CN1250766C - Method for producing composite material and composite material produced by the method - Google Patents

Abstract

The present invention relates to a method of manufacturing a composite material comprising two or more metals or non-metals and their compounds, and in particular to a manufacturing method in which a dispersion material is dispersed very uniformly in a matrix of the composite material, without the applicability depending on the composition of the composite material. The invention is characterized in that a base material of a metal or nonmetal or a compound thereof constituting a base material and a raw material of at least one dispersion material of a metal or nonmetal or a compound thereof constituting a dispersion material are simultaneously or alternately evaporated, and the evaporated particles are deposited on a substrate to form a bulk.

Description

Method for producing composite material and composite material produced by the method

technical field

The present invention relates to a kind of method of making the composite material that comprises two or more metals or metalloids and their compound, particularly, the present invention relates to dispersing material very uniformly in composite material base material, and applicability Does not depend on the manufacturing method of the composite material.

Background technique

Composite materials including metals, or nonmetals, or their compounds are widely used in various applications, such as structural materials for automotive parts, aircraft parts, etc., electrode materials, target materials for film formation, and the like. Composite materials are produced by dispersing metals or nonmetals or their compounds different from the base material in the base material, controlling the properties of the material, and making the material have properties suitable for various purposes. The term "nonmetal" used herein includes hydrogen, boron, carbon, silicon, nitrogen, phosphorus, etc., and when used as a broad concept, also includes antimony, bismuth, etc., which are called semimetals.

As methods for producing the above-mentioned composite materials, composite casting and powder metallurgy are known. In the composite casting method, the metal used as the base material is in a semi-molten state, and the non-metallic particles used as the dispersion material are poured into the semi-molten metal, and vigorously stirred to force the non-metallic particles to disperse in the base material. This approach is effective when making composites using non-metallic particles that are poorly wettable with molten metal as a substrate. Using this method, composites are fabricated in a semi-molten state to prevent separation of the non-metallic material from the substrate. However, in the compound casting method, since the semi-molten state is in a state called jelly, defects such as holes easily occur in the resulting shaped product, causing gas to be trapped therein, thereby reducing the density of the material.

Typical representatives of the powder metallurgy method are hot pressing and hot isostatic pressing (HIP). In this method, the metal powder used as the base material and the non-metallic powder used as the dispersion material are mixed in a predetermined ratio, and then processed after forming. Sintering to make composite materials. In this method, for metals that are easily oxidized, since the raw material is powder, the oxygen concentration in the composite material is relatively high, so it is sometimes difficult to control the properties of the composite material. In powder metallurgy, it is sometimes difficult to uniformly disperse the dispersion material in the substrate due to limitations in powder control and mixing processes.

In addition to composite casting and powder metallurgy, fusion casting is generally used. However, in the case where both the base material and the dispersion material are metals, respectively low-melting-point metals and high-hot-point metals, for example, it is difficult to manufacture such a metal-metal composite material by vacuum melting.

Now, taking the sputtering target material as an example, the composite material prepared by the conventional manufacturing method will be described in detail. In recent years, wiring technology using a target material sputtering method using a composite material has been used in forming circuits of liquid crystal displays or semiconductor integrated circuits. When forming circuits by sputtering, an aluminum film with high thermal resistance and low resistance is usually used. Here, a composite material based on aluminum is used as a sputtering target material to form an aluminum film.

For an aluminum film used as a circuit of a liquid crystal display or a semiconductor integrated circuit, for example, in a composite material as a target material, aluminum is a base material in which carbon and a Group IVa metal such as titanium are dispersed. This is because if such a composite material composed of aluminum is used as a target material, a circuit with high thermal resistance and low resistance can be formed, and interruption of the circuit due to stress can be prevented. For this reason, it is generally necessary to use a composite material composed of aluminum as the target material, the composition of which can form a film that meets the requirements for circuit characteristics. Moreover, it is required that the target material has fewer defects such as holes and voids, has a high density, and rarely entrains gases that form impurities.

With the prior art, although it is possible to use aluminum as the base material and carbon and IVa group metals as dispersed materials to manufacture a composite material, it is difficult for the composite material to meet the requirements of the target material for forming the circuit. Specifically, even if the above-mentioned target material composed of aluminum is produced by composite casting, powder metallurgy, or fusion casting, there is a limit to the uniformity of dispersion of carbon and Group IVa metal in the aluminum substrate, and as a result, the resulting composite material cannot be effectively It is also used as a target material to stably form circuits that meet the requirements of actual circuit characteristics. In order to use a composite material as a target material, a bulk body having a certain volume is required. However, if a composite material for a bulk object is formed by a conventional manufacturing method, internal defects such as holes are generated, so that the density of the bulk object decreases. Gases and other impurities also enter the material in many cases. Therefore, even though a bulk object manufactured by a conventional method can be used as a target material, it is still difficult to stably form lines by sputtering.

