JPH06271955A - Production of aluminum alloy - Google Patents

Abstract

PURPOSE:To provide the method for producing a bulky aluminum allay having high strength, high hardness and high heat resistance and utilizable for automobiles, electric apparatus and the other industries. CONSTITUTION:This method for producing an aluminum alloy is constituted of a stage in which the mixed powder of the material to be worked constituted of aluminum and at least one or more kinds of metals and non-metals selected from the groups 4a, 5a, 6a, 7a and 8a and silicon and baron or a green compact obtd. by subjecting the same mixed powder to compacting or a cast material is produced and a stage in which the material to be worked is inserted into a die for working and is repeatedly subjected to plastic deformation in a state in which at least a part of the material to be worked is cramped while it is held to 100 to 400 deg.C in an inert atmosphere to form a metastable phase essentially consisting of an amorphous phase and/or a supersaturated solid solution phase, and this method furthermore includes a stage in which the same aluminum allay is subjected to heating treatment, and a metastable phase and/or a stable phase essentially consisting of intermetallic compounds is finely dispersed therein.

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 aluminum alloy having high strength, high hardness and high heat resistance, which can be used in the automobile, aircraft, electric equipment and other industries.

[0002]

2. Description of the Related Art High-strength aluminum alloys with high specific strength are expected to achieve high performance in automobiles, aircraft, office equipment, etc., especially in high-speed moving parts. Therefore, they can be strengthened by the quenching method or mechanical alloying method. There is a lot of research done to improve In the quenching method, for example, aluminum-TM (TM: transition metal such as Fe, Co, Ni)-
An alloy made of Ln (Ln: a rare earth element such as Y, La, and Ce) is melted and melt-spun by a method.
0.02mm with tensile strength exceeding 100kgf / mm ²
A ribbon-shaped amorphous material having a thickness is obtained (Journal of the Japan Institute of Metals, Vol. 30, No. 5, 1991, P375).
In addition, a bulk material produced by a method of extruding an amorphous powder produced by rapid solidification of an aluminum-TM alloy at a temperature above the phase transformation start temperature is 100 kgf / mm ² (Japanese Patent Laid-Open No. Hei 10 (1999) -242242). 3-202431).

On the other hand, in the mechanical alloying method, for example, an aluminum phase and a powder having a wide range of compositions such as titanium, nickel, niobium, and zirconium are subjected to a composite treatment such as mechanical mixing, pulverization, and aggregation to form an amorphous phase. Although it is a method, there is no method of measuring the strength of the material formed by this method in bulk form. In addition, the mechanical strength of iron particles is finely dispersed in aluminum and then rolled into a bulk material, which has a tensile strength of 55 kg.
A material having a f / mm ² value or more has been produced.

However, the shape of the product obtained by these methods is usually a powder of several μm to several tens of μm. Although a ribbon-shaped material having a thickness of about 20 μm can be obtained by the quenching method, it contains a large amount of expensive rare earth elements, resulting in a high cost. Further, in any of these shapes, the application is limited. When the amorphous phase powder is used as a part, it is necessary to solidify the powder. That is,
As a method for solidifying the powder, 40% in a non-oxidizing atmosphere is used.
There are methods of canning extrusion at 0 to 550 ° C. and solidification by HIP or the like. In these methods, crystallization of the amorphous alloy by heating occurs, and the obtained alloy is usually crystalline. Further, in the above canning extrusion, if the extrusion temperature is lowered to prevent crystallization, there is a drawback that the bonding between the powders is not sufficient and the strength is poor. As described above, the material having an amorphous phase or the like obtained by the conventional quenching method or mechanical alloying method is in the form of powder or ribbon, and this has to be further processed into a product shape by canning extrusion or the like. However, there is a strong demand for the development of a method for producing an aluminum alloy that can easily obtain a bulk material having a high-strength amorphous phase at low cost.

