JP3358934B2 - Method of manufacturing Al-based alloy ingot containing refractory metal by spray forming method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention
The present invention relates to a method for producing an l-base alloy ingot by a spray forming method. In particular, high melting point metal-containing Al used as a sputtering target material for forming a reflection film for optical media, a wiring film for a liquid crystal display, a light shielding film, and the like.
The present invention relates to a method for producing a base alloy ingot by a spray forming method.

[0002]

2. Description of the Related Art Ta, Ti, Zr, V, Nb, Cr,
An Al-based alloy containing a high melting point metal such as W or Mo is used as a sputtering target material for forming a film such as a reflective film for optical media, a wiring film for liquid crystal displays, or a light-shielding film. A film made of an Al-based alloy containing a high melting point metal is formed on a substrate such as an optical medium or a liquid crystal display by a sputtering method. Previously, these films used pure Al films. However, due to the demand for higher reliability, longer life, and higher performance of these films, Ta, Ti, Zr, V, N
A film made of an Al-based alloy containing a high melting point metal such as b, Cr, W, and Mo has been developed and used.

The characteristics required of a sputtering target material for forming a film such as a reflection film for an optical medium, a wiring film for a liquid crystal display, and a light shielding film, particularly a sputtering target material of an Al-based alloy containing a high melting point metal are as follows. . A
The segregation of the high melting point metal in the l-base alloy is low, the oxygen concentration is low, and the density is high. In order to satisfy these requirements, a powder sintering method or a melting casting method has conventionally been used for producing an Al-based alloy containing a high melting point metal.

[0004] There are two powder sintering methods, a premix method and a pre-alloy method. In the premix method, an Al powder and a high melting point metal powder are separately prepared, mechanically mixed by a powder mixer such as a V-type mixer, the mixed powder is filled into a capsule, and solidified by a hot isostatic press. This is a method of molding (sintering). The pre-alloy method is a method in which an Al-based alloy containing a high melting point metal is melted, an alloy powder is produced by a gas atomizing method, the alloy powder of the pre-alloy is filled in a capsule, and solidified (sintered) by hot isostatic pressing. It is.

[0005] The melting casting method is a method in which an Al-based alloy containing a high melting point metal is melted and cast into a mold to produce an ingot of an Al-based alloy containing a high melting point metal.

[0006]

In recent years, in order to improve the productivity of sputtering and the productivity of sputtering materials, there is a high demand for a large-sized material for a sputtering target, and a large-sized, high-melting-point metal having a uniform composition distribution. Al
There is a need for a base alloy ingot. In addition, the level of demand for high-performance and highly reliable reflective films for optical media, wiring films for liquid crystal displays, light-shielding films, etc. has been further increased, and as a sputtering target material, the oxygen concentration is low and a more uniform composition distribution is achieved. A high melting point metal-containing Al-based alloy ingot is required. However, there have been cases where the powder sintering method and the melt casting method are not satisfactory. These problems will be described below.

[0007] The powder sintering method has less segregation of the high melting point metal in the ingot of the Al-based alloy containing the high melting point metal, but has the following problems. This means that the oxygen concentration increases and the packing density of the sintered body may decrease. The high oxygen concentration is due to the use of powder as a raw material. The surface of the powder is covered with oxide and has a large specific surface area. For this reason, the oxygen concentration of the sintered body increases. In addition, the active metal A
In order to use l, the surface of the powder is oxidized in consideration of safety. When the oxygen concentration of the sputtering target material is high, it becomes difficult to adjust the atmospheric pressure during film formation, and there is a problem that the film itself contains a large amount of oxygen and the reflectance is reduced.

[0008] Further, during solidification molding (sintering) by hot isostatic pressing to increase the filling density, defects may occur in the capsule filled with the powder. As a result, a required packing density may not be obtained and a problem that the material cannot be used as a sputtering target material may occur. Further, there is a problem that many steps are required until the final product is manufactured, and the manufacturing cost is high.

On the other hand, the melting casting method has a low oxygen concentration,
A high density ingot is obtained. However, the ingot has a problem that segregation of the high melting point metal component occurs. In the case of the melt casting method, a high melting point metal or an intermetallic compound of Al and a high melting point metal is crystallized during casting and solidification. Then, during the cooling and solidification process, the crystallized substances settle, causing weight segregation to be deposited at the bottom of the ingot, and there is a problem that it is difficult to obtain a compositionally uniform ingot.