As can be seen from this target material example, conventional methods of manufacturing composite materials can disperse the dispersed material into the substrate, but the degree of dispersion is insufficient, resulting in internal defects and entrained impurities in the bulk object. Therefore, there are many defects that need to be improved in the commonly used composite materials. In addition to being used as target materials, for the manufacture of composite materials for other purposes, such as structural materials or electrode materials for automotive parts, aircraft parts, etc., it is usually difficult to manufacture composite materials with different compositions by conventional manufacturing methods.

In view of the above circumstances, the present invention has been made, and therefore, an object of the present invention is to provide a method for producing a composite material comprising two or more metals or nonmetals and their compounds, in which the dispersed material is very uniformly dispersed in In contrast to conventional fabrication methods for composite substrates, the applicability of this method is generally independent of the composition of the composite.

Contents of the invention

In order to solve the above-mentioned problems, the present inventors have actively conducted research, focusing attention on a vapor phase epitaxy technique for forming a film. As a result, a method of manufacturing a composite material, which cannot be manufactured by conventional manufacturing methods, is accomplished.

First of all, the first invention provided by the present inventors is a method of manufacturing a composite material using a metal or nonmetal or their compound as a base material and at least one metal or nonmetal or their compound different from the base material as the dispersed material is dispersed in a substrate, in which process the raw materials forming these substrates of metals or nonmetals or their compounds and at least one raw material forming these dispersed materials of metals or nonmetals or their compounds are evaporated simultaneously or alternately, Particles formed by evaporation and condensation are deposited on the substrate to form massive objects.

In this first invention, the raw material forming the substrate and the raw material forming the dispersed material are formed into evaporated particles by a method called physical vapor deposition (PVD method), and the evaporated particles are deposited on the substrate to form a lump. According to the first invention, since the raw material forming the base material and the raw material forming the dispersed material can be deposited in the form of evaporated particles, unlike conventional manufacturing methods, the dispersed material can be dispersed very uniformly in the base material, therefore, it is easy to manufacture All kinds of composite materials have nothing to do with the nature of raw materials. That is, a composite material composed of a high-melting-point metal and a low-melting-point metal can be easily produced.

In this first invention, it is preferable to use the sputtering method or the vacuum deposition method among the physical vapor deposition methods. The reason is that, in these methods, evaporated particles are produced from each raw material at a relatively high rate, and a lump having a predetermined volume tends to be formed. When the sputtering method or the vacuum deposition method is applied to the first invention, even easily oxidized raw materials can be used since the raw materials are evaporated in an inert atmosphere such as argon or under vacuum conditions. Therefore, it is possible to control the oxygen content entering the obtained block and avoid the entry of gas and other impurities as much as possible. Also, it is possible to manufacture bulk objects of composite material with few internal defects.

In this first invention, the raw material of the substrate and the raw material of the dispersion material can be evaporated simultaneously or alternately. In the case where the raw materials are evaporated and deposited at the same time, the deposition of the raw materials of the base material and the raw materials of the dispersion material after evaporation is disordered. Even in the case of alternate evaporation of raw materials, as long as the deposition layer of the substrate and the deposition layer of the dispersed material are controlled in the order of angstroms, a composite material in which the dispersed material is uniformly dispersed in the substrate macroscopically can be produced. In the first invention, the sputtering method is preferably used for evaporating the raw material in consideration of the fact that the lump is formed in a relatively short time.

Next, as a second invention, the present inventors have invented a method of manufacturing a composite material using a metal or nonmetal or their compound as a base material, and at least one metal or nonmetal different from the base material Or their compounds are dispersed in the substrate as a dispersion material, in this method, the raw material used for evaporating the metal or nonmetal or their compounds forming the substrate or the metal or nonmetal or their compounds forming the dispersion material is in the hydrocarbon Evaporate in any atmosphere of gas-like gases, oxygen and nitrogen, and the evaporated particles are deposited on the substrate to form block objects.

This second invention is based on physical vapor deposition (PVD) or chemical vapor deposition (CVD). For the atmosphere for evaporating raw materials, any one of hydrocarbon gas, oxygen and nitrogen can be selected, so that in the manufactured composite material, carbides, nitrides or oxides are dispersed very uniformly in the substrate as dispersion materials. For evaporating the raw material for evaporation in the second invention, sputtering method among physical vapor deposition methods and vacuum deposition method or activation deposition method among chemical deposition methods are preferably used.