[0005]

DISCLOSURE OF THE INVENTION The present inventors examined the above problems in detail and focused on the following points. That is,
Titanium or vanadium powder is mixed with pure aluminum powder, and the mixed powder is compacted and subjected to repeated heavy working in a state of being constrained, and the work material is given more strain than conventional plastic working. It has been found that the material to be processed can be made into a bulk by only this processing step, which is composed of a metastable phase mainly composed of an amorphous phase or a supersaturated solid solution phase. Further, it was found that when this material was heated to 300 to 500 ° C., a material having a tensile strength of 70 kgf / mm ² or more in which a metastable phase mainly composed of an intermetallic compound was finely precipitated could be obtained. The present invention is a method for producing an aluminum alloy consisting of a metastable phase such as an amorphous phase or a supersaturated solid solution phase, which is simply in a bulk form only by repeated working, and a tensile strength in which a metastable phase of an intermetallic compound is finely precipitated. Is 70k
It is an object of the present invention to provide a method for producing a bulk high-strength aluminum alloy having a gf / mm ² or more.

[0006]

[Means for Solving the Problems]

(Structure of First Invention) The method for manufacturing a bulk aluminum alloy according to the first invention comprises aluminum and a fourth periodic table.
The mixed powder or the mixed powder which is a work material made of at least one metal or non-metal selected from the group consisting of a, 5a, 6a, 7a, 8a, silicon and boron is pressed. Process of producing powdered molded body or cast material, and inserting each of the materials to be processed into a processing mold, and holding each at 100 to 400 ° C. in an inert atmosphere, each structure constituting the material to be processed A plastic deformation that causes a diffusion reaction between the materials is repeatedly applied in a state in which at least a part of the work material is constrained to form a metastable phase mainly composed of an amorphous phase and / or a supersaturated solid solution phase; It is characterized by

(Structure of Second Invention) The method for manufacturing a bulk high-strength aluminum alloy according to the second invention is made of aluminum and 4a group, 5a group, 6a group, 7a group of the periodic table.
A step of producing a mixed powder, which is a work material made of at least one metal or non-metal selected from the genus, the genus 8a, silicon and boron, or a compact or a cast material obtained by pressing the mixed powder. The material to be processed is inserted into a working die, and while being maintained at 100 to 400 ° C. in an inert atmosphere, the material to be processed is subjected to plastic deformation such that a diffusion reaction occurs between the tissues constituting the material to be processed. A step of forming a metastable phase mainly composed of an amorphous phase and / or a supersaturated solid solution phase by repeatedly applying at least a part of the material in a restrained state, and heat-treating the material to be processed at a temperature of 200 to 500 ° C. And a step of finely dispersing a metastable phase and / or a stable phase mainly containing an intermetallic compound.

[0008]

[Action]

(Operation of the First Invention) The method for producing an aluminum alloy according to the present invention is characterized by carrying out repeated strong working to have an amorphous phase or a supersaturated solid solution phase which is a metastable phase, and the product shape is formed only by this repeated strong working. It is characterized in that a material in a close bulk can be obtained. The formation of the amorphous phase and / or the supersaturated solid solution phase is carried out by the genus 4a, 5a
A work material made of a mixed powder of one or more elements selected from the group consisting of genus, 6a, 7a, 8a, silicon and boron is inserted into a working mold and is placed in an inert atmosphere. 10
While maintaining the temperature at 0 to 400 ° C., strong working is performed so that a diffusion reaction occurs in the work material between powders and the like, and is repeated with at least a part of the work material being restrained. It is presumed that the reason why the amorphous phase and / or the supersaturated solid solution phase can be formed is as follows.

When the material to be processed is a powder or a compact obtained by compacting the powder, the powders are rubbed against each other and crushed by a strong processing that causes a diffusion reaction between the powders, the interface is activated, and diffusion is caused. Occurs. In the next processing, new friction and crushing occur between the powders, an active surface is formed, and diffusion progresses. By repeating such processing, the entire material to be processed becomes a bonded state due to diffusion, and a large amount of elements that cannot be dissolved by ordinary heat treatment or processing can be solid-dissolved, and a metastable phase is formed. It is.

The method for producing an aluminum alloy of the present invention comprises:
An amorphous phase or the like is formed by a diffusion phenomenon similar to the conventional mechanical alloying method, but is different in the following points. In the mechanical alloying method, a ball mill is used to perform milling at room temperature for about 10 to 1000 hours to repeat rubbing between powders, crushing and agglomeration, and a metastable phase is formed by diffusion between particles, but this is obtained. The material state is always powdery. These powders are active, although the surface is small, but due to adsorption or compound formation by atmospheric gases and the passage of time since the active surface was formed,
Surface activity is reduced. Therefore, when solidifying this powdery sample, it is necessary to take out the powder from the ball mill, put it in a container, and perform canning extrusion or HIP treatment at a high temperature of 450 to 600 ° C.

