JPH0861860A - Melting, pressurizing test device for metal material - Google Patents

Abstract

PURPOSE: To provide a melting, pressurizing test device for metallic material which can also be applied to sample of low melting point or high melting point and sample of high reacting characteristic, and further intrusion.solidification of molten samples in a pressurizing rod can be prevented. CONSTITUTION: There are provided a hollow cylindrical cartridge 3 heated at a vacuum heating furnace 2, a hollow cylindrical crucible 4 inserted into the cartridge, having one end opened and for storing metallic material 1, a cylindrical pressing plate 5 inserted into the crucible, closing the opening of the crucible and pressurizing the metallic material inwardly, and a pressurizing rod 6 for moving the pressing plate along an axis of the cartridge. One end of the cartridge is provided with an opening part 10 through which the pressurizing rod passes and a main seal plate 16 having a plurality of heat-resistant metallic foils piled up is held between the opening and the opening end of the crucible.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for melting and pressing a metallic material, and more particularly to an apparatus for melting and pressing a metallic material in a vacuum to remove bubbles generated therein.

[0002]

2. Description of the Related Art Various space material experiments using a vacuum / gravity environment in outer space have been studied. For example, a space material experiment that manufactures a high-quality alloy by heating and melting a metal material such as an alloy in a vacuum and weightlessness, and then mechanically pressing the metal material in one direction to remove bubbles generated inside. Is planned and a test apparatus as shown in FIG. 4 is manufactured for this experiment. This melt pressurizing test apparatus includes a vacuum heating furnace 2, a hollow cylindrical cartridge 3 made of a heat-resistant metal heated in the vacuum heating furnace, and a hollow cylindrical crucible 4 inserted in the cartridge and containing a metal material 1 (sample). (Crucible), a pressing plate 5 that functions as a lid of the crucible and a function of pressurizing the sample 1, a pressing rod 6 that moves the pressing plate to the inside of the cartridge, a pressing cylinder 7, and the like. The heating element 2a of FIG. 1 radiatively heats the cartridge 3 in a vacuum to melt the sample 1 inside, so that air bubbles generated in the material are generated in the gap between the crucible 4 and the pressing plate 5, the cartridge 3 and the crucible 4
And the gas is removed through the degassing hole 3a provided in the cartridge 3, and the like, and then the pressing plate 5 is moved to the inside of the cartridge 3 (to the right in the drawing) by the pressing rod 6 and the pressing cylinder 7. Then, the sample 1 was pressed in the axial direction to further remove the air bubbles inside, thereby producing a high quality alloy.

[0003]

In the above-mentioned conventional melting and pressing test apparatus, when the metal material 1 (sample) is heated and melted, the sample melts and expands as the heating progresses, and the melted sample is transferred to the pressing rod portion. It may not be able to pressurize the molten sample after it has penetrated and solidified. That is, there is a problem that the sample is cooled and solidified inside the hollow connecting pipe 8 and the pressurizing rod 6 is fixed so that the pressurizing operation cannot be performed. For this reason,
In the conventional melt pressurizing test apparatus, as shown in FIG. 4, a disk-shaped sealing glass 9 is sandwiched between the pressing plate 5 in the crucible 4 and the sample 1, and the sealing glass 9 is heated by heating. Measures have been taken to soften and prevent leakage of the sample.

However, with such means, a sample having a melting point or a higher melting point than the softening point of the sealing glass cannot exhibit the sealing property of the sealing glass, has no sealing effect, and has a high reactivity (eg, However, TiAl) reacts with the sealing glass 9 and the sealing performance cannot be exhibited.

The present invention was devised to solve such problems. That is, the object of the present invention can be applied to a sample having a low melting point or a high melting point and a sample having high reactivity, and the melting and pressing of a metal material capable of preventing the molten sample from entering and solidifying the pressing rod portion. To provide a test device.