There is no particular limitation on the composition of the hydrocarbon gas used in the second invention as long as the gas can be decomposed into carbon and hydrogen during sputtering or deposition. Preferable are methane, ethane and acetylene gases. In the second invention, the atmosphere for evaporating the raw material may further contain an inert gas such as argon, thereby controlling the evaporation efficiency of the raw material.

In the second invention, it is possible to use an evaporating raw material comprising a metal or a nonmetal or a compound thereof forming a substrate, or an evaporating raw material comprising a metal or a nonmetal or a compound thereof forming a dispersed material in addition to the substrate forming . For example, using an evaporated raw material containing copper for forming the substrate and silicon for forming the dispersed material, the evaporated particles are deposited on the substrate by sputtering in nitrogen gas, where the silicon and nitrogen react with each other to produce a stable nitrogen Silicon. Therefore, in the manufactured composite material, silicon nitride is the dispersed material, which is very uniformly dispersed in the copper as the base material. Also, using an evaporation raw material containing copper for forming a substrate and aluminum as a dispersed material, vaporized particles are deposited on the substrate in oxygen by sputtering, where aluminum and oxygen react with each other to produce stable alumina . Therefore, in the manufactured composite material, alumina is the dispersed material, which is very uniformly dispersed in the copper as the base material.

According to the second invention, a composite material in which the dispersion material is very uniformly dispersed in the base material even if the wettability of the dispersion material and the base material is poor, which cannot be produced by conventional manufacturing methods, can be produced. By controlling the atmosphere used for the evaporation of raw materials, the ingress of impurities can be limited to the greatest extent, and massive objects with almost no internal defects can be produced. In the second invention, it is preferable to evaporate the raw material by the sputtering method in consideration of the fact that the lumpy body is formed in a relatively short period of time.

The composite material obtained by the manufacturing method of the above-mentioned first invention and the second invention of the present invention is a bulk object deposited on a substrate. It is not difficult to hold this bulky object like a normal object, which is different from the material called membrane. After the bulk object is separated from the substrate, the bulk object has a certain volume so that it can be held as it is. The bulk objects produced by the method of the first invention and the second invention separated from the substrate can be used for various purposes, for example, as a target material.

In the present invention, the block-shaped objects obtained by the production methods of the first invention and the second invention of the present invention can also be melted, mixed and cast together with raw materials of metal or non-metal or their compounds forming the base material, The concentration of the dispersed material is controlled through this process. In the manufacturing methods of the first and second inventions, the composite material of the block-like objects obtained is structurally ideal, since the dispersed material is very uniformly dispersed in the base material. However, these two manufacturing methods are based on the vapor phase epitaxy growth method, and it takes a long time to manufacture massive bulk objects, and it is also difficult to obtain bulk objects with complex shapes. Therefore, the bulk objects obtained by these two methods are melted, mixed and cast together with the raw materials used as base materials to control the concentration of dispersed materials, so as to manufacture composite materials of larger bulk objects. Composite materials with complex shapes can be easily produced if a mold of a predetermined shape is used during casting.

Melting, mixing, and casting the bulk objects obtained in the first and second inventions with the raw materials for the base material may cause separation of the dispersed material from the base material, as in conventional manufacturing methods. However, in the first invention and the second invention of the present invention, the state in which the bulk object is formed is that the base material and the dispersion material are very finely dispersed with each other, that is, in the state of the formed mass object, the dispersion material is very finely dispersed to the base material. Has high wettability. Therefore, even if the mass is melted together with the raw material of the base material, the dispersed material is not separated from the base material. Therefore, the state of the composite material obtained by melting, mixing and casting the bulk body and the base material raw materials is that the dispersion material is very uniformly dispersed in the base material. If the bulk object and base material are melted in this way to make a composite material, when forming the block object, the amount of dispersion material added or the amount of base material should be controlled in advance, so that it is easy to control the composition of the final obtained composite material .

Depending on the composition of the composite material, the appropriate temperature for melting the bulk and substrate raw materials can be determined. Generally, the melting is carried out in the range from the melting point of the bulk object to the evaporation temperature. In effect, the temperature can be controlled to make the bulk object into a fully fluid state, and the base material and the material of the bulk object can be uniformly mixed with each other. There is no particular limitation on the atmosphere in which the melting is performed. For composite materials in which the substrate or dispersed material is easily oxidized, it is preferable to melt in a vacuum environment or in an inert gas environment such as argon. Also, when casting is performed after melting and mixing, it is preferable to perform casting under conditions of rapid solidification. This is because if the casting is performed under rapid solidification conditions, the crystal structure of the composite material is fine, and the dispersed material can be finely and uniformly dispersed in the matrix.