On the other hand, in the present invention, 100 to 400
The step of forming the bulk at a temperature such as ℃ causes a diffusion reaction between the powders by friction and crushing between the metal powders by high energy to form a metastable phase, and at the same time, at a high pressure and an active surface. Due to the effect, the metal powders are strongly bonded together to form a bulk. Further, even if an active new surface is formed by crushing each powder, surface activity is lost and diffusion between metals is less likely to occur if oxidation or nitridation occurs due to the gas in the atmosphere. Therefore, in order to maintain the activity of the newly formed surface, it is desirable to perform it in a high vacuum or in an inert atmosphere such as Ar.

When the material to be processed is a cast material, when a stable phase mainly composed of, for example, a relatively large intermetallic compound dispersed in the aluminum alloy cast material is subjected to heavy working,
The stable phases repeat rubbing and crushing with each other, the interface is activated, and the crushed stable phase and the aluminum mother phase react with each other to form a metastable phase.

Next, it is considered that the formation of the metastable phase is caused by the diffusion phenomenon between the powders under the application of high energy as described above. In order to increase the diffusion rate, it is most advantageous to raise the processing temperature, and it is also desirable to reduce the deformation resistance of the material. However, if the temperature is too high, the phase generated by the diffusion between the powders, etc., tends to be the phase in the equilibrium state, and even if the metastable phase is once formed, the phase is changed by holding it at a high temperature. Enter a stable phase. Therefore, the processing temperature is set to 100 to 400 ° C.

(Operation of the Second Invention) In the method for producing an aluminum alloy according to the second invention, a material in which a metastable phase mainly composed of an amorphous phase and / or a supersaturated solid solution phase is formed by performing repeated heavy working is formed. Then, this material is subjected to a heat treatment to finely disperse the metastable phase and / or the stable phase mainly containing an intermetallic compound, and high strength is obtained by these treatments. The reason why a high-strength aluminum alloy can be produced by performing the heat treatment is presumed to be as follows. When the aluminum alloy in which the metastable phase is formed is heat-treated at 200 to 500 ° C., alloy elements are aggregated from an amorphous phase or a supersaturated solid solution phase in the aluminum alloy base material, and mainly contains an intermetallic compound with aluminum. A structure in which a metastable phase or a stable phase is finely dispersed can be formed, and the strength is improved. Moreover, 200-500 ° C
However, there is no decrease in this strength. Elements such as copper, zinc, and magnesium, which are used as alloying elements in commonly used aluminum alloys, have a fast diffusion rate at 200 ° C or higher, and at 200 ° C or higher, finely dispersed phases aggregate in a short time and become large. In contrast to the stable phase of grains, it is presumed that the elements mixed with aluminum in the present invention described above have a relatively slow diffusion rate in aluminum and are unlikely to be in a stable phase, and strength is maintained even at high temperatures. To be done.

[0015]

【The invention's effect】

(Effect of the first invention) According to the method for manufacturing an aluminum alloy of the first invention, a material having a metastable phase can be obtained by a relatively simple method such as repeated heavy working. Further, since this aluminum alloy is obtained not in the form of powder or ribbon, but in the form of bulk, which is close to the product shape, it has the advantage that the danger of powder and the solidification step are unnecessary.

(Effect of the Second Invention) According to the method for producing an aluminum alloy of the second invention, the aluminum alloy is molded into a product shape in a relatively soft state before the heat treatment, and then the heat treatment is carried out, which is relatively simple. It is possible to produce a high-strength aluminum alloy material in which a metastable phase and / or a stable phase mainly composed of a high-strength intermetallic compound are finely dispersed.