Regarding this problem, an improvement method has been proposed (see Japanese Patent Application No. 50649/1993). This method
The temperature of the molten metal in the mold until the casting is completed is maintained at a temperature at which an intermetallic compound of Al and the high melting point metal is not generated. Thereafter, the molten metal in the mold is rapidly cooled and solidified to prevent weight segregation. According to this method, an ingot having a low oxygen concentration and a uniform composition of an Al-based alloy containing a high melting point metal can be obtained.

[0011] However, this improvement method has been insufficient in some cases. Especially for large ingots,
The problem is that a sputtering target material having a uniform high melting point metal composition cannot be obtained. For example, in the melt casting method, the size of the crystallized high melting point metal or intermetallic compound increases. For this reason, there is also a problem that it is difficult to process an ingot of an Al-based alloy containing a high melting point metal.

Accordingly, the invention according to claims 1 to 3 of the present invention provides a high melting point metal-containing alloy having a low oxygen concentration and a more uniform composition distribution than a conventional high melting point metal-containing alloy ingot. It is an object of the present invention to provide a method for producing an ingot by a spray forming method. In particular, it is intended to provide a method for manufacturing a high melting point metal-containing Al-based alloy ingot having a uniform composition distribution by a spray forming method in a large refractory metal-containing Al-based alloy ingot which is difficult to cope with by the melt casting method. It is the purpose.

[0013] The invention according to claim 4 has the object of the invention according to claims 1 to 3 , in addition to preventing the occurrence of defects in the ingot of an Al-based alloy containing a high melting point metal, and further recrystallizing a high melting point metal, or It is an object of the present invention to provide a gas atomizing method in the second step, which makes it possible to reduce the size of an intermetallic compound of Al and a high melting point metal. By reducing the size of the refractory metal or intermetallic compound, the workability of the refractory metal-containing Al-based alloy ingot is improved.

According to a fifth aspect of the present invention, there is provided, in addition to the objects of the first to fourth aspects, a method of manufacturing an Al-based alloy ingot having a low melting point and containing a high melting point metal by a spray forming method. It is the purpose.

The invention according to claim 6 is used for a sputtering target material for forming a reflection film for an optical medium, a wiring film for a liquid crystal display, a light-shielding film, and the like, in addition to the objects of the invention described in claims 1 to 5. It is an object of the present invention to provide a method for manufacturing an ingot by spray forming of an Al-based alloy containing a high melting point metal.

[0016]

Means for Solving the Problems In order to achieve the above-mentioned object, the inventors of the present invention have intensively studied a method for producing an Al-based alloy ingot containing a high melting point metal. The spray forming method was first applied to the production of an Al-based alloy ingot containing a high melting point metal, and various experiments were performed. As a result, a large ingot can be manufactured by manufacturing an Al-based alloy ingot containing a high melting point metal by using a spray forming method, and the ingot has a uniform composition distribution and an advantage of the powder sintering method. The present invention has been completed based on the finding that both the low oxygen concentration and the high density, which are advantages of the melting casting method, are obtained.

According to the present invention, there is provided a method for producing an ingot of a refractory metal-containing Al-based alloy by a spray forming method, wherein the refractory metal-containing Al-based alloy is melted at a temperature not lower than the liquidus temperature of the refractory metal-containing Al-based alloy. A first step, wherein the molten metal of the high melting point metal-containing Al-based alloy is heated to a temperature range of + 50 ° C. to + 200 ° C.
And wherein a second step of atomized by gas atomization in circumference, the atomized the refractory metal-containing Al-based alloy, to include a third step of by sequentially depositing solidified while deposited in molten or semi-solid state Is what you do.

In the first step, the raw material for melting the Al-based alloy containing a high melting point metal is melted at a temperature not lower than the liquidus temperature of the Al-based alloy containing a high melting point metal. Thus, the molten raw material is completely dissolved to obtain a uniform molten metal. The melting temperature is the liquidus temperature of the Al-based alloy containing the high melting point metal + 2
It is preferable that the temperature is not higher than 00 ° C. Liquidus temperature + 200 ℃
Exceeds, the formation of Al oxide in the molten metal becomes remarkable,
The amount of oxide in the Al-based alloy ingot containing a high melting point metal increases.

