JPH0757898B2 - Method and apparatus for producing metal compound particle dispersed metal composite material - Google Patents

Description

TECHNICAL FIELD The present invention relates to a metal compound, that is, a composite material composed of a metal in which particles of a compound of a metal and another element are dispersed, and more specifically, a metal compound particle dispersion. The present invention relates to a method and an apparatus for manufacturing a metal composite material.

As a method for producing a composite material comprising a fine powder of a metal compound or a metal matrix in which fine powder is dispersed, Japanese Patent Application Laid-Open No. 58-150427 filed by the same applicant as the present applicant.
JP-A-60-150828 and JP-A-60-21346 disclose that a mixed gas of a metal vapor and a reaction gas or fine particles of a metal compound is passed through a throttle passage and adiabatic expansion at that time is performed. Methods are described that include quenching steam or particles. According to these methods, a fine powder of a high-purity metal compound having a very small particle size and being substantially uniform as compared with other conventionally known manufacturing methods, or a composite material containing such fine powder as dispersed particles. Can be manufactured efficiently and inexpensively.

In addition, the present inventor manufactures a metal compound particle-dispersed metal composite material by using the above-described method of manufacturing a fine powder of a metal compound according to the above proposal or the above-described method of manufacturing a composite material according to the above proposal. In view of various problems in the case, in order to improve the method according to the above-mentioned proposal, Japanese Patent Application Nos. 61-270497 and 61-270499 filed by the same applicant as the applicant of the present application In this case, even if the metal compound is, for example, a metal carbide, a composite material comprising a metal matrix in which fine particles of a high-purity metal compound having a very small particle size and being substantially uniform is dispersed efficiently and at low cost. A method and a device that can be manufactured have been proposed.

Problems to be Solved by the Invention However, these Japanese Patent Application Nos. 61-270497 and 61-270499
In the method and apparatus proposed in No. 1, the collection rate of the fine powder produced in the molten metal is as low as about 30%, and therefore, in order to manufacture the composite material more efficiently and cheaply. Therefore, it is desired that the above-mentioned method and apparatus be further improved so that the collection rate of fine powder becomes high.

The present invention has a much higher collection rate in the molten metal of the fine powder produced in order to meet the above-mentioned demands, as compared with the conventionally proposed method and apparatus, and therefore the metal compound particle-dispersed metal composite. It is an object of the present invention to provide a method and an apparatus that enable the material to be manufactured more efficiently and inexpensively.

Means for Solving the Problems According to the present invention, the object as described above is achieved by mixing a vapor of a metal to form a metal compound and a reaction gas containing another element to form the metal compound. Reacting the metal vapor with the other element, ejecting a mixed gas of fine particles of the metal compound thus produced and the residual gas from a nozzle for adiabatic expansion, and causing the jet flow to collide with the molten metal of the matrix metal. In a method for producing a metal compound particle-dispersed metal composite material, an electric field is applied to a region between the nozzle and the molten metal, a method for producing a metal compound particle-dispersed metal composite material, and a metal vapor generation chamber, A composite material manufacturing chamber, a means for heating the metal vapor generating chamber to a predetermined temperature, and the metal vapor generating chamber and the composite material manufacturing chamber are connected in communication with each other at the end on the side of the composite material manufacturing chamber. A throttle passage means having a nozzle for adiabatic expansion, a reaction gas supply means for supplying a reaction gas into the nozzle or the metal vapor generation chamber at a position of the minimum cross section of the nozzle or an upstream side thereof, and the nozzle An electric field is applied to a region between the nozzle and the molten metal storage means, the matrix metal molten metal storage means disposed in the composite material production chamber at a position for receiving the jet flow of And an apparatus for producing a metal compound particle-dispersed metal composite material.

According to the method and apparatus of the present invention, the mixed gas of the fine particles of the metal compound and the residual gas is jetted from the nozzle for adiabatic expansion to be rapidly cooled, and the jet flow collides with the molten matrix metal. However, the fine powder of the metal compound contained in the jet is given a positive or negative electric charge as it passes through the electric field given to the region between the nozzle and the molten metal, and the fine powder is given to it. The electric attraction between the molten metal and the molten metal supplied with a potential opposite to that of the electric charge effectively leads to the molten metal.
As a result, the collection rate of fine powder in the molten metal is significantly improved. Therefore, as compared with the conventional method and apparatus according to the above-mentioned proposal, a composite material containing fine particles of a metal compound as dispersed particles can be used. Further, it can be manufactured more efficiently and inexpensively.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

Embodiment 1 FIG. 1 is a vertical sectional view showing one embodiment of the composite material manufacturing apparatus according to the present invention.

In the drawing, 10 and 12 respectively indicate an upper housing and a lower housing. Upper housing 10 has a substantially integral bottom wall 14 and a body 16 extending along axis A.
And a lid member 18 for closing the upper end of the main body.
The lower housing 12 is composed of a main body 20 extending along the axis A and closed at the upper end by a bottom wall 14, and a bottom wall member 22 closing the lower end of the main body. Seals 24, 26, 28 are arranged between the lid member 18 and the upper end of the main body 16, between the bottom wall 14 and the upper end of the main body 20, and between the lower end of the main body 20 and the bottom wall member 22, respectively. As a result, the inside of the upper housing and the lower housing is shielded from the atmosphere. Body 16 and 20
The side walls of each have a double cylindrical shape, and each has a cooling water passage.
30 and 32 are demarcated.

Inside the upper housing 10, a meandering gas preheating chamber 34
And a graphite crucible 38 having therein a metal vapor generation chamber 36 communicating with the gas preheating chamber. Crucible 38
A heater that heats the inside of the crucible to a specified temperature around the
40 is arranged, and the crucible 38 and the heater 40 are housed in a box-shaped heat insulating material 42 arranged on the bottom wall.

A gas introduction conduit 44 communicating with the gas preheating chamber 34 is fixed to the ceiling wall of the crucible 38, and a metal vapor transfer conduit 46 is fixed to the bottom wall of the crucible 38. An upper portion of the conduit 46 extends upward in the metal vapor generation chamber 36, and a lower portion of the conduit 46 penetrates the bottom wall 14 and extends downward. In the illustrated embodiment, the lower end of the conduit 46 is integrally provided with a tapered divergent nozzle 48 having a throat portion 48a. The nozzle 48 communicates with the composite material manufacturing chamber 50 at its downstream opening end 48b.

A lower end of the side wall of the lower housing 20 is connected to one end of a conduit 66 having an opening / closing valve 64 in the middle thereof, and a vacuum pump 68 is connected to the other end of the conduit, whereby the composite material manufacturing chamber 50 Etc. are reduced to a predetermined pressure. Inside the composite material manufacturing chamber 50, below the nozzle 48, that is, at a position where the jet flow 70 from the nozzle is received, a container 74 for storing the molten matrix metal 72 is arranged. In the illustrated embodiment, the container 74 is formed integrally with the bottom wall member 22, and the main part thereof projects downward from the bottom wall member. A heater 76 for heating the inside of the container 74 to maintain the molten metal 72 in a molten state is arranged around the container 74. Further, the molten metal 72 is agitated by a propeller 80 which is rotationally driven by a motor (not shown) via a shaft 78.

In the illustrated embodiment, the rod-shaped electrode 51 has an insulating seal 51a.
It is fixed to the main body 20 via. One end of the electrode 51 extends below the nozzle 48, and the other end is connected to a negative terminal of the high-voltage DC power supply 53 through a switch 52a by a conducting wire 52. The + terminal of the power supply 53 is connected by a conductor 54 to a terminal 54a extending to the inside of the container 74, so that when the molten metal 72 of the matrix metal is present in the container 74, the molten metal is used for the other electrode. Is designed to act as Therefore, when the switch 52a is closed, the electrode 51 and the molten metal 7
An electric field is formed between the fine particles and the fine particles of the metal compound contained in the jet stream 70, and a negative charge is applied to the fine particles, which effectively guides the fine particles into the molten metal 72 to which a positive potential is applied. .
Of course, electrolysis may be applied with the opposite polarity to that described above.

Next, an embodiment of the manufacturing method of the present invention performed using the composite material manufacturing apparatus configured as described above will be described.

First, the molten metal 72 of the matrix metal is introduced into the container 74, the molten metal is heated to a predetermined temperature by the heater 76, and the solid or liquid metal that constitutes the metal compound is charged into the metal vapor generation chamber 36. The vacuum pump 68 is operated while introducing the mixed gas of the carrier gas and the reaction gas from the gas introduction conduit 44. Next, the switch 52a is closed, and the cooling water passages 30 and 32 are
While flowing cooling water to the heater, the heater 40 is energized to heat the metal vapor generation chamber to a predetermined temperature. At this stage, the metal charged into the metal vapor generation chamber becomes the molten metal 82, and although not shown in the figure, metal vapor is generated from the liquid surface thereof.

In this case, the metal vapor generated from the molten metal 82 is mixed with the carrier gas and the reaction gas in the metal vapor generation chamber, whereby the metal vapor and the reaction gas react with each other to form fine particles of the high temperature metal compound, and the fine particles are included. The mixed gas flows into the nozzle 48 through the conduit 46, jets out as a jet 70 from the downstream opening end 48b of the nozzle, and is rapidly cooled by adiabatic expansion when passing through the nozzle. The fine powder of the metal compound thus produced is conveyed toward the molten metal 72 by the inertia of the jet stream 70, and when passing through the electric field between the electrode 51 and the molten metal 72, a negative charge is given and a positive potential is given. It is effectively guided to the molten metal by the electric attraction between the molten metal and the molten metal, whereby the fine powder penetrates into the molten metal, and the fine powder and the molten metal are uniformly stirred and mixed by the propeller 80.

In this case, by adjusting the flow rate of the carrier gas, the flow rate of the reaction gas, the pressure in each chamber, etc., the size of the fine powder of the metal compound to be generated can be made smaller, and the temperature in the metal vapor generation chamber and By adjusting the flow rate of the reaction gas and the like, the amount of fine powder of the metal compound produced per unit time can be changed.

Next, a specific example of the manufacturing method of the present invention performed using the composite material manufacturing apparatus shown in FIG. 1 will be described.

Example 1 A silicon melt was selected as the metal melt 82, a pure aluminum melt was selected as the matrix metal melt, argon was selected as the carrier gas, and methane gas was selected as the reaction gas, as shown in Table 1 below. By operating the apparatus shown in FIG. 1 under the conditions, a composite material made of pure aluminum in which fine powder of silicon carbide was dispersed was manufactured.

Table 1 Si molten metal temperature: 2000 ℃ Argon flow rate: 2 / min CH ₄ gas flow rate: 3 / min Pressure in metal vapor generation chamber: 15Torr Pressure in composite material production chamber: 2Torr Molten metal-electrode voltage: 60000V Result It is possible to collect silicon carbide fine powder having an average particle size of about 500Å in a molten aluminum at a rate of about 80 g / hr, and in the case of the method described in JP-A-60-21346 described above. In comparison, the collection rate of fine powder was dramatically improved from about 20% to about 60%.

Although the nozzle 48 is a tapered divergent nozzle in the above embodiment, the nozzle provided at the lower end of the conduit 46 may be a tapered nozzle, for example. The reaction gas may be supplied into the nozzle by the reaction gas supply means described in the above-mentioned Japanese Patent Application No. 61-270499, in which case the reaction gas supply means blows out the reaction gas on the downstream side of the nozzle. It is preferably radially outward or radially outwardly inclined toward the opening end, but may be radially outwardly inclined toward the upstream side when viewed in the flow direction of the metal vapor. In this case, a means for preventing metal particles from entering the reaction gas supply conduit is arranged at a position upstream of the tip of the conduit.

Embodiment 2 FIG. 2 is a vertical sectional view similar to FIG. 1 showing another embodiment of the composite material manufacturing apparatus according to the present invention. Incidentally, in FIG. 2, the same members as those shown in FIG. 1 are designated by the same reference numerals as those shown in FIG.

In the figure, 10 and 12 respectively indicate an up housing and a lower housing. Upper housing 10 has a substantially integral bottom wall 14 and a body 16 extending along axis A.
And a lid member 18 for closing the upper end of the main body.
The lower housing 12 is composed of a main body 20 extending along the axis A and closed at the upper end by a bottom wall 14, and a bottom wall member 22 closing the lower end of the main body. Seals 24, 26, 28 are arranged between the lid member 18 and the upper end of the main body 16, between the bottom wall 14 and the upper end of the main body 20, and between the lower end of the main body 20 and the bottom wall member 22, respectively. As a result, the inside of the upper housing and the lower housing is shielded from the atmosphere. Body 16 and 20
The side walls of each have a double cylindrical shape, and each has a cooling water passage.
30 and 32 are demarcated.

Inside the upper housing 10, a meandering gas preheating chamber 34
And a graphite crucible 38 having therein a metal vapor generation chamber 36 communicating with the gas preheating chamber. Crucible 38
A heater that heats the inside of the crucible to a specified temperature around the
40 is arranged, and the crucible 38 and the heater 40 are housed in a box-shaped heat insulating material 42 arranged on the bottom wall. Tsurubo
A carrier gas introduction conduit 44 ′ communicating with the gas preheating chamber 34 is fixed to the ceiling wall of 38, and a metal vapor carrying conduit 46 is fixed to the bottom wall of the crucible 38, and the upper portion of the conduit is made of metal. It extends upward in the steam generation chamber 36, and a lower portion of the conduit 46 penetrates the bottom wall 14 and extends downward.

A reaction chamber member 55 is fixed to the lower surface of the bottom wall 14 along the axis A concentrically with the conduit 46, and the member cooperates with the bottom wall 14 to define a reaction chamber 55a. The reaction chamber 55a is connected at its upper end to the metal vapor generation chamber 36 by a conduit 46, and is connected at its lower end to the composite material manufacturing chamber 50 in the lower housing through a throttle opening (nozzle) 55b. A heater 56 for heating the reaction chamber to a predetermined temperature is provided around the reaction chamber member 55 as needed.
Is provided. The reaction gas is introduced into the reaction chamber 55a through a plurality of, in the illustrated embodiment, four reaction gas introduction conduits 58 which are circumferentially separated from each other by 90 degrees.

As shown, the openings 5 located in the reaction chamber 55a of each conduit 58.
8a is bent so as to extend radially inward, downward, and circumferentially, whereby the reaction gas is spirally introduced into the reaction chamber, and the metal vapor supplied to the reaction chamber via the conduit 46 and It is designed to be uniformly mixed with the carrier gas. The axial length of the reaction chamber 55a is set to a length sufficient for the metal vapor and the reaction gas to sufficiently react with each other.
Further, in order to sufficiently mix and react the metal vapor and the reaction gas, a wire mesh 60 made of a heat-resistant metal is provided in the reaction chamber 55a between the opening 58a of the conduit 58 and the throttle opening 55b. .

A lower end of the side wall of the lower housing 20 is connected to one end of a conduit 66 having an opening / closing valve 64 in the middle thereof, and a vacuum pump 68 is connected to the other end of the conduit, whereby the composite material manufacturing chamber 50 Etc. are reduced to a predetermined pressure. Inside the composite material manufacturing chamber 50, a container 74 for storing the molten metal 72 of the matrix metal is arranged below the throttle opening 55b, that is, at a position where it receives the jet flow 70 from the throttle opening. In the illustrated embodiment, the container 74 is formed integrally with the bottom wall member 22, and the main part thereof projects downward from the bottom wall member. A heater 76 for heating the inside of the container 74 to maintain the molten metal 72 in a molten state is arranged around the container 74. Further, the molten metal 72 is agitated by a propeller 80 which is rotationally driven by a motor (not shown) via a shaft 78.

In the illustrated embodiment, the annular electrode 51 has its arm portion 51.
It is fixed to the bottom wall 22 via an insulating seal 51a at b.
The electrode 51 extends around the axis A below the nozzle 48, and the tip of the arm portion is connected to the negative terminal of the high-voltage DC power supply 53 via a switch 52a by a conductor 52. Power 53
The positive (+) terminal is connected to the terminal 54a extending to the inside of the container 74 by a conductor 54, so that when the molten metal 72 of the matrix metal exists in the container 74, the molten metal acts as the other electrode. It is supposed to do. Therefore, as in the case of the embodiment shown in FIG. 1, when the switch 52a is closed, an electric field is formed between the electrode 51 and the molten metal 72, and the jet flow is generated.
A minus charge is given to the fine powder of the metal compound contained in 70, whereby the fine powder is effectively guided into the molten metal 72 to which a positive potential is given. Of course, also in this embodiment, the electric field may be applied with the opposite polarity to the above case.

Depending on the combination of the metal vapor and the reaction gas and the setting of the operating parameters of the apparatus, the heater 56 may be omitted from energization or the heater 56 itself may be omitted. Further, the wire mesh 60 as a means for promoting the uniform mixing and mutual reaction of the metal vapor and the reaction gas extends across the reaction chamber as long as it can generate a turbulent flow of the fluid in the reaction chamber 50. It may be of any other construction, such as a plurality of wire rods.

Next, an embodiment of the manufacturing method of the present invention performed using the composite material manufacturing apparatus configured as described above will be described.

First, the molten metal of the matrix metal is introduced into the container 74, the molten metal is heated to a predetermined temperature by the heater 76, and the solid or liquid metal that constitutes the metal compound is charged into the metal vapor generation chamber 36, and the carrier is used. The vacuum pump 68 is operated while introducing the carrier gas through the gas introduction conduit 44 '. Next, the switch 52a is closed, and while flowing the cooling water through the cooling water passages 30 and 32, the heater 40 (and 56) is energized to heat the metal vapor generation chamber (and the reaction chamber 50) to a predetermined temperature. At this stage, the metal charged into the metal vapor generation chamber is the molten metal 82
Although not shown in the figure, metal vapor is generated from the liquid surface. Next, from the reaction gas introduction conduit 58 to the reaction chamber 55
Introduce the reaction gas into a.

In this case, the metal vapor generated from the molten metal 82 is mixed with the carrier gas in the metal vapor generation chamber, and the mixed gas flows into the reaction chamber through the conduit 46 without greatly decreasing the temperature,
Mixed with the reaction gas introduced into the reaction chamber via conduit 58,
As a result, the metal vapor and the reaction gas react with each other to form fine particles of the high-temperature metal compound, and the mixed gas containing such fine particles is ejected as a jet flow 70 from the throttle opening 55b, and adiabatic expansion occurs when passing through the throttle opening. Be cooled rapidly. The fine powder of the metal compound thus produced is conveyed toward the molten metal 72 by the inertia of the jet stream 70, and when passing through the electric field between the electrode 51 and the molten metal 72, a negative charge is given and a positive potential is given. Is effectively guided to the molten metal by the electric attraction between the molten metal and
As a result, the fine powder penetrates into the molten metal, and the fine powder and the molten metal are uniformly stirred and mixed by the propeller 80.

In this embodiment also, the size of the fine powder of the metal compound to be produced can be changed by adjusting the flow rate of the carrier gas, the flow rate of the reaction gas, the pressure in each chamber, etc. By adjusting the temperature in the generation chamber, the flow rate of the reaction gas, and the like, the amount of fine powder of the metal compound produced per unit time can be changed.

Next, a specific example of the manufacturing method of the present invention performed using the composite material manufacturing apparatus shown in FIG. 2 will be described.

Example 2 A molten metal 82 and a pure aluminum molten metal are selected as a matrix metal molten metal, argon is selected as a carrier gas, and methane gas is selected as a reaction gas.
By operating the apparatus shown in FIG. 2 under the conditions shown in Table 2 below without energization, a composite material made of pure aluminum in which fine powder of aluminum carbide was dispersed was manufactured.

Table 2 molten metal temperature of 1800 ° C. Argon flow rate: 2 / min CH ₄ gas flow rate: 6 / min metal vapor generating chamber pressure: 18 Torr reaction chamber pressure: 16 Torr composites production chamber pressure: 3 Torr melt - electrode Intervoltage: 60000V As a result, aluminum carbide fine powder having an average particle size of about 400Å can be collected at a rate of about 100 g / hr in the molten aluminum, and it is described in JP-A-60-21346. The collection rate of the fine powder was improved from about 30% to about 60% by about 2 times as compared with the method described above.

In the above, the present invention has been described in detail with respect to specific examples and some specific examples, but the present invention is not limited to these examples and specific examples, and is within the scope of the present invention. It will be apparent to those skilled in the art that various other embodiments are possible.

[Brief description of drawings]

1 and 2 are vertical cross-sectional views showing one embodiment of the composite material manufacturing apparatus according to the present invention. 10 …… Upper housing, 12 …… Lower housing, 14 ……
Bottom wall, 16 …… Main body, 18 …… Lid member, 20 …… Main body, 22 …… Bottom wall member, 24,26,28 …… Seal, 30,32 …… Cooling water passage, 34
...... Gas preheating chamber, 36 …… Metal vapor generating chamber, 38 …… Trubo, 4
0 …… Heater, 42 …… Insulation, 44 …… Gas introduction conduit, 44 ′…
… Carrier gas introduction conduit, 46 …… Metal vapor carrier conduit, 48…
… Tapered divergent nozzle, 48a …… Throat part, 48b …… Downstream opening end, 50 …… Composite material manufacturing room, 51 …… Electrode, 51a …… Insulation seal, 51b …… Arm part, 52 …… Conductor, 52a ...... Switch, 53 ...
… High-voltage DC power supply, 54 …… lead wire, 55 …… reaction chamber member, 55a ……
Reaction chamber, 55b …… Throttle opening, 56 …… Heater, 58 …… Reaction gas introduction conduit, 60 …… Wire mesh, 64 …… Open / close valve, 66 …… Conduit, 68 ……
Vacuum pump, 70 ... Jet, 72 ... Molten metal melt, 74 ... Vessel, 76 ... Heater, 78 ... Shaft, 80 ... Propeller, 82 ... Molten metal

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Junichi Yokkaichi 1 Toyota Town, Toyota City, Aichi Prefecture, Toyota Motor Corporation (72) Nobuo Kobayashi 1 Toyota Town, Toyota City, Aichi Prefecture Toyota Motor Corporation

Claims (2)

[Claims] 1. A method of reacting the metal vapor with the other element by mixing the vapor of the metal that constitutes the metal compound and a reaction gas containing the other element that constitutes the metal compound, thus producing In a method for producing a metal compound particle-dispersed metal composite material, which comprises ejecting a mixed gas of fine particles of a metal compound and a residual gas from a nozzle for adiabatic expansion, and causing the jet flow to collide with a molten metal of a matrix metal, A method for producing a metal compound particle-dispersed metal composite material, which comprises applying an electric field to a region between a nozzle and the molten metal. 2. A metal vapor generating chamber, a composite material manufacturing chamber, a means for heating the metal vapor generating chamber to a predetermined temperature, and the metal vapor generating chamber and the composite material manufacturing chamber are connected and communicated with each other. A throttle passage means having a nozzle for adiabatic expansion at the end on the side of the material manufacturing chamber, and a reaction gas into the nozzle or the metal vapor generation chamber at the minimum cross-section of the nozzle or at a position upstream thereof. Reactive gas supply means, matrix metal molten metal storage means arranged in the composite material manufacturing chamber at a position for receiving a jet flow from the nozzle, means for decompressing the composite material manufacturing chamber, the nozzle and the molten metal storage means And a means for applying an electric field to a region between the metal compound particle dispersed metal composite material and the metal compound particle dispersed metal composite material manufacturing device.