The crystal structure of the bulk body formed according to the first invention and the second invention, and the composite material obtained by melting, mixing and casting the bulk body and base materials is controlled by rolling or heat treatment. The resulting composite can have properties suitable for its use. By controlling its crystal structure by rolling or heat treatment, a composite material with properties suitable for the purpose such as high strength can be obtained. At this time, rolling and heat treatment can be used, or only one of them can be used.

In the method of manufacturing a composite material according to the first invention and the second invention, evaporated particles are preferably deposited on a rotating substrate. Using a substrate that rotates at a predetermined constant rotational speed, evaporated particles can be uniformly deposited on the entire surface of the rotating substrate, and therefore, can be formed with a higher composition and thickness than in the case of depositing evaporated particles on a static substrate. Uniform lumpy objects.

Furthermore, the substrate on which the evaporation particles are deposited is preferably composed of the same material as the substrate. In this case, the deposited particles are deposited on the substrate with the same structure, so it is easy to obtain a uniform crystal structure. In the case of composites produced by melting, mixing and casting block and substrate raw materials, the block can be produced without delamination from the substrate if the block is made from the same substrate as the substrate it contains Melting simplifies the manufacturing method.

Composite materials suitable for various purposes can be produced by using the method for manufacturing composite materials of the present invention. The applicability of the method generally does not depend on its composition, and the dispersed materials can be dispersed in the base material very uniformly, which limits the entry of impurities and can A bulk object composite material free of internal defects such as voids is produced. Therefore, the composite material obtained by the manufacturing method of the present invention can actually be used in various applications, and is particularly suitable for use as structural materials for automotive parts, aircraft parts, etc., electrode materials, or target materials for film formation.

Moreover, by adopting the manufacturing method of the present invention, aluminum is used as the base material and carbon is used as the dispersion material, and the obtained composite material is particularly suitable as the target material. As described above, the aluminum film can be effectively used as a wiring of a liquid crystal display or a semiconductor integrated circuit. Can use the target material called mosaic in the known technology, in this material, when adopting sputtering method to form carbon-containing aluminum film, the chip of carbon or silicon is directly embedded in aluminum metal material as sputtering material ( Japanese Patent Laid-Open No. 2-292821). However, with this type of mosaic target material, it has been pointed out that there are problems in the non-uniformity of the formed film composition and the occurrence of dust, so this type of target material has not been practically used to form aluminum films. However, in the composite material obtained by the manufacturing method of the present invention, the carbon is finely and evenly distributed in the aluminum as the base material. Therefore, if such a composite material is used as a target material for forming wiring, it is possible to stably form wiring with high thermal resistance and low electrical resistance.

Brief description of the drawings

Fig. 1 is the schematic diagram that sputtering method forms the situation of massive object on static substrate;

Fig. 2 is the schematic diagram that vacuum deposition method forms the situation of massive object on static substrate;

Fig. 3 is the schematic diagram that sputtering method forms the situation of massive object on rotating substrate;

Fig. 4 is the schematic diagram that sputtering method and vacuum deposition method form bulk object situation on rotating substrate;

Fig. 5 is the cross-sectional micrograph of the composite material cast through water cooling in embodiment 1;

Fig. 6 is the schematic diagram that adopts sputtering method to form the situation of massive object on static substrate under the situation of feeding hydrocarbon gas;

Fig. 7 is a schematic diagram of the formation of massive objects on a static substrate by a deposition method under the condition of feeding hydrocarbon gas.

Best Mode for Carrying Out the Invention

Some preferred embodiments of the method for producing composite materials of the present invention are described below. The first embodiment relates to the production method of the aforementioned first invention, and the second embodiment relates to the production method of the aforementioned second invention.

The first embodiment: In the manufacturing method related to the first embodiment, the raw material of the base material and the raw material of the dispersed material are evaporated to form a bulk object by sputtering method or vacuum deposition method. 1 to 4 are schematic views showing various manufacturing methods of the first embodiment.

In the method shown in FIG. 1 , metal raw materials are used as substrates and non-metallic raw materials are used as dispersion materials, and these raw materials are evaporated by sputtering to deposit on static substrate plates. A static substrate plate 2 is installed in the chamber 1 , on each substrate 3 a metallic target 4 for the substrate and a non-metallic target 5 for the dispersed material are placed, facing the static substrate 2 . The static substrate 2 and the targets 4 and 5 are connected to a power source (not shown in the figure). The static substrate 2 may also be formed from the metal used for the substrate. Although FIG. 1 shows the use of two targets, a metallic target 4 for the base material and a non-metallic target 5 for the dispersed material, multiple targets may be provided as appropriate depending on the composition of the final composite material.

