JPH0627020B2 - Method for producing long-fiber metal composite material - Google Patents

Description

TECHNICAL FIELD The present invention relates to a method for producing a long fiber metal composite material using metal powder, particularly a difficult-to-process Ti-based and Ni-based composite material.

(Prior Art) At present, long-fiber metal composite materials are usually formed by a so-called drum winding method in which a metal foil having a thickness of 0.05 mm to 1 mm and a fiber filament are wound around a drum at regular intervals and fixed with a resin. Cut out the fiber mat and the specified size,
It is manufactured by a foil metallurgical method of alternately laminating, fitting in a mold, degreasing in a vacuum, preliminarily solidifying with a vacuum hot press, hot isostatic pressing (HIP) or vacuum hot pressing, and then HIP solidifying.

However, in general, metals are alloyed and have poor spreadability, and in particular, high alloyed Ti alloys and Ni alloys cannot be processed into thin foils. this house,
In the case of Ti alloy, the alloyed two phase (α phase β phase) alloy is
Although Ti-6 Al-4V alloy foil is made for experimental Ti alloy matrix composite material, it is expensive and not industrially profitable.

With regard to Ni-based alloys, alloys containing a large amount of γ (Ni ₃ Al · Ti) have high deformation resistance and are difficult to process into foil.

Therefore, the above-mentioned foil metallurgy method uses the above-mentioned Ti alloy, Ni
Not suitable for base alloys.

However, recently, as the use of heat-resistant alloy materials has expanded, the functional roles of Ti alloys and Ni-based alloys have been great, and the development of composite materials containing these is one of the important concerns.

(Problems to be Solved by the Invention) Therefore, the present inventors have dealt with the above-mentioned trends and
As a result of working on the development of Ni-based and Ni-based composite materials and investigating the manufacturing method suitable for them, we have reached the utilization of metal powder of Ti alloy and Ni-based alloy.

Conventionally, there are mechanical and physical methods for producing metal powders, which are widely used for producing each metal powder.
For i, Ti alloys, Ni-based alloys, etc., there are physical rotating electrode method, inert gas atomizing method, etc. In the rotating electrode method, a powdered material is used as an electrode, and an arc or plasma is applied while rotating to melt the molten portion. It is a method of producing powder by spinning with centrifugal force, which is mainly used for the production of Ti and Ti alloy powders.On the other hand, the inert gas atomization method atomizes molten metal with an inert gas to produce powder. How to get Ni
Many base alloys are produced by this.

Therefore, in any case, even if it is a material such as a Ti-based or Ni-based alloy that is difficult to process into a foil, powder has been produced conventionally.

The present invention focuses on the powders of such Ti alloys and Ni-based alloys, and by forming the powders into a sheet similar to a foil, the powders are alternately laminated with a fiber filament array mat. The purpose is to produce Ni-based and Ni-based composite materials.

(Means for Solving Problems) That is, the feature of the method of the present invention that meets the above-mentioned object is that a metal powder selected from the above Ti alloy and Ni-based alloy is formed into a desired thickness by using a binder. Using a sheet formed by molding, this and a fiber mat having fiber filaments arranged at regular intervals and fixed with a binder are alternately laminated to form a preform, and the preform is degreased in vacuum and then vacuumed. A method for producing the above composite material by a powder sheet method, in which a long fiber metal composite material is produced by hot pressing, HIP treatment, or preliminary solidification by a treatment hot press, and then solidifying by HIP treatment.

Here, the metal powder sheet is formed by using a knife edge to form a mixture of a required alloy powder selected from a Ti alloy and a Ni-based alloy on a release paper such as a polyester film and a binder. The alloy powder used has a particle size of 70% or less of the powder sheet thickness after molding. Specifically, since the powder particle diameter used for sheet formation limits the sheet thickness, 0.5 mm or less is preferable in view of the fiber volume ratio.

The lower limit is not particularly limited, but the trapped amount of oxygen and nitrogen of the solidified molded product increases as the particle size decreases, so that it is preferable to set it to 10 μm or more.

FIG. 1 shows the relationship between the particle size of such alloy powder and the powder sheet thickness (powder-binder mixture viscosity 70,000-13
The maximum particle size of the powder is at most 0.6 mm when the powder sheet thickness is 1 mm at the maximum.
If the powder particle size includes more than 70% of the powder sheet thickness after molding, the powder is clogged in the gap between the release paper and the knife edge,
This is not preferable because it causes streak defects.

Also, the viscosity of the mixture of the binder and the powder at the time of molding has an influence on the sheet production.
A range of P to 150,000 CP is effective.

FIG. 2 shows the relationship between the particle size and the viscosity of this alloy powder. At 50,000 CP or less, the alloy powder and the hinder tend to separate during molding, resulting in a stripe pattern of low particle density.

On the other hand, when it is 150,000 CP or more, the viscosity of the mixture becomes too high, so that the surface of the sheet is roughened and a sheet in which the mixture is discontinuous is formed.

Also, the powder sheet is dried after being shaped with a knife edge, but this drying is preferably carried out at 60 ° C. or lower, and if it is higher than that, bubbles may occur between the sheet and the release paper and the surface may become uneven, which is desirable. Absent.

The binder used in the method of the present invention is usually an acrylic resin-based binder prepared by dissolving an acrylic resin in an organic solvent. As a solvent, a solvent having a low vapor pressure such as Solvesso 150 (trade name) has a slower drying speed than a solvent having a high vapor pressure such as toluene or acetone, and the surface texture of the sheet after drying is good.