In the second step, the molten metal of the high melting point metal-containing Al-based alloy is heated to the liquidus temperature +
Gas atomization in the temperature range of 50 ° C to liquidus + 200 ° C , high melting point metal or metal compound (Al and high melting point metal)
Is a step of atomizing without crystallizing.

Since gas atomization is performed at a temperature at which the high melting point metal or intermetallic compound (Al and high melting point metal) is not crystallized, clogging of the atomizing nozzle by the crystallized substance (high melting point metal or intermetallic compound) can be prevented. Further, generation of a huge crystallized substance in the ingot of a high melting point metal-containing Al-based alloy can be suppressed.

By setting the temperature of the gas atomization to be equal to or higher than the liquidus temperature of the high melting point metal-containing Al-based alloy + 50 ° C., the clogging of the atomizing nozzle can be prevented more effectively, and the high melting point metal-containing Al-based alloy can be cast. It is preferable to suppress the generation of a huge crystallized substance (high melting point metal or intermetallic compound) in the lump. Further, it is preferable to suppress the formation of Al oxide in the molten metal in the tundish by setting the temperature of the gas atomization equal to or lower than the liquidus temperature of the Al-based alloy containing the high melting point metal + 200 ° C.

In the first step or the second step, it is preferable to use an alumina refractory or a spinel refractory for one or both of the melting crucible and the tundish.
It is preferable to select a material having low porosity, low thermal expansion coefficient, and excellent erosion resistance and spalling resistance in consideration of the reactivity with the Al-based alloy containing a high melting point metal.

Further, it is preferable to dispose a ceramic filter on one or both of the melting crucible and the tundish in order to remove oxides generated during melting. It is preferable to use an alumina filter that does not cause erosion or cracking even at a high temperature (dissolution temperature to 1600 ° C.).

In the second step, the gas / metal ratio (Nm ³ / kg) at the time of gas atomization is preferably in the range of 1 to 5. Here, the gas / metal ratio is the gas outflow (Nm ³ / min) / molten metal outflow (kg)
/ Min). If the gas / metal ratio is less than 1,
The size of the crystallized substance (high melting point metal or intermetallic compound) in the ingot of the high melting point metal-containing Al-based alloy becomes 20 μm or more. The size of the crystallized material in the ingot of the high melting point metal-containing Al-based alloy is 20 μm
Above this, the workability is significantly reduced. Further, characteristics required for the sputtering target material are also deteriorated. On the other hand, if the gas / metal ratio exceeds 5, the cooling capacity of the gas becomes high, and the melt of the finely divided Al-based alloy containing a high melting point metal is solidified. As a result, many holes are generated in the ingot of the high melting point metal-containing Al-based alloy produced in the third step, and defects occur. As a result, the density and the deposition yield of the Al-based alloy ingot are significantly reduced.

The third step is a step of sequentially depositing and solidifying the finely divided high-melting-point metal-containing Al-based alloy while adhering it in a molten or semi-solid state. This step has the following effects. Since the molten Al-based alloy containing the high melting point metal is atomized, component segregation of the ingot of the Al-based alloy containing the high melting point metal is small. Since it is rapidly solidified, crystallized substances such as high melting point metal or intermetallic compound are uniformly and finely distributed in the ingot of the Al-based alloy containing high melting point metal. Further, the solid solution of the high melting point metal in Al can be increased, and a precipitation effect due to the solid solution of the high melting point metal in Al can be expected. Since they are sequentially deposited and solidified while being attached in a molten or semi-solid state, contamination with unnecessary elements (oxygen, nitrogen, etc.) is small. In particular, the amount of oxygen can be reduced. In addition, since the ingot is deposited in a semi-molten state, the density of the Al-based alloy ingot containing a high melting point metal increases. Further, in order to increase the density of the Al-based alloy ingot containing a high melting point metal, it is preferable to increase the density by hot isostatic pressing.

By using the method of the present invention for producing an Al-based alloy ingot containing a high melting point metal by spray forming, an ingot of an Al-based alloy containing a high melting point metal having a low oxygen concentration and a more uniform composition distribution is produced. it can. Even in the case of a large refractory metal-containing Al-based alloy ingot that is difficult to cope with by the melt casting method, a refractory metal-containing Al-based alloy ingot having a uniform composition distribution can be manufactured.