An inert gas such as argon is introduced into the chamber 1, and the pressure of the gas is controlled to a predetermined value. After that, a voltage is applied between the metal target 4 for the base material and the static base material 2 and between the non-metallic target 5 for the dispersed material and the static base material 2, causing a sputtering phenomenon, so that the Metals and non-metals for dispersing materials are then evaporated and then deposited on the static substrate 2 . A voltage is applied to cause sputtering on the targets 4 and 5 at the same time, or a voltage can be applied to alternately cause sputtering. Although a DC 2-pole sputtering system is shown in FIG. 1, a high frequency sputtering system or a magnetron sputtering system may be used.

Sputtering is performed in this way for a given period of time, and lumps 6 are formed on the static substrate 2 . After forming a predetermined mass, the mass 6 is removed from the substrate 2 by grinding or etching the static substrate 2 . Thus, this common bulk object can be used for various purposes such as structural material, electrode material or target material. Although the bulk can be used untreated, it can be rolled or heat treated if it is desired to control its crystal structure.

It is also possible not to remove the bulk object 6 from the static substrate 2, but to heat and melt the bulk object 6 and the static substrate 2 together with the separately prepared base metal. By controlling the amount of additionally prepared substrate metal, the composition of the finally obtained composite material, ie the concentration of dispersed materials therein, can be artificially determined. After these materials are heated to a predetermined temperature and melted to a certain degree of flowable state, they are fully stirred and mixed evenly, and then cast and formed under rapid solidification conditions. In this way, composite materials with required composition and shape can be obtained. Also, the composite material can be rolled or heat treated to control the crystal structure, if desired.

In the method shown in FIG. 2 , metal raw materials are used as substrates, and non-metallic raw materials are used as dispersed materials. These raw materials are evaporated by vacuum deposition and deposited on static substrate plates. A plate-shaped static substrate 2 is mounted in the chamber 1, and within each deposition crucible 7 is placed a metallic deposition source 8 for the substrate and a non-metallic deposition source 9 for the dispersed material, facing the static substrate 2. The deposition sources 8 and 9 are connected to a power source (not shown in the figure). If the structure of the deposition source is a rod-shaped source that can be supplied continuously, the composite material can be efficiently mass-produced. The static substrate 2 is also formed from the metal used for the substrate. In the vacuum deposition method shown in FIG. 2 , as in the case shown in FIG. 1 , multiple deposition sources can also be appropriately provided according to the composition of the final composite material.

The chamber 1 is evacuated to a predetermined pressure, creating a vacuum environment. The metal deposition source 8 for the substrate and the non-metal deposition source 9 for the dispersed material are heated by current flow, the metal for the substrate and the non-metal for the dispersed material are evaporated from the deposition sources 8 and 9, respectively, and deposited on Static Substrate 2. Deposition is carried out in this way for a certain period of time, forming a composite material of block-like objects on the static substrate 2 . As in the case shown in FIG. 1, after forming a predetermined block object 6, the block object 6 can be used as a single common object, or it can be melted, mixed and cast with the metal used for the base material to control the dispersed material. The concentration becomes the answering material, and if necessary, the composite material can be rolled or heat treated to control its crystal structure.

Referring to Figures 3 and 4, a manufacturing method using a rotating substrate will now be described. Figure 3 shows the fabrication of bulk objects on a rotating substrate by sputtering. A rotating cylindrical substrate 10 is installed in the chamber 1, on each substrate 3 a metal target 4 for the substrate and a non-metallic target 5 for dispersing the material are placed, the target faces the rotating substrate 10, the target 4 and 5 are at right angles to each other.

In this case, argon gas is also introduced into the chamber 1, and a voltage is applied by a power source (not shown in the figure) to carry out sputtering, so that the metal used for the substrate and the non-metal used for the dispersed material are deposited on the rotating cylinder. On the peripheral surface of the substrate 10, a block-shaped object 6' is formed. In this manner, a rotating substrate is used to form a block 6' whose microstructure is the metal for the base material and the non-metal for the dispersed material deposited in alternating layers on the order of angstroms. However, the bulk object 6' has a uniform composition of the metal used for the base material and the non-metal used for the dispersed material from a macroscopic point of view, and the dispersed material is finely dispersed in the base material.

As in the case shown in Figure 1, the block-shaped object 6' formed on the rotating substrate can be used as a composite material for various purposes, and it is not necessary to process it, and it can also be melted together with the base metal to control the dispersion of the material. Concentration, casting into composites. Moreover, the composite material can be controlled in its crystal structure by rolling or heat treatment. Although Figure 3 shows the use of two targets, three or more targets may be provided around the rotating substrate, depending on the desired composition of the composite material. The description in conjunction with FIG. 3 is only used to illustrate the case of using the sputtering method. In the same way, the vacuum deposition method can also be used to manufacture the composite material of the bulk object 6' by using the rotating substrate 10. When using the vacuum deposition method, as long as the targets 4 and 5 in FIG. 3 are replaced by deposition sources, the detailed description thereof is omitted.

