material is used in order to form this aluminum thin film.

As 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 in which Group IVa metals such as carbon and titanium are dispersed is used. This is because when the target material of the aluminum composite material is used, wiring excellent in heat resistance and low resistance can be formed, and the wiring breakage due to stress can be prevented. Therefore, it is natural that the target material of the aluminum composite material is composed of a composition capable of forming a thin film satisfying the wiring characteristics, and the defects such as voids and voids in the target material itself are small, high density, and impurities. It is required that the amount of gas to be mixed is small.

By the way, in the above-mentioned prior art, a composite material can be manufactured using aluminum as a base material and carbon and a Group IVa metal as a dispersing material, but it was difficult to produce a satisfactory target material for wiring formation. In other words, even if the above-described aluminum target material is produced by the semi-melt stirring method, the powder metallurgy method, or the melt casting method, there is a limit in uniformly dispersing the carbon and the Group IVa metal in the aluminum base material. It was insufficient as a target material for stably forming wiring that satisfies practical wiring characteristics. In addition, in order to use it as a target material, a bulk body that maintains a certain volume is required. However, when a bulk composite material is formed by a conventional manufacturing method, internal defects such as cavities are generated, resulting in a low density of the bulk body. In many cases, impurities such as gas are mixed. Therefore, even when using a bulk body as a target material by the conventional manufacturing method, it was difficult to realize stable wiring formation by sputtering.

As can be seen by using this target material as an example, in the conventional method for producing a composite material, it is possible to disperse the dispersant in the base material, but its dispersibility is insufficient, and internal defects generated in the bulk body, mixing of impurities, etc. There are many things to improve. Considering the case of manufacturing not only the target material but also structural materials such as automobile parts and aircraft parts, and composite materials for other uses as electrode materials, conventional manufacturing methods generally employ composite materials of various compositions. It can be said that manufacturing by the manufacturing method of this is quite difficult.

The present invention has been made on the basis of the above circumstances, and in the method for producing a composite material composed of two or more metals or nonmetals and compounds thereof, it is possible to disperse the dispersion material more uniformly in the base material of the composite material than in the conventional production method. The present invention provides a method for producing a composite material, which is not limited to the composition of the composite material, but which can be applied universally.

The present invention relates to a method for producing a composite material composed of two or more metals or nonmetals and compounds thereof, and more particularly, to a manufacturing technology capable of dispersing a dispersion material very uniformly in a matrix of a composite material regardless of the composition of the composite material. will be.

1 is a schematic view showing a case where a bulk body is formed on a stationary substrate by the sputtering method.

2 is a schematic view showing a case where a bulk body is formed on a stationary substrate by a vacuum deposition method.

3 is a schematic view showing a case where a bulk body is formed on a rotating substrate by a sputtering method.

4 is a schematic view showing a case where a bulk body is formed on a rotating substrate by using a sputtering method and a vacuum deposition method together.

FIG. 5 is a cross-sectional photograph of a composite material after water-cooled casting in Example 1. FIG.

Fig. 6 is a schematic diagram showing a case where a bulk body is formed on a stationary substrate by introducing a hydrocarbon gas by the sputtering method.

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.

In order to solve the above problems, the present inventors focused on the vapor phase growth technology used for thin film formation, and as a result of careful research, the present inventors have completed a technology capable of manufacturing a composite material that could not be realized by the conventional manufacturing method. will be.

The present invention is, as a first invention, a method for producing a composite material obtained by dispersing at least one or more kinds of metals or nonmetals or compounds thereof different from the base material as a dispersant, using a metal or nonmetal or a compound thereof as a base material. The raw material for a base material which consists of the metal or nonmetal or a compound which comprises the said base material, and the raw material for at least one dispersion material which consists of the metal or nonmetal or these compound which comprises the said dispersing material are vaporized simultaneously or alternately. These vaporized particles are deposited on a substrate to form a bulk body.

In the first invention, the bulk material is formed by depositing a base material for forming a base material and a raw material for dispersing material as vaporized particles by a so-called physical vapor deposition method (PVD method) and depositing them on a substrate. To form. According to the first invention, since the raw materials constituting the base material and the dispersing material are deposited as evaporated particles, respectively, and are different from the conventional manufacturing method, the dispersing material is dispersed very uniformly in the base material and is not influenced by the properties of each raw material. Various composite materials can be manufactured easily without doing this. In short, a composite material combining a high melting point metal and a low melting point metal can be easily manufactured.