It is preferable to use an inert gas such as Ar or N ₂ gas as a dissolving atmosphere gas, a gas atomizing gas or a deposition atmosphere gas. By dissolving in an inert gas atmosphere, oxidation of the high melting point metal-containing Al-based alloy can be prevented.
Further, by performing gas atomization in an inert gas atmosphere, solid solution of oxygen in the ingot of the Al-based alloy containing a high melting point metal can be reduced. Furthermore, surface oxidation of the high melting point metal-containing Al-based alloy ingot can be suppressed, and the intrusion of foreign matter can be prevented.

The refractory metals contained in the refractory metal-containing Al-based alloy are Ta, Ti, Zr, V, Nb, Cr, W, M
It is preferable that at least one of o is used. Al-based alloys containing these high-melting metals are used as reflective films for optical media,
When used as a sputtering target material for forming a wiring film for a liquid crystal display, a light-shielding film, and the like, the characteristics of these films are improved. By using the spray forming method of the present invention to produce such a high melting point metal-containing Al-based alloy ingot, to obtain a high melting point metal-containing Al-based alloy ingot having a low oxygen concentration and a uniform composition distribution. Can be done.

The amount of the high melting point metal contained in the high melting point metal-containing Al-based alloy is preferably 0.1 to 10.0 at%. The amount of refractory metal added to the Al-based alloy is 0.
If it is less than 1 at%, it does not contribute to improving the performance of the Al-based film used for optical media, liquid crystal displays and the like. It was found that as the amount of the refractory metal added to the Al-based alloy increased, the size of the refractory metal or intermetallic compound crystallized in the refractory metal-containing Al-based alloy ingot increased. If the amount of the refractory metal added to the Al-based alloy exceeds 10.0 at%, a huge crystallized substance is formed in the Al-based alloy ingot. Preferably, the amount of the refractory metal added to the Al-based alloy is 5.0a.
t% or less.

It is preferred that the method for producing an Al-based alloy ingot containing a high melting point metal by the spray forming method of the present invention be used for producing a sputtering target material for forming a film. The characteristics required for the sputtering target material (low oxygen concentration, low component segregation, and high density) can be satisfied. Also, the sputtering target material is desired to have a low specific resistance. In order to reduce the specific resistance, the amount of the high melting point metal added to the Al-based alloy is preferably 10.0 at% or less, more preferably 5 at% or less. .0at
% Or less.

The method of the present invention for producing an Al-based alloy ingot containing a high melting point metal by the spray forming method is used only for producing a sputtering target material for forming a reflection film for an optical medium, a wiring film for a liquid crystal display, a light-shielding film and the like. It is not used, but is also used for manufacturing materials for applications such as heat-resistant sliding members.

[0032]

DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described with reference to FIG. FIG. 1 is an explanatory diagram showing an example of an apparatus used in the present invention. In the present invention, the melting raw material of the Al-based alloy containing a high melting point metal is placed in a melting furnace (not shown) in an inert gas atmosphere.
Melts above the liquidus temperature of the Al-based alloy containing the high melting point metal. The melt of the molten Al-based alloy containing the high melting point metal was cast into the tundish 1. The temperature of the molten metal 2 in the tundish 1 was maintained in a temperature range from the liquidus temperature of the high melting point metal-containing Al-based alloy + 50 ° C to the liquidus temperature + 200 ° C.

As a melting crucible (not shown) and the tundish 1, an alumina refractory or a spinel refractory was used.
An alumina filter was provided in the melting crucible and the tundish 1 to remove oxides generated during melting. Further, the molten metal 2 of the Al-based alloy containing a high melting point metal was protected by an inert gas.

The molten metal 2 was allowed to flow naturally through the tundish nozzle 3 into the chamber 4 in an inert gas atmosphere. A gas atomizer 5 is provided below the tundish 1.
The high-pressure inert gas jet stream 6 ejected from the gas atomizer 5 is sprayed on a molten metal stream 7 of an Al-based alloy containing a high melting point metal, and the molten metal stream 7 is atomized. At this time, the ratio of the flow rate of the inert gas jet (Nm ³ / min) to the flow rate of the molten metal of the Al-based alloy containing the high melting point metal (kg / min), that is, the ratio of the gas / metal ratio (Nm ³ / kg) is 1
-5.