Figure 4 shows the use of two methods, sputtering and vacuum deposition, to manufacture bulk composites on a rotating substrate. A rotating cylinder substrate 10 is installed in the chamber 1, a sputtering target 4 for the substrate is placed on the substrate 3, and a non-metallic deposition source 9 for dispersing materials is placed in the deposition crucible 7, all of which are useful for Rotating substrates 10 are at right angles to each other.

In this case, after argon gas is introduced and its pressure is controlled to a predetermined value, the metal used for the base material is evaporated by sputtering, and on the other hand, the non-metal used for the dispersed material is heated by current flow until its temperature reaches a non-metallic state. The temperature at which the vapor pressure of the metal substance is higher than the pressure in the chamber 1 vaporizes the non-metal used to disperse the material. As a result, the metal for the base material and the non-metal for the dispersion material are deposited on the peripheral surface of the rotating substrate 10, forming lumps 6'. The formed bulk object composite material 6' has the same structure as that described in FIG. 3 and can also process the bulk object 6' in the same manner as described in FIG. 1, and its description is omitted.

Some examples of the first embodiment are described below.

Example 1

Example 1 represents the production of an aluminum-carbon composite material using the rotating substrate shown in FIG. 3 by the sputtering method. Two kinds of materials were prepared, namely, a metal target using aluminum (purity: 99.999%) as a base material and a non-metallic target using carbon (purity: 99.9%) as a dispersion material. The two targets are 127mm long, 279.4mm wide and 10mm thick. As the sputtering device, a 3-cathode magnetron sputtering type device using two of the three cathodes can be used. The rotating bottom material of octahedron shape is manufactured by connecting the long sides of eight stainless steel plates (each length 279mm, width 80mm) to each other. A 12 µm thick aluminum foil (measurement: 99.999%) was wound on the side of the rotating substrate, on which aluminum and carbon were deposited.

The sputtering conditions are as follows: argon gas is introduced into the chamber, the sputtering pressure is 0.87Pa, the applied electric power is 12kw (24.8W/cm ² ) for the aluminum target, 4kw (8.3W/cm ² ) for the carbon target, and the rotating bottom The rotation speed of the material was 30 rpm. Sputtering was carried out for 30 hours, forming a 0.6 mm thick lump on the side of the rotating substrate. In the cross-sectional structure of the formed bulk object, an aluminum layer with a thickness of about 0.3 μm and a carbon layer with a thickness of about 0.01 μm were stacked, and the thickness was converted from the film formation rate. Chemical analysis indicated a carbon concentration of 2.6% by weight (5.6% by atomic weight) in the bulk.

The bulk object was melted together with separately prepared aluminum (purity: 99.999%) under vacuum so that the composition of aluminum carbon was controlled so that the carbon concentration was 0.7% by weight, and casting was performed using a water-cooled copper mold. The cast-formed composite was observed under a microscope. The results confirmed that carbon was dispersed in the aluminum substrate with a particle size of about 1 mm in the form of Al—C (Al ₄ C ₃ ) phase. FIG. 5 shows the observation results of the dispersion state of Al—C (Al ₄ C ₃ ) in the aluminum-carbon composite material obtained in Example 1. FIG. In Fig. 5, the black portion represents the Al-C (Al ₄ C ₃ ) phase.

The aluminum-carbon (0.7% by weight) composite material formed by the above casting was used as a target material for sputtering, and an aluminum film was formed using this target material. The conditions for forming the aluminum film are as follows: DC magnetron sputtering equipment is used, the sputtering pressure is 0.333 Pa (2.5 mTorr), and the applied electric power is 3 watt/cm ² . Under these conditions, a film with a thickness of about 3000 angstroms was formed on the glass substrate. The time required to form a film with a thickness of about 3000 angstroms is about 100 seconds. After forming a film of 3000 angstroms, the glass substrate was replaced, and the film was formed again. By repeating the operation of forming a film and using one sputtering target material, the film forming process can be continuously performed for a long period of time. The presence of hillocks, which represent thermal resistance properties, were observed on the film formed for the first time, the film formed when the sputtering was performed for a total of about 20 hours, and the film formed when a total of about 40 hours passed. Herein, hillocks refer to protrusions generated on the surface of the film after heat-treating the glass substrate with the film at 300° C. under vacuum for a certain period of time. The results confirmed that hillocks rarely appeared on the films and were independent of the total sputtering time. The electrical resistance of each film was also measured. The results confirmed that the resistivity was about 5 μΩcm under optimal conditions. These results indicate excellent circuit properties for liquid crystal displays and semiconductor integrated circuits. Therefore, it was found that if the composite material obtained in Example 1 is used as a raw material of a sputtering target material, a film excellent in characteristics can be stably produced.