[0006]

According to the present invention, a hollow cylindrical cartridge made of a heat-resistant metal, which is heated in a vacuum heating furnace, and a hollow cylinder which is inserted into the cartridge and has one end opened to accommodate a metal material Cylindrical crucible, cylindrical push plate inserted in the crucible to close the opening of the crucible and press the metal material inward, and a pressure rod for moving the push plate along the axis of the cartridge. And a main seal plate in which an opening through which the pressure rod passes is provided at one end of the cartridge, and a plurality of heat resistant metal foils are laminated between the opening and the opening end of the crucible. Is pinched,
A melt pressure test apparatus for a metal material is provided.

According to a preferred embodiment of the present invention,
An auxiliary seal plate in which a plurality of heat resistant metal foils are laminated is sandwiched between the main seal plate and the pressing plate. The heat resistant metal foil is preferably tantalum foil.

[0008]

The inventors of the present invention have found that even a tantalum foil having a melting point of about 3000.degree.
It was confirmed by experiments that it reacts with molten metal of Al (melting point of about 1530 ° C.) in a short time to form slag. Furthermore, this experiment shows that, in the TiAl melt, the tantalum foil forms a slag with a high melting point, and when this slag exceeds a certain amount, it easily adheres to the surface of the tantalum foil when it contacts another fresh tantalum foil. It was found that a slag film was produced by the method and the reaction with the TiAl melt was suppressed. The present invention is based on this novel finding.

That is, according to the above-described structure of the present invention, a seal plate (main seal) in which a plurality of heat-resistant metal foils are laminated between the opening of the cartridge through which the pressure rod passes and the opening end of the crucible Since the plate and the auxiliary seal plate) are sandwiched, even if the molten TiAl leaks from the pressing plate during the test, it will react with the multiple heat-resistant metal foils (tantalum foils) that make up the seal plate in sequence, and By generating the high melting point slag, the surface of the metal foil near the undissolved pressure rod is filled with the high melting point slag, and the molten sample can be prevented from entering and solidifying into the pressure rod portion.

Further, in the case of a sample having low reactivity, since the tantalum foil itself has a melting point of about 3000 ° C., it was melted between a plurality of laminated heat resistant metal foils (tantalum foil) of the main seal plate. It is possible to prevent a molten sample from entering the solidification rod portion and solidifying it by a part of the sample being filled.

[0011]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT A preferred embodiment of the present invention will be described below with reference to the drawings. In the drawings, common parts are designated by the same reference numerals and used. FIG. 1 is a configuration diagram of a device for testing the durability of a tantalum foil in a TiAl melt.
In this figure, 11 is a crucible, 12 is a hanging fitting, and 13
Is a test piece, and the TiAl melt is 15 in the crucible 11.
It is maintained at a test temperature of 30 ° C and has a thickness of 15
A test piece 13 in which a plurality of μm tantalum foils are stacked to form a bag
A test was carried out in which the moisturizing metal 12 was dipped for a certain period of time. It is known that even a tantalum foil having a melting point of about 3000 ° C. reacts with a molten metal of TiAl, which is a highly reactive sample, in a short time.

[0012] As a result of this test, in the test piece in which five tantalum foils were laminated, after the immersion for about 30 seconds, the surface was reacted, but the melt did not reach the inner surface. Further, in the test piece in which ten tantalum foils were laminated, the inside was completely protected by the high melting point slag even after the immersion for 5 minutes. This is because the high melting point slag generated by the reaction adheres to the surface, protects the outer foil, and blocks the penetration of the TiAl melt.

From the test results, in the TiAl melt, the tantalum foil forms a slag with a high melting point, and when the slag exceeds a certain amount (about 3 g in this test), it comes into contact with another new tantalum foil, It can be seen that it has the effect of easily adhering to the surface of the tantalum foil to form a slag film and suppressing the reaction with the TiAl melt.