The finely divided Al-based alloy particles containing a high melting point metal were sequentially deposited and solidified while being adhered in a molten or semi-solid state on a substrate 9 set on a collector 8 below. The collector 8 was moved up and down and rotated as necessary by a driving means such as a stepping motor 10. The collector 8 is gradually lowered according to the deposition amount of the high melting point metal-containing Al-based alloy particles, and the distance between the tundish nozzle 3 and the top surface of the deposition is kept constant,
A high melting point metal-containing Al-based alloy ingot 11 was manufactured. The obtained refractory metal-containing Al-based alloy ingot 11 is optionally
Densification treatment was performed by a hot isostatic press (not shown). Furthermore, the Al-based alloy ingot containing a high melting point metal was processed into a sputtering target material through forging or rolling.

[0036]

【Example】

(Example 1) Al-1at% Ta high melting point metal-containing Al
A base alloy ingot was manufactured by the spray forming method, the melting casting method, and the powder sintering method (premix method) of the present invention. As a typical example of the powder sintering method, a premix method which is easy to manufacture and low in cost is described as a comparative example. Example 1
Was manufactured by the method described in the embodiment of the present invention and the prior art. The liquidus temperature of the Al-based alloy of Al-1 at% Ta is 1130 ° C. The manufacturing conditions for these ingots are shown below. 1) Spray forming method, the melting temperature of the present invention: liquidus temperature + 120 ° C., atomizing temperature liquidus temperature + 120 ° C., atomized by weight (ingot weight): 30kg · Gas / metal ratio: 3 Nm ³ / kg · Atomizing gas and atmosphere gas: N ₂ gas-Melting crucible and tundish: Alumina refractory-Ceramic filter: Use alumina filter 2) Melting casting method-Melting temperature: Liquidus temperature + 100 ° C-Pouring temperature: Liquid phase Linear temperature + 100 ° C ・ Pouring weight: 20kg ・ Melting crucible: Refractory made of alumina 3) Powder sintering method (premix method) ・ Mixing condition: Mixing Al powder and Ta powder with V-type mixer ・ Solidification molding amount: 30kg Solidification molding conditions: Solidification molding by hot isostatic pressing (500 ° C-1000 atm)

With respect to these ingots, analytical samples were taken at the positions shown in FIG. 2, and the Ta concentration and the distribution of gas components (O, N) were examined. Table 1 shows the results.

[0038]

[Table 1]

The method of the present invention has a Ta analysis value of 0.96 to 0.96.
In the range of 0.98 at%, segregation was small, and an ingot having a uniform composition could be obtained. On the other hand, Ta of the melting casting method
The analysis value was in the range of 0.85 to 1.08 at%, and the dispersion was large. In the melting casting method, the ingot becomes as large as 20 kg, the cooling rate of the ingot becomes slow, and the size of the high melting point crystallized substance (Ta or intermetallic compound of Al and Ta) exceeds 40 μm. It is considered that the cause is.

The Ta analysis value of the powder sintering method is 0.82-0.
The range is 92 at%. The variation in the Ta analysis value of the powder sintering method was smaller than that of the melt casting method, but larger than that of the present invention. It is considered that the variation in the Ta analysis value of the powder sintering method became large because a sintered body was manufactured by mixing Al powder and Ta powder having a large difference in specific gravity.

Regarding the gas components, the method of the present invention has an oxygen amount of 0.011 to 0.22 at% and a nitrogen amount of 0.01 to 0.2 at%.
A low value was shown at 1 to 0.014 at%. In particular, the oxygen content of the method of the present invention is the oxygen content of the powder sintering method (0.29 to 0.29).
0.43 at%). The high value of the oxygen content in the powder sintering method is due to the high oxygen content of the raw material powder. This is the same in the premix method, and the oxygen content of the sintered body in the premix method is about 0.3 wt%. Although the amount of oxygen in the method of the present invention is higher than the amount of oxygen in the melt casting method, the amount of oxygen is sufficiently low for use as a sputtering target material. Further, the nitrogen content is low because the cooling rate of the atomized molten metal at the time of gas atomization is high, so that the solid solution of nitrogen in the molten metal becomes extremely small. Therefore, the amount of nitrogen of the present invention was not much different from the amount of nitrogen of the casting method.