Comparative example 1

In Comparative Example 1, a composite casting method was used. 2 kg of aluminum (purity: 99.999%) was heated to about 700° C. in a carbon crucible. After the aluminum is melted, it is cooled to about 640°C, so that the aluminum is in a semi-molten state (solid-liquid coexistence state). In this state, 15 g of carbon powder having an average particle size of 150 µm was added to the aluminum melt, and vigorously stirred with a stirrer. Afterwards, casting takes place in water-cooled copper molds. The obtained aluminum ingot is in the shape of a plate, 200 mm long x 200 mm wide x 20 mm thick. The carbon concentration in the portion of the aluminum ingot corresponding to the bottom surface of the copper mold was measured. As a result, the carbon concentration was 0.003-0.008% by weight, and the carbon was hardly dispersed. Visual inspection of the aluminum ingot revealed that carbon segregation was in the upper part of the aluminum ingot. It can be assumed that the reason for this is that there is little wetting between aluminum and carbon in the composite casting method, so carbon is separated from aluminum, and carbon floats on top due to the difference in specific gravity between aluminum and carbon.

Second embodiment: In the production method of the second embodiment, the raw material for evaporation is evaporated in a mixed atmosphere of hydrocarbon gas, oxygen and nitrogen gas and an inert gas such as argon, and the evaporated particles are deposited On the substrate, lumpy objects are formed. 6 and 7 are schematic diagrams of the manufacturing method of the second embodiment of the present invention. Figure 6 shows the case of using the sputtering method, and Figure 7 shows the case of using the deposition method.

As shown in FIG. 6, in the case of using the sputtering method, a static substrate plate 2 is installed in a chamber 1, and a target 11 for evaporation formed of a substrate metal and a dispersion material nonmetal is placed on a substrate 3. The target Against a static substrate2. The static substrate 2 and the target 11 for evaporation are connected to a power source 12 . The static substrate 2 is made of the metal used for the substrate. Although a DC2-pole gold sputtering system is shown in FIG. 6, a high frequency sputtering system and a magnetron sputtering system can be used.

Chamber 1 has an inlet 13 and an outlet 14 for atmospheric gas. From an atmospheric gas inlet 13, an atmospheric gas prepared by passing a mixture of a hydrocarbon gas such as acetylene and an inert gas such as argon enters the chamber 1.

The atmospheric pressure in the chamber 1 is controlled to a predetermined value, and a predetermined voltage is applied to cause a sputtering phenomenon, so that the metal used for the base material and the non-metal used for the dispersion material are evaporated from the target 11 for evaporation. At this time, the hydrocarbon gas such as acetylene introduced into the chamber 1 is decomposed into carbon and hydrogen. For example, carbon enters the mass 6 formed on the static substrate together with the evaporated metal for the substrate and the non-metal for the dispersed material. It is also possible that the carbon reacts with the evaporated metal for the substrate and the non-metal for the dispersed material to produce stable carbides that enter the block 6 formed on the static substrate 2 in the form of carbides. At this time, the amount of hydrocarbon gas in the atmosphere gas passed into the chamber 1 is controlled, or the voltage applied during sputtering is controlled, so that the carbon concentration in the composite material in the form of the bulk object 6 can be appropriately determined.

Next, the case of using the deposition method shown in FIG. 7 will be described. In FIG. 7 , in the installation chamber 1 of the static substrate plate 2 , the deposition source 15 is formed by the metal used for the substrate, and the non-metal used for the dispersed material is placed in the dispersing crucible 7 , all facing the static substrate 2 . The deposition source 15 is connected to a power source (not shown). Like the first embodiment, this deposition source 15 is effective for mass-producing composite materials if the rod-shaped source is supplied continuously. The static substrate 2 may also be formed from the metal used for the substrate.

Chamber 1 has an inlet 13 and an outlet 14 for atmospheric gas. From an atmospheric gas inlet 13, an atmospheric gas prepared by mixing a hydrocarbon gas such as acetylene and an inert gas such as argon is introduced toward the chamber 1 . Subsequently, the pressure of the atmosphere in the chamber 1 is controlled to a predetermined value, and the deposition source 15 is heated by electric current. The metal used for the substrate and the non-metal used for the dispersion material are deposited on the static substrate 2 in the form of particles after being evaporated and passed through an accelerating probe electrode 16 . At this time, as in the situation shown in Figure 6, the hydrocarbon gas such as acetylene introduced into the chamber 1 is decomposed into carbon and hydrogen, and the carbon generated by the decomposition is together with the evaporated metal used for the substrate and the evaporated nonmetal used for the dispersed material. into the mass 6 formed on the static substrate. It is also possible that the carbon reacts with the evaporated metal for the substrate and the non-metal for the dispersed material to produce stable carbides which enter the block 6 formed on the static substrate 2 in the form of carbides. At this time, controlling the amount of hydrocarbon gas in the atmosphere gas passed into the chamber 1, or controlling the heating temperature during deposition can properly determine the carbon concentration in the composite material in the form of the bulk object 6 .