In this first invention, it is preferable to use a sputtering method or a vacuum deposition method in the physical vapor phase growth method. This is because these methods generate evaporated particles from each raw material at a relatively high speed, making it easy to form a bulk body having a predetermined volume. In the first invention, when the sputtering method or the vacuum deposition method is applied, since the raw material is evaporated in an inert gas atmosphere such as argon or in a vacuum atmosphere, even a raw material which is easy to oxidize can be applied. In addition to controlling the amount of oxygen mixed into the sieve, the mixing of impurities such as gas can be avoided as much as possible, and a bulk body of a composite material can be produced in a state where the internal defects are considerably less.

In this first invention, the evaporation of the raw material can be performed simultaneously or alternately with the base material and the dispersant material. At the same time, when evaporating and depositing, evaporated particles of the base material and the dispersion material are randomly deposited. In the case of alternately evaporating each other, by controlling the deposition layer between the base material and the dispersant at the angstrom level, the dispersant is uniformly dispersed in the base material in a macroscopic manner. In addition, in this 1st invention, in consideration of forming a bulk body in a comparatively short time, it is preferable to evaporate a raw material by the sputtering method.

Next, the present inventors, as a second invention, use a metal or nonmetal or a compound thereof as a base material, and disperse at least one or more kinds of a metal or nonmetal or a compound thereof different from the base material as a dispersant. In the production method, a raw material for evaporation comprising the metal or nonmetal or compound thereof constituting the base material or the metal or nonmetal or compound thereof constituting the dispersant is any one of a hydrocarbon gas, oxygen gas and nitrogen gas. It was made to evaporate in the middle, and evaporated particle was deposited on the board | substrate to make it a bulk body.

The second invention is based on the physical vapor growth method (PVD method) or the chemical vapor growth method (CVD method), and selects any of hydrocarbon gas, oxygen gas and nitrogen gas as the atmosphere for evaporating the raw material for evaporation. Thus, a composite material in which carbides, nitrides, and oxides as dispersion materials are dispersed in a base material very uniformly can be produced. In the second invention, the evaporation of the raw material for evaporation is preferably a sputtering method, a physical vapor deposition method, or an activation vapor deposition method in a chemical vapor deposition method.

In this second invention, the composition of the hydrocarbon gas is not particularly limited, and may be decomposed into carbon and hydrogen at the time of sputtering or vapor deposition, and methane, ethane or acetylene gas is preferable. In the second invention, the evaporation atmosphere of the raw material can be adjusted by including an inert gas such as argon.

In this second invention, a raw material for evaporation composed of a metal or nonmetal or a compound thereof constituting the base material may be used, or a raw material for evaporation comprising a metal or nonmetal or a compound constituting the dispersant in addition to the base material is used. You may use it. For example, when an evaporation raw material composed of copper as a base material and silicon as a dispersant is generated by evaporation particles by sputtering in nitrogen gas and deposited on a substrate, silicon and nitrogen react to form stable silicon nitride. A composite material can be produced in which silicon nitride is very uniformly dispersed in copper as a base material as a dispersant. Similarly, when evaporation raw material consisting of copper as a base material and aluminum as a dispersing material is generated by evaporation particles by sputtering in oxygen gas and deposited on a substrate, aluminum and oxygen react to form stable aluminum oxide, and the aluminum oxide As this dispersing material, a composite material in a very uniform state dispersed in copper of the base material can be produced.

According to this second invention, even if the composite material, that is, a dispersant having poor wettability with respect to the base material, could not be produced by the conventional manufacturing method, it is possible to produce a composite material in which the dispersant is very uniformly dispersed in the base material, By adjusting the atmosphere in which the raw material is evaporated, the incorporation of impurities can be suppressed as much as possible, thereby making it possible to produce a bulk body with a considerably less internal defect. In this second invention, in consideration of forming the bulk body in a relatively short time, the evaporation of the raw material is preferably performed by the sputtering method.