On the other hand, the fiber mat used is one in which long fiber filaments are arranged at regular intervals and fixed with a binder.
SiC fibers are most commonly used as the fibers.

As SiC fiber, pyrolytic SiC is deposited on the surface of carbon fiber or tungsten wire by the CVD method, and S
Fibers made into iC filaments, SiC whiskers, SiC fibers produced by stereopolymerization from polycarbosilane, etc. are conceivable, but they are used in consideration of their respective characteristics.

Further, it is practical to use the above-mentioned acrylic resin-based binder as the binder to be fixed.

The powder sheet fiber mats respectively obtained as described above are cut into desired dimensions, alternately laminated, laminated with a binder and dried integrally, and then subjected to subsequent press treatment as a preform.

As the press treatment, hot pressing or HIP treatment under vacuum or pre-solidification by hot pressing in advance, and then H
Either method of IP processing can be implemented,
The most effective method is a method in which HIP treatment is performed after preliminary solidification by the final hot pressing.

The fiber volume fraction of the composite material solidified and formed in this way is determined by the apparent density, thickness, fiber diameter, fiber spacing, etc. of the particles of the powder sheet. Of these, sheet thickness, fiber diameter,
Since the fiber spacing is determined in advance, it is possible to easily design the volume ratio of the composite material after solidification molding by measuring the apparent density of the particles of the powder sheet molded body.

(Examples) Specific examples of the method of the present invention will be described below.

Each fiber-metal composite material was experimentally manufactured by applying the method of the present invention according to each of Samples 1 to 6 in the table below. On the other hand, for comparison, a composite material was manufactured by a conventional foil metallurgy method, and is also shown as Sample 7.

Each powder of the method of the present invention used in the experiment was used as a test material having a particle size of not more than each particle size.

The viscosity of the powder / binder mixture was adjusted by the amount of the powder / binder solvent. Hot press is 0.5 kg before heating
/ Mm ² was added to prevent the shrinkage due to softening of the resin due to heating and the disorder of the regularity of the arrayed fibers due to the vaporization of the resin.

The pressure of 0.5 kg / mm ² does not damage the fiber.
The heating was carried out at a slow heating rate of 3 ° C to 5 ° C / min because vaporization of the resin occurs at 200 ° C to 600 ° C.

The applied pressure is 900 ℃, 5 kg / mm ² , 15-30 minutes, it does not solidify yet, but 950 ℃, 10 kg / mm ² , 120
It was solid enough in minutes.

Each example will be described below.

In the above table, each press treatment and evaluation of the material test material were performed by the fiber volume fraction and the tensile strength, and the results are shown in FIG.

In the figure, ○ indicates Ti-6Al-4V / SiC composite material, △ indicates Ti-6Al-2Sn-4Zr-6Mo / SiC composite material, black indicates test temperature at room temperature, and others indicate test. Temperature 450
This is the case of ° C.

From the results of the above table and FIG. 3, except for the test conditions of Sample No. 2, Ti-6Al-4V / SiC composite material has no process and the difference between powder and foil (foil) is not sufficiently observed.
Ti-6Al-2Sn-4Zr-, which is usually impossible by foil metallurgy
The 6Mo / SiC composite material is produced by the method of the present invention, and Ti-6Al-4V produced by the method of the present invention.
Higher values were obtained at room temperature and 450 ° C than the / SiC composite material.

(Effects of the invention) The present invention is a metal powder sheet obtained by molding a metal powder consisting of a Ti alloy or a Ni-based alloy to a desired thickness using a binder as described above, and a fiber in which fibers are arranged at regular intervals and fixed with a binder. This is a method in which a mat is alternately laminated to form a preformed body, which is then preliminarily solidified by hot pressing, HIP or hot pressing under vacuum, and then HIP is performed for solidifying and molding. It can be applied to alloys or Ni-based alloy materials without limitation, and has the effect of producing fiber-metal composite materials without being restricted by the type of alloy compared to conventional foil metallurgy. However, it has a remarkable effect that a Ti-based and Ni-based composite material, which has been considered difficult to manufacture due to difficult workability, can be easily and industrially manufactured.

In addition, the powder sheet method of the present invention is no different from the conventional foil metallurgy method in its characteristics, and has sufficient and desired functional characteristics, and also in the characteristics of the composite material which cannot be obtained by the foil metallurgy method. It has excellent properties and is expected to be widely used in various fields in the future.

[Brief description of drawings]

FIG. 1 is a chart showing the relationship between the sheet thickness of the powder sheet and the powder particle diameter in the method of the present invention, FIG. 2 is a chart showing the relationship between the viscosity of the powder-binder mixture and the powder particle diameter, and FIG. It is an evaluation chart which shows the fiber volume fraction and the tensile strength of the Ti alloy / SiC (CVD) composite material in an Example.

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Claims (3)

[Claims] 1. A metal powder sheet obtained by molding a metal powder selected from a Ti alloy powder and a Ni-based alloy powder to a desired thickness using a binder, and an array fiber in which fiber filaments are arrayed at regular intervals and fixed with a binder. After alternately laminating mats to obtain a preform, the preform is hot-pressed under vacuum or hot isostatic press or pre-solidified by hot press, and then hot isostatic press is applied for solidification. A method for producing a long-fiber metal composite material, which comprises molding. 2. The method for producing a long fiber metal composite material according to claim 1, wherein the metal powder sheet is a sheet formed by using metal powder having a particle diameter of 70% or less of the sheet thickness. 3. The metal powder sheet has a viscosity of 50,000 CP.
The method for producing a long-fiber metal composite material according to claim 1 or 2, which is formed from a powder-binder mixture of 150,000 CP.