[0017]

【Example】

(Specific Example) Hereinafter, a specific example in which the method for producing an aluminum alloy according to the first invention and the second invention is more specific will be described. In this example, the element to be mixed with the aluminum powder or the like must first be an element that easily forms a metastable phase such as an amorphous phase, a supersaturated solid solution phase or an intermetallic compound. Furthermore, by the heat treatment in the final step, it is possible to disperse and precipitate a metastable phase or a stable phase mainly composed of a fine intermetallic compound in the aluminum alloy base material, and exist finely without agglomeration at the highest temperature possible. It is desirable that the element is capable of forming the obtained precipitation particles. As such an element, one or more selected from Group 4a, Group 5a, Group 6a, Group 7a, Group 8a, Silicon, and Boron of the periodic table may be used. As described above, in order to improve the high temperature strength, it is necessary to finely disperse the precipitated particles and prevent the fine particles from aggregating and growing. For that purpose, it is desirable to mix an element having a relatively slow diffusion rate in aluminum. Among the above-mentioned elements, especially titanium, chromium, vanadium,
Cobalt and iron are preferred.

In typical Al--Cu alloys and Al--Zn--Mg alloys used as high strength alloys, fine particles grow at a heat treatment temperature of 180 ° C. or higher. The reason is C, which is an alloying element
This is because the diffusion rate of u, Zn, and Mg is high in aluminum. That is, the activation energy for diffusion of these elements is about 20 to 35 kcal / mol.
On the other hand, the activation energy for the diffusion of Cr, Ti, Fe, Co, etc. is about 40 to 58 kcal / mol, indicating that the diffusion is slow. It has been pointed out earlier that it is desirable to heat-treat a supersaturated solid solution of an element that is difficult to diffuse, such as the latter, in order to increase the high-temperature strength. It was not possible to form a melted supersaturated solid solution. The inventors have succeeded in forming a metastable phase which is a solid solution in supersaturation with these elements by the above method. The addition amount of these alloy elements is 0.5% or more in atomic ratio, 4
It is desirable that the range does not exceed 0%. A part or all of the alloying elements constitutes a metastable phase such as an amorphous phase or a supersaturated solid solution phase mainly containing aluminum. When the amount of the additional element is less than 0.5%, there is no strengthening effect, and when it is more than 40%, the dispersed particles occupy the majority, and the toughness of the material is lost.

Next, in this embodiment, the method of forming the metastable phase is (A) crushing of various phases in the aluminum powder and the additive metal powder or the aluminum alloy, formation of a new surface, and diffusion between the surfaces. In order to cause diffusion between (B) aluminum and various phase surfaces, an inert atmosphere that keeps the surface of aluminum and the like clean is used, and (C) plastic deformation and diffusion In order to make it easy, it is performed at 100 ° C. or higher and at a stable phase formation temperature or lower. Regarding (A), when using either a raw material mixed with metal powder or an aluminum alloy cast material in which a stable phase is dispersed by a melting method or the like as a work material,
It is necessary to have a sufficient processing rate and load so that each phase repeats rubbing and crushing with each other by the processing, activates the interface, and bonds by diffusion. Due to such strong working, a part of the contacted surface diffuses to form a metastable phase. In the next processing,
Further, in order to form new crushing and an active surface, it is necessary to repeat the processing several tens of times or more. In addition, the working stress is at least 40 times the yield strength of the aluminum alloy.
kg / mm ² or more is required. Desirably, considering the frictional force on the sliding surface of the mold and damage to the mold, 60-200 kg
It is better to process at / mm ² .

The repeating processing method is performed, for example, by the following method. Cruciform compression method: A die having movable punches arranged vertically and horizontally as shown in FIG. 1 is used, and the die is attached to a processing machine usually used for press working or the like for processing. That is, the work piece is put in the center of the die, and first the punch 1
A load is applied to the A direction to compress. The work material is compressed, but since the punch 2 is movable, part of the work material is extruded in the direction perpendicular to the load application direction. Then, the punch 2 applies a load to the workpiece from the B direction to compress the workpiece. Processing is repeated by repeating this operation. According to this processing method, since one punch directly moves the other punch, the deformation amount of the sample can be increased. With this processing method, the volume of the cavity in the mold changes, so cracks may occur in the workpiece, but in order to prevent the occurrence of cracks, the closed type that the volume hardly changes as shown in FIG. There is a cross compression method. In this method, it is desirable to provide a mechanism for retracting the other punch in conjunction with the punch to which a load is applied so that the volume of the cavity does not change.