In addition, the Al-1 produced in the embodiment of the present invention
The deposition density of an Al-based alloy ingot of at% Ta is 95% (Al
The true density of an Al-based alloy of -1 at% Ta was defined as 100%), and a high density was obtained. By rolling this Al-based alloy ingot and processing it into a sputtering target material, the ingot became a true density. This sputtering target material was used for forming a reflective film for optical media.

Example 2 An ingot of an Al-based alloy containing a high melting point metal of Al-4 at% Ta was produced by the spray forming method, the melting casting method and the powder sintering method (premix method) of the present invention. An Al-based alloy ingot of Al-4 at% Ta was produced under the same conditions as in Example 1, and the Ta concentration and the distribution of gas components (O, N) were investigated. In addition, Al-4
The liquidus temperature of the Al-based alloy of at% Ta is 1400 ° C. Table 2 shows the results.

[0044]

[Table 2]

The method of the present invention has a Ta analysis value of 3.93 or more.
It is in the range of 3.99 at%. On the other hand, Ta of the melting casting method
The analysis value was in the range of 3.49 to 3.90 at%, and the variation was large. Further, the variation became large when the Ta analysis value of the powder sintering method was in the range of 3.48 to 4.12 at%. High melting point metal-containing A produced by the method of the present invention
It was confirmed that the l-base alloy ingot had less segregation and had a uniform composition. Further, the Al-based alloy ingot produced by the method of the present invention had a low oxygen concentration, and the deposition density of the ingot was as high as 95%, and the same results as in Example 1 were obtained. This Al-based alloy ingot was also rolled, processed into a true density sputtering target material, and used for forming a reflective film for optical media.

(Example 3) Next, the gas / metal ratio (Nm ³ / kg) was set to 0.5 to 0.5 by spray forming.
7 to produce an Al-based alloy ingot containing a high melting point metal of Al-1.0 at% Ta. The manufacturing conditions are gas /
Except for the metal ratio, it is the same as the spray forming method of Example 2. The size, the deposition density, and the deposition yield of the crystallization product (Ta, intermetallic compound) in the ingot of an Al-based alloy containing a high melting point metal were investigated. Table 3 shows the results.

[0047]

[Table 3]

When the gas / metal ratio is in the range of 1 to 5, the size of the crystallized material is 20 μm or less. In addition, the deposition density is 90%
As described above, a deposition yield of 70% or more could be secured. If the deposition density of the ingot is 90% or more, there is no problem in the performance of the sputtering target material. Usually, ingots are subjected to plastic working such as rolling and forging. As a result, when the deposition density of the ingot is 90% or more, the deposition density of the ingot can be increased to the true density or close to the true density by plastic working. Further, by ensuring the deposition yield of 70% or more, the manufacturing cost can be reduced.

When the gas / metal ratio is 0.5, the size of the crystallized material is 38 μm. In addition, the deposition density and the deposition yield are reduced. When the gas / metal ratio is 0.5,
The gas flow rate of the gas atomization decreases, the atomization of the molten metal of the Al-based alloy containing the high melting point metal becomes insufficient, and the size of the crystallized material increases. Along with this, a large number of vacancies were generated inside the Al-based alloy ingot, and the deposition density and the deposition yield were reduced.

On the other hand, when the gas / metal ratio exceeds 5, the deposition density and the deposition yield of the Al-based alloy ingot containing a high melting point metal are significantly reduced. This is because when the gas / metal ratio exceeds 5, the gas flow rate of gas atomization with respect to the molten metal outflow amount increases. As a result, the cooling capacity of the gas is increased, and the atomized molten metal is solidified. Along with this,
The deposition density and the deposition yield of the Al-based alloy ingot are reduced.

[0051]

As described above, by using the method of the present invention, it is possible to produce a large ingot of an Al-based alloy containing a high melting point metal, and the ingot can be made uniform by the powder sintering method. It has both a high composition distribution and low oxygen concentration and high density, which are advantages of the melting casting method. In particular, it can have excellent characteristics (low segregation of high melting point metal in Al-based alloy, low oxygen concentration and high density) as a sputtering material.

According to the first to third aspects of the present invention, it is possible to produce an Al-based alloy ingot containing a high melting point metal having a more uniform composition distribution than conventional powder sintering and melting casting methods. Is what you do. In particular, the present invention makes it possible to produce a high-melting-point metal-containing Al-based alloy ingot having a uniform composition distribution in a large-sized high-melting-point metal-containing Al-based alloy ingot that is difficult to cope with by the melt casting method. This makes it possible to improve the productivity of sputtering and the productivity of sputtering material.