FIG. 2 is a block diagram of a melting and pressing test apparatus for metallic materials according to the present invention. In this figure, a melting and pressing test apparatus for metallic materials according to the present invention comprises a hollow cylindrical cartridge 3 made of heat-resistant metal which is heated in a vacuum heating furnace 2 and one end which is inserted into the cartridge 3 and has one end opened. A hollow cylindrical crucible 4 for accommodating 1 and a movably inserted crucible 4 for closing the opening of the crucible 4 and the metal material 1
Cylindrical pressing plate 5 for pressing the inside of the cartridge (to the right in the figure), a pressing rod 6 for moving the pressing plate 5 along the axis of the cartridge 3, and a pressing rod provided outside the vacuum heating furnace 2. A pressurizing cylinder 7 that moves 6 and a hollow connecting pipe 8 that surrounds the pressurizing rod 7 and connects the cartridge 3 and the pressurizing cylinder 7 are provided. Such a configuration is similar to that of the conventional melt pressurizing test apparatus shown in FIG.

In FIG. 2, the metal material 1 is, for example, TiA.
It is a test material (sample) such as 1 and is formed in a short cylindrical shape so that a plurality of crucibles 4 can fit in the crucible 4. Further, partition plates 14 are provided between the respective metal materials 1 so that the metal materials 1 do not mix with each other. With this configuration, it is possible to simultaneously test a plurality of metallic materials 1 having different compositions as test materials.

The crucible 4, the partition plate 14, and the push plate 5
Is preferably made of a ceramic material having high heat resistance, such as calcia (pure CaO). Also, the cartridge 3
Is preferably made of a refractory metal, such as tantalum (Ta), which withstands temperatures of about 3000.degree. Further, in FIG. 2, the pressurizing cylinder 7 has a liquid (for example, deionized water) between them.
Has two pistons filled therein, one of which is connected to one end (the left end in the figure) of the pressurizing rod 6 and supplies pressurized gas to the left side of the piston as indicated by an arrow in the figure. The pressurized gas exerts a hydraulic pressure on the piston, so that the pressure rod 6 can be moved along the axis of the cartridge 3. Further, the push plate 5 is provided with a plurality of circumferential grooves, and a part of the metal material 1 leaked from between the crucible 3 and the push plate 5 is retained in the circumferential grooves.

FIG. 3 is a partially enlarged view of FIG. In this figure, an opening 10 through which the pressure rod 6 penetrates is provided at one end (left end in the figure) of the cartridge 3. A heat resistant shield film 15 is attached to the opening 10. The heat-resistant shielding film 15 is a thin metal film that can prevent the passage of metal vapor at least at the melting temperature of the metal material 1 and can be easily pierced by the pressure rod 6, and preferably has a thickness of about 15 μm. It should be thick tantalum foil. With this configuration, the shielding film 15 can prevent the metal vapor from entering the hollow connecting pipe 8 when the metal material 1 is melted, and prevents the pressure rod 6 from sticking due to the condensation of the metal vapor. can do.

Further, in FIG. 3, between the opening 10 of the cartridge 3 and the opening end 4a of the crucible 4, a main sealing plate 16 having a plurality of heat-resistant metal foils laminated is sandwiched, and further,
An auxiliary seal plate 18 having a plurality of heat-resistant metal foils laminated is sandwiched between the main seal plate 16 and the push plate 5. The metal foil forming the main seal plate 16 is a circular plate having an outer diameter substantially equal to the inner diameter of the cartridge 3, and the opening 1 of the cartridge 3 prevents the TiAl melt from leaking to the pressure rod 6 side.
It is strongly sandwiched between 0 and the open end 4a of the crucible 4. On the other hand, the metal foil forming the auxiliary seal plate 18 is a circular plate having an outer diameter substantially equal to the inner diameter of the crucible 4, and is configured to easily move when the pressing plate 5 is operated by the pressure rod 6. These heat resistant metal foils are tantalum foils having a thickness of about 15 μm. Further, the number of laminated main sealing plates 16 is preferably as large as possible within a range that does not hinder the operation (movement) of the pressing plate 5 by the pressure rod 6, and is preferably at least 5 or more, and the auxiliary sealing plate 18 is made of TiAl. The amount is preferably a certain amount (for example, about 3 g) or more so as to form a high melting point slag that reacts with the melt and exhibits sealing property.

With this structure, Ti melted during the test
Even if Al leaks from the push plate, it will be as shown in FIG.
As schematically shown in FIG. 1, a plurality of heat-resistant metal foils (tantalum foils) forming the auxiliary seal plate 18 first react to generate a certain amount of high melting point slag, and then a plurality of heat sealable metal foils forming the main seal plate 16 are formed. By sequentially reacting with the heat-resistant metal foil, the high melting point slag fills the surface of the metal foil near the unmelted pressure rod, and it is possible to prevent the molten sample from entering and solidifying the pressure rod part. it can. That is, during heating before pressurization (B), TiAl leaked from the pressing plate 5 reacts with tantalum foil to generate slag, which suppresses leakage of TiAl, and after pressurization (C), tantalum is partially sound. The foil remains.

In the case of a sample having low reactivity, the tantalum foil itself has a melting point of about 3000 ° C., so that the heat-resistant metal foils (tantalum foils) laminated on the main seal plate are melted. It is possible to prevent the molten sample from penetrating into the pressure rod portion and solidifying in the same manner, because a part of the sample is filled.
Therefore, the pressing plate 6 is pierced by the pressure rod 6 and the pressure cylinder 7, and the main seal plate 16 and the auxiliary seal plate 18 prevent the molten sample from invading and solidifying the pressure rod portion while the pressing plate 5 is inserted into the cartridge. By moving the metal material 1 inwardly, the metal material 1 is pressed in the axial direction to remove bubbles inside, and a high quality alloy can be manufactured.

The present invention is not limited to the above-described embodiments, and it goes without saying that various modifications can be made without departing from the gist of the present invention.

[0022]

As described above, the melting and pressing test apparatus for metallic materials according to the present invention can be applied to a sample having a low melting point or a high melting point and a sample having high reactivity. It has excellent effects such as prevention of invasion and solidification.

[Brief description of drawings]

FIG. 1 is a configuration diagram of an apparatus for testing the durability of a tantalum foil in a TiAl melt.

FIG. 2 is a configuration diagram of a melting and pressing test apparatus for metallic materials according to the present invention.

FIG. 3 is a partially enlarged view of FIG.

FIG. 4 is a block diagram of a conventional melt pressurizing test apparatus.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Metal material (sample) 2 Vacuum heating furnace 2a Heating element 3 Cartridge 3a Gas vent hole 4 Crucible (crucible) 5 Push plate 6 Pressurizing rod 7 Pressurizing cylinder 8 Hollow connecting pipe 9 Sealing glass 10 Opening 11 Crucible 12 Hanging fitting 13 Test piece 14 Partition plate 15 Shielding film 16 Main seal plate 18 Auxiliary seal plate

Claims (3)

[Claims] 1. A hollow cylindrical cartridge made of a heat-resistant metal, which is heated in a vacuum heating furnace, a hollow cylindrical crucible which is inserted into the cartridge and has one end opened, and which accommodates a metal material, and a crucible inside the crucible. A cylindrical pressing plate that is inserted and closes the opening of the crucible and pressurizes the metal material inward, and a pressing rod that moves the pressing plate along the axis of the cartridge are provided at one end of the cartridge. An opening through which the pressure rod passes is provided, and a main seal plate having a plurality of heat-resistant metal foils laminated is sandwiched between the opening and the opening end of the crucible. Melt pressure tester for metallic materials. 2. The metal material according to claim 1, further comprising: an auxiliary seal plate having a plurality of heat-resistant metal foils laminated between the main seal plate and the pressing plate. Melt pressure test equipment. 3. The heat resistant metal foil is tantalum foil,
The melt pressure test apparatus for a metal material according to claim 1 or 2, characterized in that.