Extrusion method: This is a method carried out by a die shown in FIG. 3, in which a material to be processed is inserted between punches, alternately extruded, and processed by passing through an orifice portion 31 having a small cross-sectional area. . When a load is applied by the upper punch 1, the other punch 11 descends while keeping the volume of the cavity constant. Therefore, the cross-sectional area of the workpiece is expanded to the diameter of the punch after being extruded. According to this method, the processing rate can be increased, and a material free from cracks can be obtained by performing closed extrusion in which the volume hardly changes.

Oscillating forging method: The workpiece placed in the central portion of the fixed lower die is oscillated by rotating the upper punch to locally fluidize and press the workpiece, and plastically deform the entire workpiece. It is a method of pressing. In this method, although the processing rate per operation is relatively small, it is easy to increase the number of repetitions,
Moreover, since the processing load can be reduced, a material having a large shape can be obtained.

The aluminum alloy produced by the method for producing an aluminum alloy according to the first aspect of the present invention includes aluminum, and a group 4a, 5a, 6a and 7 of the periodic table.
A bulk aluminum alloy comprising at least one metal selected from a group, 8a group, silicon and boron, and a nonmetal, the aluminum alloy comprising:
It is characterized in that it has at least a part of a metastable phase mainly composed of an amorphous phase and / or a supersaturated solid solution phase composed of aluminum, a metal and a nonmetal. The aluminum alloy of the present invention has a great feature in that it has a metastable phase mainly composed of an amorphous phase and / or a supersaturated solid solution phase in at least a part thereof and is in a bulk state.

The aluminum alloy produced by the method for producing an aluminum alloy according to the second aspect of the present invention contains aluminum, and a group 4a, 5a and 6a of the periodic table.
A bulk aluminum alloy comprising at least one or more metals and non-metals selected from the group consisting of genus, 7a, 8a, silicon and boron, the aluminum alloy comprising: It is characterized in that the metastable phase and / or the stable phase mainly composed of the constituted intermetallic compound are finely dispersed. This aluminum alloy has a high tensile strength of 70 kgf / mm ² or more, high hardness, and high heat resistance because the metastable phase and / or stable phase mainly composed of intermetallic compounds are finely precipitated and dispersed. It has a great feature in that it is bulky.

Example 1 Pure aluminum powder of -350 mesh and pure titanium powder of -350 mesh were blended in an atomic ratio of 80:20, mixed sufficiently, and then a hydraulic press was used. About 200kgf / cm
^At a pressure of ² , the height, width, and height are 20, 8.2, and 8. respectively.
It was compacted into 5 mm. The weight of the molded product was 4.1 g. Put this sample in the center of the mold in which the movable punches 1 and 2 are arranged vertically and horizontally as shown in FIG.
In order to prevent oxidation, it was put in an electric furnace and heated to 300 ° C. while Ar gas was caused to flow at a flow rate of 1 to 3 l / min. Then, it was taken out from the furnace, the mold was assembled in a press molding machine having a mechanism for pressing from above and below, and it was compressed from the direction A to a sample thickness of 2 mm as shown in FIG. 1- (b). A part of the sample was extruded in the direction perpendicular to the A direction by this compression. Next, the mold was rotated by 90 ° and then pressed by the punch 2 from the B direction as shown in FIG. 1- (c), and the sample was similarly compressed to a thickness of 2 mm. This operation was repeated 120 times. The initial peak value of the compressive load was about 10 tons, but gradually increased with the increase in the number of repetitions, to 120
After the turn, it was 38 tons. This load value is about 110 kg
This corresponds to f / mm ² . The temperature of the mold after 120 times was lowered to 190 ° C.

The sample taken out by disassembling the mold has some cracks on a part of the surface, but the powders are well bonded and the whole is bulky. There were no cracks or inclusions. As a result of X-ray diffraction of this sample, a pattern as shown in Fig. 4- (a) was obtained, and the result was analyzed. As a result, this sample was face-centered with solid solution of Ti in supersaturation [about 20 atom (at)%]. It became clear that the aluminum alloy had a cubic structure. Conventionally, the maximum solid solution amount of titanium in aluminum is 0.2 at% by the quenching method, whereas a large amount of titanium can be solid-dissolved by the method for manufacturing an aluminum alloy of this example. . When the sample before processing was examined by X-ray diffraction, it was confirmed that it was composed of a mixture of pure aluminum and pure titanium as shown in FIG. 4- (b). Furthermore, a part of the compressed sample is placed in an Ar stream for 35
An X-ray diffraction pattern after heating (aging treatment) at 0, 400, 450, 500, and 600 ° C. for 1 hour each and a result of measuring the hardness at room temperature are shown in FIGS. 5 and 6, respectively.