The invention described in claim 4 has, in addition to the effects of the inventions described in claims 1 to 3, a defect in the ingot of an Al-based alloy containing a high melting point metal is prevented, and a crystallized substance (high melting point metal, (Intermetallic compound). By setting the size of the crystallized material to 20 μm or less, it is possible to remarkably improve the workability of the Al-based alloy ingot containing a high melting point metal.

The fifth aspect of the present invention provides, in addition to the effects of the first to fourth aspects, a reduction in the amount of oxygen dissolved in an ingot of an Al-based alloy containing a high melting point metal and further prevention of foreign matter from entering. It is possible to do.

The invention according to claim 6 is used for manufacturing a sputtering target material for forming a reflection film for an optical medium, a wiring film for a liquid crystal display, a light shielding film, and the like.
It enables the production of a sputtering target material capable of producing a highly reliable, long life, high performance film. that's all

[Brief description of the drawings]

FIG. 1 is an explanatory diagram showing an example of an apparatus used in the present invention.

FIG. 2 is a view showing a sampling position of an analysis sample of Examples 1 and 2, wherein a is a rolled sheet material (10 × 1) of an example of the present invention;
50 × 800 mm) sampling position, b is a comparative material (casting method,
Rolled sheet material (powder metallurgy) (10 x 150 x 800 mm)
It is explanatory drawing which shows the sampling position.

[Explanation of symbols]

 REFERENCE SIGNS LIST 1 tundish 2 molten metal of Al-based alloy containing high melting point metal 3 tundish nozzle 4 chamber 5 gas atomizer 6 jet stream 7 molten stream of Al-based alloy containing high melting point metal 8 collector 9 substrate 10 stepping motor 11 Al-based alloy containing high melting point metal Ingot

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI C23C 14/34 C23C 14/34 A // B22F 9/08 B22F 9/08 S (72) Inventor Seiya Furuta Kobe, Hyogo Prefecture 1-5-5 Takatsukadai, Nishi-ku Kobe Steel, Ltd. Kobe Research Institute In the area (56) References JP-A-64-57965 (JP, A) JP-A-6-330263 (JP, A) JP-A Heisei 3-82722 (JP, A) (58) Field surveyed (Int. Cl. ⁷ , DB name) B22D 23/00 C23C 6/00

Claims (6)

(57) [Claims] 1. A method for producing an ingot of an Al-based alloy containing a high melting point metal by a spray forming method, comprising:
A first step of melting at a temperature equal to or higher than the liquidus temperature of the base alloy; and melting the molten metal of the high melting point metal-containing Al-based alloy from the liquidus temperature of the high melting point metal-containing Al-based alloy + 50 ° C to the liquidus line +20
2nd atomization by gas atomization in the temperature range of 0 ° C
And a third step of sequentially depositing and solidifying the finely divided Al-based alloy containing high melting point metal while adhering it in a molten or semi-solidified state, and spray forming the Al-based alloy containing high melting point metal. Method for producing ingots. 2. The refractory metal contained in the refractory metal-containing Al-based alloy is Ta, Ti, Zr, V, Nb, Cr,
The method for producing an ingot by spray forming a refractory metal-containing Al-based alloy according to claim 1, wherein the ingot is at least one of W and Mo. 3. The spray forming of a high melting point metal-containing Al-based alloy according to claim 1, wherein the amount of the high melting point metal contained in the high melting point metal-containing Al-based alloy is 0.1 to 10.0 at%. Method for producing ingots. 4. In the second step, gas atomization is performed.
Gas / metal ratio (Nm ³ / kg) in the range of 1 to 5
The high melting point metal-containing material according to any one of claims 1 to 3.
Production of ingot by spray forming method of Al base alloy
Method. Here, gas / metal ratio = (gas atomizing gas
Outflow / melt outflow). 5. The method according to claim 1 , wherein the dissolving atmosphere in the first step, the second step
Atomizing gas and deposition atmosphere of the third step
5. The method according to claim 1, wherein an inert gas is used.
Forming Method of Al-based Alloy Containing High Melting Point Metal
Method for producing ingots. 6. A sputtering target material for forming a film.
The method according to claim 1, which is used for manufacturing
Spray forming method for Al-based alloy containing high melting point metal
Method for producing ingots.