After adopting the manufacturing method described in conjunction with FIG. 6 and FIG. 7 to form a predetermined block object 6, as in the case of the first embodiment, the block object 6 can be used as an ordinary object, and it can also be used for The metals of the base materials are melted, mixed and cast together to control the concentration of the dispersed materials to form a composite material. If desired, the composite can also be rolled or heat treated to control the crystal structure.

Examples related to the second embodiment are described below.

Example 2

Example 1 represents the situation in which an aluminum-carbon composite material is manufactured by using the sputtering method shown in FIG. 6 . Using a reactive magnetron sputtering device, a disk-shaped aluminum (purity: 99.999%) having a diameter of 203.2 mm and a thickness of 10 mm was used as a target for sputtering. Aluminum foil (purity: 99.999%) having a thickness of 10 μm was used as a static substrate.

A mixed gas of argon gas (purity: 99.999%) and acetylene gas (purity: 99.5%) is provided in the chamber, the flow rate of argon gas is 40ccm, the flow rate of acetylene gas is 20ccm, and the sputtering pressure is controlled at 0.4Pa. The electric power applied to the aluminum target is 8kw (24.7W/cm ² ), and the substrate temperature is set at 200°C.

Sputtering was carried out for 60 minutes, thus forming 80 µm thick lumps with a total weight of 6.14 g on the static substrate. The gas was analyzed for the concentration of carbon in the formed lump, and the carbon content in the lump was 2.4% by weight.

Under vacuum, the block was melted together with separately prepared aluminum (measurement: 99.999%), the composition of aluminum carbon was controlled so that the carbon concentration was 0.7% by weight, and casting was performed using a water-cooled copper mold. The cast-formed composite was observed under a microscope. The results confirmed that carbon was dispersed in the aluminum substrate with a particle size of about 1 mm in the form of Al—C (Al ₄ C ₃ ) phase in Example 1 as shown in FIG. 5 .

The aluminum-carbon (0.7% by weight) composite material formed by the above-mentioned casting was used as a target material for sputtering, and an aluminum film was formed using this target material under the same conditions as in Example 1. The film properties of the aluminum film were investigated, and the results showed that, as in Example 1, if the aluminum-carbon composite material obtained in Example 2 was used as the raw material of the target material, a film with excellent properties could be stably prepared.

Industrial applications

As mentioned above, according to the method for manufacturing composite materials of the present invention, compared with conventional methods for manufacturing composite materials, the dispersion material can be uniformly dispersed in the base material of the composite material, so different composite materials can be manufactured, and the applicability of the method Generally independent of the composition of the composite material. The composite material obtained by the manufacturing method of the present invention can meet the requirements for structural materials and electrode materials, and can be applied to various purposes because the dispersed material can be uniformly dispersed in the substrate and has no internal defects such as holes. In particular, when such a composite material is used as a target material in the manufacture of wiring for liquid crystal displays or semiconductor integrated circuits, desired film characteristics can be stably achieved.

Claims (8)

1. method of making aluminum series composite material, this aluminum series composite material be with aluminium as base material, carbon is dispersed in the base material as dispersing material, method is characterised in that:

The base material raw material and the dispersing material raw material that comprises above-mentioned dispersing material that will comprise aluminium or aluminum compound, while or alternatively vaporised, the particle deposition of evaporation forms block object on a ground.

2. method of making aluminum series composite material, this aluminum series composite material be with aluminium as base material, carbon is dispersed in the base material as dispersing material, method is characterised in that:

To comprise the raw material that is used to evaporate of aluminium or aluminum compound, and evaporate in hydrocarbon gas atmosphere, the particle deposition of evaporation forms block object on a ground.

3. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that described block object is melted, mixes cast form then with the aluminium that constitutes base material again, controls the concentration as the carbon of dispersing material like this.

4. the method for manufacturing aluminum series composite material as claimed in claim 3 is characterized in that described aluminum series composite material also is rolled or thermal treatment, controls crystalline structure.

5. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that described raw material evaporates by sputtering method.

6. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that the particle of described evaporation deposits on the rotation ground.

7. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that described ground has and base material identical materials aluminium.

8. an aluminum series composite material that is used for sputtering target adopts the method manufacturing of manufacturing aluminum series composite material as claimed in claim 3.

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