According to the result of X-ray diffraction, the sample (a) after the repeated processing was a supersaturated solid solution phase of aluminum in which Ti was solid-dissolved, and the hardness thereof was Hv230, but this should be aged. Results in a metastable phase at about 350 ° C [1]
(Al ₅ Ti ₂ ) is formed, and further changes to a metastable phase [2] (Al ₂₃ Ti ₉ ) at a high temperature near 500 ° C. At the same time, the maximum hardness was Hv470. In addition, 600 ℃
In the sample heated to (f), stable phase TiAl ₃ was precipitated and cracks were generated due to the indentation of hardness measurement.

As described above, according to the method for producing an aluminum alloy of this embodiment, it is possible to obtain a metastable phase in which a large amount of titanium is solid-dissolved, which is impossible with the prior art, by repeated processing. The aging treatment has made it possible to produce a bulk material with significantly improved hardness.

(Example 2) A powder of pure aluminum of -350 mesh and a powder of pure chromium of -350 mesh were blended in an atomic ratio of 80:20 and mixed sufficiently. As in Example 1, the operation of compressing the sample to a thickness of 2 mm in a mold kept at 300 ° C. was repeated 150 times. The sample taken out by disassembling the mold had some cracks, but the powder was sufficiently bonded and the whole was in a bulk form. As a result of X-ray diffraction of this sample, a pattern as shown in FIG. 7- (a) is obtained, and the aluminum alloy of this sample is
It was clarified that it is composed of an amorphous phase composed of aluminum and chromium and a chromium alloy in which aluminum is dissolved. When the sample before processing was examined by X-ray diffraction, it was confirmed to be a mixture of pure aluminum and pure chromium as shown in Fig. 7- (b).

(Embodiment 3) Pure aluminum and Al ₃ V alloy powder mixed so that V in atomic ratio of 10% were melted under vacuum and then rapidly cooled and solidified to prepare a sample, which was prepared at 300 ° C. as in Embodiment 1. The operation of holding the sample in place and compressing it to a thickness of 1 mm in the mold was repeated 360 times. As a result of X-ray diffraction of the obtained sample, a pattern showing an aluminum diffraction line and an amorphous phase was observed. This is called mechanical grinding and is a metastable phase due to decomposition of a stable phase (Al ₃ V). Have been formed.

Example 4 The same powder as in Example 1 was used, compounded so that the atomic ratio of titanium to aluminum was 10%, and compressed. The weight of the compact is 5.4.
It was g. This sample was placed in the completely closed mold shown in FIG. 2, held at 300 ° C. as in Example 1, and compressed and deformed 300 times. The sample taken out by disassembling the mold did not have cracks, the powder was sufficiently bonded, and the whole was in a bulk form. With respect to this sample, a tensile test piece was prepared, and after heating at 400 ° C. for 1 hour in an Ar stream, the X-ray diffraction, the hardness at room temperature, and the tensile strength were measured. The sample after the repeated processing consisted of a pure aluminum phase and a supersaturated solid solution phase of aluminum in which titanium was solid-dissolved, and its hardness was Hv120. By heating this sample to 400 ° C. and subjecting it to an aging treatment, a metastable phase (Al ₅ Ti ₂ ) which is an intermetallic compound is formed, and at the same time, the hardness is maximum H.
It became v250. Further, the room temperature tensile strength after repeated processing was 38 kgf / mm ² , but by aging this at 400 ° C., it could be remarkably improved to 75 kgf / mm ² .

Example 5 Using the powder having the same composition as in Example 1, a molded body having a diameter of 15 mm and a height of 25 mm was produced. Next, the extrusion die shown in FIG. 3 was prepared. Graphite was applied to the portion of this mold that contacts the molded body and the sliding surface portion at the time of press-fitting, and then the molded body was placed in this extrusion mold. The mold was then held at 300 ° C. After reaching a predetermined temperature, a load was first applied from one punch by a hydraulic press, then the mold was turned upside down, and the load was applied from the other punch, and the repeated compression processing was repeated 60 times. The processing load was 28 tons (160 kgf / mm ² ) at maximum.
The aluminum alloy after extrusion was solidified and was in a bulk form without cracks. As a result of X-ray diffraction, it was a phase close to pure aluminum and a supersaturated solid solution phase of aluminum containing Ti as a solid solution.