Although the composite material obtained by the manufacturing method of the 1st and 2nd invention which concerns on this invention mentioned above consists of the bulk body formed by depositing on a base material, it is difficult to handle this bulk body as a single body like a so-called thin film. Instead, it has a volume of the extent that the bulk body itself can be handled as it is by peeling from the substrate. And the bulk body peeled from the board | substrate can be used for each use, such as a target material, as it is by the manufacturing method which concerns on the 1st and 2nd invention.

In the present invention, the bulk body obtained by the production method according to the first and second inventions is dissolved and mixed together with the base material for the base metal made of the metal or the nonmetal or the compound constituting the base material, and cast and molded. , Dispersant concentration can be adjusted. The bulk composite material obtained by the production methods of the first and second inventions is a structurally ideal one in that the dispersant is very uniformly dispersed in the base material, but these two production methods are vapor growth. Since it is based on the method, when making into a bulk body which has a larger volume, it is necessary to carry out manufacture for a long time, and it is also difficult to obtain a complicated shape. Therefore, by dissolving, mixing and molding the bulk body and the base material obtained by these two methods together, the concentration of the dispersant is adjusted to produce a composite material having a larger bulk body. In the case of casting, when a mold having a predetermined shape is used, it is also easy to obtain a composite material having a complicated shape.

When dissolving, mixing, and molding the bulk body and the base material obtained by the first and second inventions, it is also conceivable that a phenomenon in which the dispersant separates from the base material occurs as in the conventional manufacturing method. In the first and second inventions, the bulk material is formed in a state where the base material and the dispersant are finely dispersed and combined, that is, since the dispersing material constitutes the bulk body in a state of high wettability with respect to the base material, Even if it melt | dissolves with a base material, a dispersing material does not isolate from a base material. Therefore, the composite material obtained by melt-molding and mixing a bulk material and a base material, and casting molding will be in the state which the dispersing material disperse | distributed to a base material very uniformly. Moreover, when manufacturing a composite material by dissolving a bulk body and a base material in this way, when forming a bulk body, the composite finally obtained by adding or subtracting the quantity of a dispersing material beforehand, or the amount of the base material for which it was added is added or subtracted. The composition control of the material can be easily performed.

The temperature at the time of melt | dissolving this bulk body and a base material raw material may be suitably determined by the composition of a composite material, and basically it may be performed in the range from the melting point temperature of a bulk body to evaporation temperature. In other words, it is sufficient to adjust the temperature such that the bulk body is in a sufficient flow state and the raw material for the base material to be introduced and the bulk body can be uniformly mixed. Although there is no restriction | limiting in particular in the atmosphere at the time of performing this melt | dissolution process, In a composite material with which a base material or a dispersing material is easy to oxidize, it is preferable to carry out in a vacuum atmosphere or inert gas atmosphere, such as argon. Moreover, when casting and molding after melting and mixing, it is preferable that the casting is to be quench solidified. This is because when cast under quench solidification conditions, the crystal structure of the composite material becomes fine and the dispersion material in the base material is very uniform and finely dispersed.

In addition, the bulk structure according to the first and second inventions, and the composite material obtained by dissolving, mixing, and molding the bulk body and the base material for the base material can be subjected to rolling processing or heat treatment to control the crystal structure. Finally, the composite material to be manufactured needs to have characteristics that can be adapted to each application. However, when the composite material has excellent characteristics, for example, strength properties, for each application, the crystal structure is subjected to rolling or heat treatment. This can be achieved by adjusting. In this case, you may use together a rolling process and a heat processing, and it can respond also by performing only rolling processing or heat processing.

In the method for producing a composite material according to the first and second inventions described above, it is preferable to deposit evaporated particles while rotating the substrate. By using a rotating substrate maintained at a predetermined rotational speed, deposition of evaporated particles proceeds uniformly in each part of the surface of the rotating substrate, and is more uniform in composition than in the case of depositing on a stationary substrate. This is because a bulk body having a thickness can be formed.

The substrate on which the evaporated particles are deposited is preferably made of the same material as the base material. This is because vapor deposition particles are deposited consistently with the substrate, whereby a uniform crystal structure is easily obtained. In addition, in the case of manufacturing a composite material by dissolving, mixing and casting the above-mentioned bulk body and the base material, if the material of the substrate is the same as the base material, the formed bulk body can be dissolved without peeling from the substrate, thus producing the process. Can be simplified.

In the method for producing a composite material according to the present invention, a composite material according to each use can be produced in general without being limited to its composition, the dispersion material is dispersed in a very uniform state in the base material, and the incorporation of impurities is controlled, In addition, a bulk composite material without internal defects such as a cavity can be obtained. Therefore, the composite material obtained by the manufacturing method of the present invention can be suitably used for each application, and is very suitable for structural materials such as automobile parts and aircraft parts, electrode materials, target materials for thin film formation, and the like.

Furthermore, in the composite material obtained by the production method of the present invention, it is very suitable as a target material to use aluminum as the base material and carbon as the dispersant. As described above, the aluminum thin film is used as an effective material for wiring of liquid crystal displays and semiconductor integrated circuits. Conventionally, when forming an aluminum thin film containing carbon by sputtering, it is known to use a so-called mosaic target material in which a chip made of carbon, silicon, or the like is embedded directly in an aluminum metal material (Japanese Patent Application Laid-Open No. 2-292821). report). However, such mosaic-like targets have been pointed out such as unevenness of the thin film composition to be formed and generation of dust, and have not been put into practical use as target materials for thin film formation. On the other hand, according to the composite material obtained by the production method of the present invention, carbon is very uniformly and finely dispersed in aluminum, which is a base material, and when the wiring material is formed using such a composite material as a target material, heat resistance and low resistance are achieved. Excellent wiring can be formed stably.

Embodiments preferred for the method for producing a composite material according to the present invention will be described. In the following first embodiment, the manufacturing method of the first invention described above will be described, and in the second embodiment, the manufacturing method of the second invention described above will be described.

1st Embodiment: This 1st Embodiment relates to the manufacturing method which forms a bulk body by evaporating a raw material for base materials and a raw material for dispersion materials by a sputtering method or a vacuum deposition method.

1-4 show the various manufacturing methods in this 1st Embodiment as a schematic diagram.

Fig. 1 shows a method of depositing a metal raw material composed of a base material and a nonmetal raw material composed of a dispersing material by sputtering to deposit a plate-like stationary substrate. In the chamber 1, a plate-like stop board 2 is provided, and a base metal target 4 and a base metal target 5 for dispersing material are placed on the base material 3 so as to face the stop board 2, respectively. We install thing which we equipped. The stationary substrate 2, each target 4, 5 is connected to a power supply not shown. The stationary substrate 2 is made of a base metal. Although the case where two targets, the metal target 4 for a base material, and the target 5 for a dispersing material are used is shown in FIG. 1, it is also possible to provide several targets more suitably according to the composition of the target composite material. .

Then, the chamber 1 is adjusted to a predetermined pressure by introducing an inert gas such as argon gas, and then stopped between the base metal target 4 and the stationary substrate 2 and the base metal target 5 for the dispersing material. Sputtering phenomenon is caused by applying a predetermined voltage between the substrate 2 and the base metal and the base metal for the dispersant are evaporated and deposited on the stationary substrate 2. The applied voltage may be applied to both targets 4 and 5 so as to cause sputtering at the same time, or may be applied so as to alternately cause sputtering. In FIG. 1, a DC pole sputtering system is described as an example, but a so-called high-frequency sputtering system or a magnetron sputtering system may be used.

When sputtering for a predetermined time is performed in this manner, a composite material of the bulk body 6 is formed on the stationary substrate 2. After the predetermined bulk body 6 is formed, the bulk body 6 is removed from the stationary substrate 2 by grinding or etching the stationary substrate 2 and the bulk body 6. As a single unit, it can be used for each use of structural materials, electrode materials and target materials. Although this bulk body 6 can also be used as it is, it is also possible to adjust and use a crystal structure by performing rolling process or heat processing as needed.

The composition of the composite material finally obtained by heating and melting together with the base metal prepared separately without adjusting the bulk body 6 from the stationary substrate 2 and adjusting the amount of the base metal prepared separately. In other words, the concentration of the dispersant may be arbitrarily determined. After heating to a predetermined temperature and dissolving to a certain flow state, the mixture is mixed so as to be uniform by sufficient stirring, and cast molding is carried out under rapid cooling and solidifying conditions to obtain a composite material having a desired composition and shape. If necessary, the crystal structure can be adjusted by rolling or heat treating the composite material.

Next, FIG. 2 shows a method of depositing a metal raw material composed of a base material and a nonmetal raw material composed of a dispersing material by vacuum evaporation to deposit a plate-like stationary substrate. In the chamber 1, a plate-like stop substrate 2 is provided, and a base metal deposition source 8 and a base metal deposition source 9 for dispersing materials are deposited on the deposition crucible 7 so as to face the stop substrate 2. We install thing equipped with. Both deposition sources 8 and 9 are connected to a power source (not shown). This vapor deposition source becomes effective when mass production of a composite material is made possible by supplying a rod-like thing continuously. The stationary substrate 2 is made of a base metal. Also in the case of the vacuum vapor deposition method demonstrated by this FIG. 2, it is also possible to install more deposition sources suitably according to the composition of the target composite material similarly to the case of FIG.

Then, the chamber 1 is depressurized to a predetermined pressure to obtain a vacuum atmosphere, and the evaporation sources 8 and 9 are heated by energizing the base metal deposition source 8 and the base metal deposition source 9 for dispersing materials. The base metal and the base metal for the dispersant are evaporated therefrom and deposited on the stationary substrate 2. In this way, when vapor deposition is performed for a predetermined time, a composite material of the bulk body 6 is formed on the stationary substrate 2. After the predetermined bulk body 6 is formed, as described in FIG. 1, the bulk material 6 may be used as a single bulk body 6, or dissolved, mixed, and cast together with the base metal to adjust the concentration of the dispersant. It can be used as a composite material. Further, if necessary, rolling processing or heat treatment can be performed to adjust the crystal structure.

3 and 4, a manufacturing method using the rotating substrate will be described. Fig. 3 shows a case where a bulk composite material is produced from a rotating substrate by the sputtering method. In the chamber 1, a cylindrical rotating substrate 10 is provided, and the base metal target 4 and the base metal for the dispersing material are disposed on the substrate 3 in a direction opposite to the rotating substrate 10 and perpendicular to each other. Each with the target 5 is installed.

Also in this case, argon gas is introduced into the chamber 1 and sputtering is performed by applying a predetermined voltage by a power source (not shown), so that the base metal and the base metal are rotated on the side surface of the rotating substrate 10. The nonmetals for the dispersant are deposited to form the bulk body 6 '. When the bulk body 6 'is formed using the rotating substrate in this way, the microstructure of the bulk body 6' is such that the base metal and the base metal for the dispersing material are stacked in the layer of angstroms. However, when the bulk body 6 'is used as a whole, the base metal and the base metal for the dispersant are uniform in composition, and the dispersant is very finely dispersed in the base material.

The bulk body 6 'formed on the rotary substrate can be used as it is as a composite material for each application as described in FIG. 1, and the bulk body 6' and the base metal are dissolved together to disperse the concentration of the dispersant. It can be used as a composite material adjusted. Furthermore, it is also possible to adjust the crystal structure by rolling or heat treatment. In addition, although FIG. 3 shows the case where two targets are used, it is naturally possible to provide three or more targets around a rotating board | substrate according to the composition of the target composite material. In addition, although the case by the sputtering method was demonstrated in this FIG. 3, the composite substrate of the bulk body 6 'can be similarly manufactured by the vacuum evaporation method using this rotating substrate 10. As shown in FIG. In the case of this vacuum evaporation method, since both targets 4 and 5 are basically replaced by each vapor deposition source in FIG. 3, detailed description is abbreviate | omitted.

4 shows a case where a bulk composite material is produced on a rotating substrate by using a sputtering method and a vapor deposition method together. In the chamber 1, a cylindrical rotating substrate 10 is provided, and a base metal target 4 is provided on the base material 3 in a direction opposite to and perpendicular to the rotary substrate 10. And the non-metal deposition source 9 for dispersing material are provided in the deposition crucible 7.

In this case, after argon gas is introduced and adjusted to a predetermined pressure, the base metal is evaporated by sputtering, while the base metal for the dispersing material is energized and heated until the vapor pressure of the non-metallic material becomes a temperature higher than the pressure in the chamber 1. To evaporate the base metal for the dispersion. Thereby, the base metal and the base metal for dispersing material are deposited on the side surface of the rotary substrate 10 to form the bulk body 6 '. The formed bulk body 6 'is obtained with a composite material having the same structure as that described in FIG. In addition, since handling of the bulk body 6 'is the same as that of description in FIG. 1, it abbreviate | omits.

Hereinafter, the Example which concerns on this 1st Embodiment is demonstrated.

Example 1 : This Example 1 is a case where an aluminum-carbon composite material is produced by using the rotary substrate shown in Fig. 3 by sputtering. Two kinds of materials were prepared: aluminum (purity 99.999%) as the base metal target and carbon (purity 99.9%) as the base metal target for the dispersant. The shape of both targets is 127 mm long, 279.4 mm wide, and 10 mm thick. The sputtering apparatus used the thing of the 3 cathode magnetron sputtering type, and used the 2 cathode of 3 cathodes. In addition, an octagonal cylindrical substrate in which eight stainless plates each having a length of 279 mm and a width of 80 mm were connected to each other was prepared. %) Was wound up and aluminum and carbon were deposited on this aluminum foil.

In sputtering conditions, argon gas is introduced into the chamber, the sputtering pressure is 0.87 Pa, the input power is 12 kW (24.8 W / cm 2) for the aluminum target, 4 kW (8.3 W / cm 2) for the carbon target, and the rotational speed of the rotating substrate is It was set as 30 rpm. Sputtering for about 30 hours was performed, and the bulk body of thickness 0.6mm was formed in the side surface of a rotating substrate. The cross-sectional structure of the formed bulk body is a state in which an aluminum layer having a thickness of about 0.3 μm and a carbon layer having a thickness of about 0.01 μm are laminated in terms of the film formation rate, and the carbon concentration in the bulk body is 2.6% by weight (5.6). Atomic percent).

This bulk was vacuum-dissolved together with separately prepared aluminum (purity 99.999%) to adjust the carbon concentration to a composition of aluminum-carbon at 0.7% by weight, and cast by water-cooled copper casting. As a result of microscopic observation that the casting was performed, it was confirmed that carbon was powdered in the Al-C (Al ₄ C ₃ ) phase in the aluminum of the base metal with a particle diameter of about 1 mm. The result of observing the dispersion state of the Al-C (Al ₄ C ₃ ) phase with respect to the aluminum-carbon composite material obtained in Example 1 is shown in FIG. 5. Of Figure 5, it is the portion shown by the black _{Al-C (Al 4 C 3} ).

The cast-molded aluminum-carbon (0.7 wt%) composite material was molded into a sputtering-gate material as described above, whereby an aluminum thin film was formed. As a film forming condition of the aluminum thin film, a DC magnetron sputtering device was used, and a thin film having a thickness of about 3000 Pa was formed on a glass substrate at a sputtering pressure of 0.333 Pa (2.5 mTorr) and an input power of 3 Watt / cm 2. The sputtering time required to form a thin film with a thickness of about 3000 mm 3 was about 100 seconds. After forming a thin film of 3000 mm, the glass substrates were replaced to further form a thin film. By repeating this thin film formation operation, a long time thin film formation was performed continuously with one sputtering gate material. In addition, the occurrence of hillock, which is a heat-resistant property, was investigated for the first thin film formed, the thin film when the sputtering time passed about 20 hours, and the thin film when the sputtering time passed about 40 hours. It was. This hillock refers to a curve-like protrusion that is generated on the surface of the thin film when the glass substrate with the thin film is subjected to heat treatment at a temperature of 300 ° C. for a predetermined time. As a result, it was confirmed that the hillock was hardly generated in each thin film without being limited to the sputtering time of the total. Moreover, when the electrical resistivity of each thin film was measured, it turned out that it is a resistivity of about 5 micrometer cm in an optimal condition. These results are quite excellent as wiring characteristics of a liquid crystal display or a semiconductor integrated circuit. Therefore, when the composite material obtained in Example 1 is used as a raw material of the target material, it has been found that a thin film having excellent thin film characteristics can be stably formed.

Comparative Example 1 : This Comparative Example 1 is based on an anti-melt stirring method. 2 kg of aluminum (purity 99.999%) was heated to about 700 ° C. in a carbon crucible and dissolved once, and then cooled to 640 ° C. to obtain a semi-melt state (solid liquid coexistence state). In this state, 15 g of carbon powder having an average particle diameter of 150 µm was added to the molten aluminum, and stirred with a stirrer, followed by longitudinal casting with a water-cooled copper mold. The obtained ingot was 200 mm long x 200 mm wide 20 mm thick, and the carbon concentration of the portion corresponding to the bottom side of the copper mold was examined to be 0.003 to 0.008% by weight, and almost no carbon was dispersed. It became. As a result of visual observation, this ingot was confirmed that carbon segregated on the upper part of the ingot. It is assumed that the anti-melt stirring method has little wettability between aluminum and carbon, and that carbon is separated from aluminum and floated upward due to the difference in specific gravity between aluminum and carbon.

Second Embodiment In this second embodiment, a raw material for evaporation is evaporated in a mixed atmosphere of an inert gas such as argon gas with any gas of hydrocarbon gas, oxygen gas or nitrogen gas, and evaporated particles on a substrate. It relates to a manufacturing method of forming a bulk body by depositing. 6 and 7 show various manufacturing methods in this second embodiment as a schematic view. FIG. 6 shows the case by the sputtering method and FIG. 7 shows the case by the vapor deposition method.

In the case of the sputtering method, as shown in FIG. 6, a plate-like stationary substrate 2 is provided in the chamber 1, and dispersed with a base metal on the substrate 3 so as to face the stationary substrate 2. An evaporation target 11 made of a nonmetal for reuse is provided. The stationary substrate 2 and the evaporation target 11 are connected to a power source 12. The stationary substrate 2 is made of a base metal. In FIG. 6, a direct current two-pole sputter is described as an example, but a so-called high frequency sputter or a magnetron sputter can be applied.

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 gas such as acetylene gas and an inert gas such as argon gas are supplied. The mixed atmospheric gas is supplied, and this atmospheric gas is introduced into the chamber 1.

After adjusting the inside of the chamber 1 to a predetermined pressure, a predetermined pressure is applied to cause sputtering, and the base metal and the base metal for the dispersant are evaporated from the evaporation target 11. At this time, hydrocarbon gas such as acetylene gas introduced into the chamber 1 is decomposed into carbon and hydrogen. For example, the carbon is blown into the bulk body 6 formed on the stationary substrate 2 together with the base metal or the dispersing base metal to be evaporated. Is generated and blown into the bulk body 6 formed on the stationary substrate 2 in the state of the carbide. In this case, it is possible to appropriately determine the carbon concentration in the composite material formed as the bulk body 6 by adjusting the amount of hydrocarbon gas in the atmosphere gas introduced into the chamber 1 or the applied voltage during sputtering. .

Next, the case by the vapor deposition method shown in FIG. 7 is demonstrated. In FIG. 7, a plate-shaped stop substrate 2 is provided in the chamber 1, and a deposition source 15 composed of a base metal and a base metal for dispersing material is disposed in the deposition crucible 7 so as to face the stop substrate 2. We install thing which we equipped. This vapor deposition source 15 is connected with the power supply which is not shown in figure. As described in the first embodiment, the vapor deposition source 15 is effective when mass production of a composite material is made possible if the rod-like material can be continuously supplied. The stationary substrate 2 is made of a base metal.

The chamber is provided with an atmosphere gas inlet 13 and an atmosphere gas outlet 14, and an atmosphere in which a hydrocarbon gas such as acetylene gas and an inert gas such as argon gas are mixed from the atmosphere gas inlet 13. Gas is supplied and this atmospheric gas is introduced into the chamber 1. Thereafter, the deposition source 15 is energized and heated at a predetermined pressure to evaporate the base metal and the base metal for the dispersant, and the evaporated particles pass through the acceleration probe electrode 16 and are deposited on the stationary substrate 2. do. At this time, hydrocarbon-based gas such as acetylene gas introduced into the chamber 1 is decomposed into carbon and hydrogen as in the case of FIG. 6, and the decomposed carbon is together with the base metal or the base metal for dispersing which evaporates. It is blown into the bulk body 6 formed on the stationary substrate 2, and reacts with the base metal for evaporation or the base metal for dispersant to produce stable carbide, and is formed on the stationary substrate 2 in the state of the carbide. Blown into the bulk body (6). In this case, the carbon concentration in the bulk body 6 can be appropriately determined by adjusting the amount of hydrocarbon gas in the atmosphere gas introduced into the chamber 1 and the energizing heating temperature at the time of vapor deposition.

After the predetermined bulk body 6 is formed by the manufacturing method described with reference to Figs. 6 and 7, the same as the description in the first embodiment is used as the bulk body 6 of a single body or the base metal. It can be used as a composite material which is melted, mixed and cast together with the concentration adjustment of the dispersant. In addition, as necessary, the crystal structure can be adjusted by rolling or heat treatment.

Hereinafter, the Example which concerns on 2nd Embodiment is demonstrated.

Example 2 In this Example 2, the case where an aluminum-carbon composite material was produced by the sputtering method shown in FIG. The apparatus used reactive magnetron sputtering apparatus, and used disk shaped aluminum (purity 99.999%) of diameter 203.2mm and thickness 10mm as a sputtering target. In addition, an aluminum (purity 99.999%) foil having a thickness of 10 μm was used as the stationary substrate.

Into the chamber, a mixed gas of argon gas (purity 99.999%) and gas flow rate 20ccm acetylene gas (purity 99.5%) was supplied, and the sputtering pressure was adjusted to 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.

The sputtering for 60 minutes was performed, and the bulk body of thickness 80micrometer and a total amount of 6.14g was formed on the stationary substrate. As a result of gas analysis of the carbon concentration of the formed bulk body, it was found that the bulk body contained 2.4% by weight of carbon.

The bulk was vacuum-dissolved together with separately prepared aluminum (purity 99.999%) to adjust the composition so as to have a composition of aluminum-carbon having a carbon concentration of 0.7% by weight, and casting was performed by a water-cooled copper mold. As a result of microscopic observation of the casting molding, carbon was uniformly dispersed in the Al-C (Al ₄ C ₃ ) phase around 1 mm in diameter in the aluminum of the base material as in the observation photograph shown in FIG. It was confirmed that there was.

The cast-molded aluminum-carbon (0.7 wt%) composite material is processed into a sputtering target material as described above, whereby an aluminum thin film is formed under the same conditions as in Example 1, and the thin film is formed. The properties were investigated. As a result, when the aluminum-carbon composite material obtained in Example 2 is used as a raw material of the target material, it is possible to stably form a thin film having excellent heel resistance and low electric resistivity as in the case of Example 1. Confirmed.

As described above, according to the manufacturing method of the composite material according to the present invention, it is possible to disperse the dispersion material more uniformly in the base material of the composite material than in the conventional method of manufacturing the composite material, and is not limited to the composition of the composite material, The composite material of can be manufactured universally. In the composite material obtained by the manufacturing method of the present invention, since the dispersant is very uniformly dispersed in the base material and there are no internal defects such as cavities, the composite material satisfies the required characteristics of the constituent material and the electrode material and the like. It becomes appropriate. In particular, when used as a target material in the case of forming the wiring of a liquid crystal display or a semiconductor integrated circuit, it is possible to stably realize the required thin film characteristics.

Claims (9)

As a method for producing an aluminum-based composite material comprising aluminum as a base material and carbon being dispersed as a dispersant, A method for producing an aluminum-based composite material, characterized in that the base material made of aluminum or an aluminum compound and the raw material for dispersing material of the dispersing material are evaporated simultaneously or alternately to deposit these vaporized particles on a substrate to form a bulk body. . As a method for producing an aluminum-based composite material comprising aluminum as a base material and carbon being dispersed as a dispersant, A method for producing an aluminum-based composite material, characterized by evaporating a raw material for evaporation made of aluminum or an aluminum compound in a hydrocarbon gas atmosphere to deposit evaporated particles on a substrate to form a bulk body. A method for producing an aluminum-based composite material characterized by adjusting the concentration of carbon as a dispersant by dissolving and mixing the bulk body produced by the method according to claim 1 or 2 with aluminum as a base material and casting the same. . A method for producing an aluminum-based composite material, characterized in that the crystal structure is adjusted by rolling or heat-treating the aluminum-based composite material produced by the method of claim 3. The method according to claim 1 or 2, The evaporation of a raw material is performed by the sputtering method, The manufacturing method of the aluminum type composite material characterized by the above-mentioned. The method according to claim 1 or 2, A method for producing an aluminum-based composite material, comprising depositing evaporated particles while rotating a substrate. The method according to claim 1 or 2, The substrate is a manufacturing method of the aluminum-based composite material, characterized in that using the same material as the base material. An aluminum-based composite material produced by the method according to claim 3. delete