(Example 6) A pure aluminum powder of -350 mesh, a pure titanium powder of -350 mesh and a pure iron powder of -350 mesh were used in an atomic ratio of 90 :.
It was blended so as to be 5: 5 and mixed well. Similar to Example 1, this sample was 2 mm in a mold held at 300 ° C.
The operation of compressing to a thickness was repeated 120 times. The sample taken out by disassembling the mold had some cracks, but the powder was sufficiently bonded and the whole was in a bulk form. As a result of X-ray diffraction and magnetic field measurement of this sample, the pure titanium powder used as the starting material and the -350 mesh pure iron powder were mixed so that the atomic ratio was 90: 5: 5, and they were sufficiently mixed. In the same manner as in Example 1, this sample was compressed to a thickness of 2 mm in a mold held at 300 ° C. for 120 operations.
Repeated times. The sample taken out by disassembling the mold had some cracks, but the powder was sufficiently bonded and the whole was in a bulk form. As a result of X-ray diffraction and magnetic field measurement of this sample, the amounts of pure titanium and pure iron used as starting materials were small, and the aluminum alloy of this sample was composed mainly of an alloy containing aluminum, titanium and iron as a solid solution. It was revealed that it is composed of a metastable phase. When this alloy is heated at 400 ° C for 1 hour, the hardness is Hv before heating.
From 170 to Hv240. The same effect was obtained when silicon or copper was used instead of pure iron.

[Brief description of drawings]

FIG. 1 is a diagram showing a processing step of a repeated processing method (cross type compression method).

FIG. 2 is a diagram showing processing steps of a repeated processing method (closed cross compression method).

FIG. 3 is a diagram showing processing steps of a repeated processing method (extrusion method).

FIG. 4 is a diagram showing the results of X-ray diffraction of a sample before and after repeated processing (cross compression method) in Example 1.

FIG. 5: Samples and 350, 400, 450, 500, 600 that were subjected to repeated processing (cross type compression method) in Example 1
It is a figure which shows the result of having carried out the X-ray diffraction of the sample each hold | maintained at ℃.

FIG. 6 is a diagram showing a relationship between a holding treatment temperature and a Vickers hardness of a sample subjected to repeated processing (cross compression method) in Example 1.

7 is a diagram showing the results of X-ray diffraction of a sample before and after repeating processing (cross compression method) in Example 2. FIG.

[Explanation of symbols]

 1.2. Movable punch 3. Container 31. Orifice 4. Work material

Claims (2)

[Claims] 1. Aluminum and Group 4a of the Periodic Table,
Mixed powder which is a work material made of at least one metal or non-metal selected from the 5a group, 6a group, 7a group, 8a group, silicon and boron, or compacting of the mixed powder. Step of producing a body or cast material, and inserting the work material into a working die, and
While maintaining the temperature at 00 to 400 ° C., plastic deformation such that a diffusion reaction occurs between the structures constituting the work material is repeatedly applied in a state in which at least a part of the work material is constrained, and an amorphous phase and / or Or a step of forming a metastable phase mainly composed of a supersaturated solid solution phase, the method for producing a bulk aluminum alloy having at least the metastable phase as a part thereof. 2. Aluminum and Group 4a of the Periodic Table,
Mixed powder which is a work material made of at least one metal or non-metal selected from the 5a group, 6a group, 7a group, 8a group, silicon and boron, or compacting of the mixed powder. Step of producing a body or cast material, and inserting the work material into a working die, and
While maintaining at 00 to 400 ° C., a plastic deformation that causes a diffusion reaction between the structures constituting the workpiece is repeatedly applied in a state in which at least a part of the workpiece is constrained, and an amorphous phase and / or A step of forming a metastable phase having a supersaturated solid solution phase as a main component, and heat-treating the work material at a temperature of 200 to 500 ° C. to finely disperse the metastable phase and / or the stable phase having an intermetallic compound as a main component. A method of manufacturing a bulk aluminum alloy, which comprises: