JPS63125626A - Method and apparatus for producing metal compound particle dispersed metallic composite material - Google Patents

Abstract

PURPOSE:To efficiently and inexpensively produce a fine metal compd. particle- dispersed metallic material having uniform quality by bombarding a gas contg. the fine metal compd. particles formed by bringing the vapor of the metal and other elements into reaction to the melt of a matrix metal. CONSTITUTION:The metal 82 is heated and melted by a heater 40 in a crucible 38 enclosed by a heat insulating material 42 in an upper housing 10 to generate the vapor of the metal to form the metal compd. The metal vapor thus formed is introduced together with the carrier gas introduced through a preheating chamber 34 into a reaction chamber 50 having a wire net 60 for accelerating the reaction through a conduit 46 penetrating in the melt 82 of the above- mentioned metal without largely decreasing the temp. thereof. The gaseous mixture composed of the fine grains of the metal compd. and residual gas generated in such a manner is adiabatically expanded and ejected from a diaphragm aperture 52 into a composite material producing chamber 54 subjected to evacuation to a vacuum in a lower housing 12. The jet 70 thereof is bombarded to the melt 72 of the matrix metal in a vessel 74 by which the fine metal compd. particles are dispersed.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a composite material made of a metal in which particles of a metal compound, that is, a compound of a metal and another element are dispersed, and more particularly, it relates to a composite material made of a metal in which particles of a metal compound, that is, a compound of a metal and another element are dispersed. Pertains to a method and device for manufacturing metal composite materials.

Prior Art A method for producing a composite material made of a fine powder of a metal compound or a metal matrix in which such a fine powder is dispersed is disclosed in Japanese Patent Application Laid-Open No. 58-15 filed by the same applicant as the present applicant.
No. 0427, JP-A-60-1, JP-A-60828, and JP-A-60-21''346 disclose that a mixed gas of a metal vapor and a reactive gas or fine particles of a metal compound is passed through a constriction passage. Methods are described that involve quenching vapor or particles by adiabatic expansion during production. It is possible to efficiently and inexpensively produce a fine powder of a highly pure metal compound or a composite material containing such a fine powder as dispersed particles.

Problems to be Solved by the Invention However, the following problems occur particularly when a composite material having dispersed particles of fine metal carbide powder is manufactured by the manufacturing method according to the above-mentioned earlier proposal.

The apparatus shown in FIGS. 3 and 4 of JP-A No. 58-150427 or No. 1 of JP-A-60-21346
In the case of the apparatus shown in the figure: ■ Since the reactant gas that generates carbon (for example, methane, ethane, propane, etc.) is heated in the gas preheating chamber, the reactant gas causes a cracking phenomenon in the gas preheating chamber. Generates carbon. If the flow rate of the reaction gas is increased in order to supply enough reaction gas to sufficiently advance the combination reaction in the metal vapor generation chamber, carbon will accumulate in the gas preheating chamber, and in the worst case, the gas preheating chamber will be blocked. This makes it impossible to supply reactive gas to the metal vapor generation chamber.

■In order to avoid such problems, it is possible to supply the reaction gas directly to the metal vapor generation chamber, but if the flow rate of the reaction gas is increased to allow the reaction to proceed sufficiently in the metal vapor generation chamber, A film of metal carbide is formed on the surface of the molten metal in the steam generation chamber, which inhibits the generation of metal vapor, resulting in a reduction in the rate of production of fine powder of the metal compound, and carbon in the conduit with the nozzle at the lower end. In the worst case, the nozzle is blocked, and as a result, it may become impossible to manufacture a composite material containing dispersed particles of fine powder of a metal compound.

In the case of the apparatus shown in FIG. 5 of JP-A-58-1.50427, since the reaction gas is supplied into the reaction chamber 26, the above-mentioned problems (1) and (2) do not occur. In the case of the apparatus, the metal vapor generated in the metal vapor generation chamber 5 is rapidly cooled by adiabatic expansion when passing through the nozzle 11, so that the metal vapor is already relatively low at the time it is introduced into the reaction chamber 26. The temperature of the metal powder has decreased, and since the metal powder is passed through the reaction chamber at a very high speed by the jet stream ejected from the nozzle 11, a sufficient combination reaction can be carried out in the reaction chamber 26. Therefore, it is difficult to produce a fine metal carbide powder of high purity that does not contain unreacted metal, and therefore does not contain unreacted metal parts or unreacted metal particles. Composite materials are difficult to manufacture.

In the case of the production method disclosed in JP-A-60-150828, when the reaction gas is supplied only to the lower chamber 4, double
and ■ problems do not occur. However, since the temperature of the metal particles introduced into the lower chamber 4 has already decreased significantly, they react with the metal particles as in the case of the device described in FIG. It is difficult to quickly react with the gas, and some of the metal particles remain unreacted, making it difficult to produce a composite material that does not contain unreacted metal parts or unreacted metal particles. be.

In addition, since the compounding reaction occurs throughout the F chamber and the flow velocity of the resulting fine powder of the metal compound is low, the efficiency with which the fine powder penetrates into the molten metal of the matrix is extremely low. The problem is that it cannot be manufactured.

The present invention is directed to the case where a metal composite material in which metal compound particles are dispersed is produced by using the method for producing fine powder of a metal compound according to the above-mentioned earlier proposal or by the method for producing a composite material according to the above-mentioned earlier proposal. In view of the above-mentioned problems,
Even when the metal compound is a metal carbide, it is possible to efficiently and inexpensively produce a composite material consisting of a metal matrix in which fine powder of a high-purity metal compound with a very small particle size and substantially uniformity is dispersed. The present invention aims to provide methods and apparatus.

Means for Solving the Problems 1 - According to the present invention, the vapor of the metal that is to constitute the metal compound is introduced into the reaction chamber without greatly reducing its temperature, and the metal compound is A reaction gas containing another element to be formed is introduced into the reaction chamber, and the metal vapor and the other element are reacted by mixing the metal vapor and the reaction gas, and the metal compound thus generated is formed. A method for producing a metal composite material in which metal compound particles are dispersed, the method comprising ejecting a mixed gas of the fine particles and residual gas from the reaction chamber through an adiabatic expansion aperture opening, and colliding the jet with a molten matrix metal; a metal vapor generation chamber, a reaction chamber, a composite material manufacturing chamber, a means for heating the metal vapor generation chamber to a predetermined temperature, and a means for communicating and connecting the metal vapor generation chamber and the reaction chamber, passage means for guiding the metal vapor into the reaction chamber without greatly reducing the temperature; means for supplying a reaction gas into the reaction chamber; a throttle opening that communicates and connects the reaction chamber and the composite material production chamber; By means of a manufacturing apparatus for a metal composite material in which metal compound particles are dispersed, the metal compound particle-dispersed metal composite material manufacturing apparatus has a matrix metal molten metal storage means disposed in the composite material manufacturing chamber at a position receiving the jet from the aperture opening, and a means for reducing the pressure in the composite material manufacturing chamber. achieved.

Functions and Effects of the Invention According to the method of the present invention, metal vapor is introduced into the reaction chamber without greatly reducing its temperature, and is mixed with and reacted with the reaction gas at a relatively high temperature. , the chemical reaction between the metal vapor and other elements constituting the metal compound has sufficiently progressed, and the resulting mixed gas of the fine particles of the metal compound and the residual gas exits the reaction chamber through the adiabatic expansion aperture. Since the jet is made to collide with the molten matrix metal, even when the metal compound is a metal carbide, it is possible to produce a fine amount of high-purity metal compound compared to the conventional manufacturing method according to the above-mentioned earlier proposal. Composite materials containing dispersed particles of powder can be efficiently and inexpensively produced.

Further, according to the manufacturing apparatus of the present invention, the metal vapor generation chamber and the reaction chamber are connected to each other by a passage means that guides the metal vapor in the metal vapor generation chamber to the reaction chamber without greatly reducing the temperature. 9= The aperture opening that communicates and connects the powder collection chamber with the gas mixture containing fine particles of the metal compound generated by sufficient reaction in the reaction chamber is ejected into the composite material manufacturing chamber and converted into molten metal of the matrix metal. Since they are configured to collide, the manufacturing method of the present invention as described above can be carried out easily and reliably.

According to one detailed feature of the method of the invention, the reaction gas is introduced into the reaction chamber in a direction radially inwardly and circumferentially and obliquely towards the diaphragm opening; According to one detailed feature, the means for supplying the reaction gas into the reaction chamber are configured to supply the reaction gas in a direction radially inwardly and circumferentially and obliquely towards the aperture opening. According to such a method and apparatus, it is ensured that the metal vapor and the reaction gas are mixed and reacted well.

According to another detailed feature of the apparatus of the invention, the reaction chamber is provided with means for promoting the mixing and reaction of the metal vapor and the reaction gas introduced into the reaction chamber. According to this configuration, the mixing and reaction of the metal vapor and the reaction gas are further improved.

According to yet another detailed feature of the apparatus of the invention, means are provided for heating the interior of the reaction chamber to a predetermined temperature, which means prevent the metal vapor from condensing between the strips and prevent the reaction gas from condensing. The reaction chamber is maintained at a temperature that facilitates decomposition.

The method and apparatus according to the present invention are applied to the production of composite materials containing dispersed particles of fine powder of metal carbide, which is difficult to produce efficiently and inexpensively using the methods proposed above. Although suitable, the method and apparatus of the present invention may be applied to the production of composite materials having dispersed particles of fine powder of any other metal compound such as metal oxides or metal nitrides.

DESCRIPTION OF THE PREFERRED EMBODIMENTS The invention will be explained in detail below by way of example embodiments with reference to the accompanying figures.

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

In the figure, 10 and 12 indicate the upper housing and the lower housing, respectively. The sock housing 10 includes a main body 16 having a substantially integral bottom wall 14 and extending along an axis A, and a lid member 1 closing one end of the main body.
8 and more. Also, lower housing] 2 is axis A
A main body 2 which extends along the main body 2 and whose upper end is closed by a bottom wall 14
0 and a bottom wall member 22 that closes the lower end of the main body. Between the lid member 18 and one end of the main body 16, the bottom wall 14
and one end of the main body 20, and between the lower end of the main body 20 and the bottom wall member 22, seals 24, 26, and 28 are arranged, respectively. It is blocked. Main body 16
The side walls of and 20 are double cylindrical and define cooling water passages 30 and 32, respectively.

Inside the upper housing 10 is a meander-shaped gas preheating chamber 3.
4, and a graphite crucible 38 having therein a metal vapor generation chamber 36 communicating with the gas preheating chamber. A heater 40 for heating the inside of the crucible to a predetermined temperature is arranged around the crucible 38, and the crucible 38 and the heater 40 are housed in a box-shaped heat insulating material 42 arranged on the bottom wall. . A carrier gas introduction conduit 44 communicating with the gas preheating chamber 34 is fixed to the ceiling wall of the crucible 38.
A metal vapor conveying conduit 46 is fixed to the bottom wall of the crucible 38, and the side portion of the conduit carries the inside of the metal vapor generation chamber 36.
The F side portion of the conduit 46 extends downward through the bottom wall 14 .

A reaction chamber member 48 is fixed to the lower surface of the bottom wall 14 concentrically with the conduit 46 along the axis A, and cooperates with the bottom wall 4 to define a reaction chamber 50.

The reaction chamber 50 is connected to the metal vapor generation chamber 36 by a conduit 46 at the -L end, and communicated with a composite 8-material production chamber 54 in the lower housing through a throttle opening 52 at the lower end. A heater 56 is arranged around the reaction chamber member 48 to heat the inside of the reaction chamber to a predetermined temperature as necessary. Further, a reaction gas is introduced into the reaction chamber 50 through a plurality of reaction gas introduction conduits 58, in the illustrated embodiment four reaction gas introduction conduits 58 spaced apart from each other by 90 degrees in the circumferential direction.

As shown in the figure, the opening 58a of each conduit 58 located inside the reaction chamber 50 is bent so as to extend radially inward, downward, and circumferentially, thereby allowing the reaction gas to flow spirally into the reaction chamber. The metal vapor and carrier gas are uniformly mixed with the metal vapor and carrier gas supplied to the reaction chamber via conduit 46. Further, the length of the reaction chamber 50 in the axial direction is set to a length sufficient to cause sufficient reaction between the metal vapor and the reaction gas. Further, a wire mesh 60 made of a heat-resistant metal is provided in the reaction chamber 50 between the opening 58a of the conduit 58 and the throttle opening 52 so that the metal vapor and the reaction gas are sufficiently mixed and reacted. .

An on-off valve 6 is located in the lower part of the side wall of the lower housing 20.
4 is connected to one end of a conduit 66, and a vacuum pump 68 is connected to the other end of the conduit, thereby reducing the pressure in the composite material manufacturing chamber 54, etc. to a predetermined pressure. . A container 74 for storing a matrix metal molten metal 72 is disposed in the composite 8 material production chamber 54 at the bottom j of the aperture opening 52, that is, at a position that receives the jet stream 70 from the aperture opening. In the illustrated embodiment, the container 74 is formed integrally with the bottom wall member 22, and its main portion protrudes from the bottom wall member in the direction F. A heater 76 is disposed around the container 74 to heat the inside of the container and maintain the molten metal 72 in a molten state. Further, the molten metal 72 is agitated via a shaft 78 by a propeller 80 which is rotationally driven by a motor (not shown).

Note that depending on the combination of metal vapor and reaction gas and the setting of the operating parameters of the apparatus, the energization of the heater 56 may be omitted or the heater 56 itself may be omitted. Further, the wire mesh 60 as a means for promoting homogeneous mixing and mutual reaction between the metal vapor and the reaction gas may be extended across the reaction chamber 50 as long as it can generate turbulent flow of the fluid within the reaction chamber 50. It may be of any other construction, such as a plurality of wires.

Next, an embodiment of the manufacturing method of the present invention, which is carried out using the composite material manufacturing chamber configured as described in -1-- will be described.

First, a 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 a solid or liquid metal to form a metal compound is charged into the metal vapor generation chamber 36. The vacuum pump 68 is operated while introducing carrier gas from the gas introduction conduit. Next, while flowing cooling water into the cooling water passages 30 and 32, the heater 40
(and 56) to heat the metal vapor generation chamber (and reaction chamber 50) to a predetermined temperature. At this stage, the metal charged into the metal vapor generation chamber becomes molten metal 82, and although not shown in the figure, metal vapor is generated from the liquid surface. Next, a reaction gas is introduced into the reaction chamber 50 through the reaction gas introduction conduit 58 .

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 via the conduit 46 without significantly decreasing the temperature, and then flows into the reaction chamber via the conduit 58. The metal vapor and the reaction gas react to form fine particles of a high-temperature metal compound, and the mixed gas containing such fine particles is ejected as a jet 70 from the aperture opening 52, It is rapidly cooled by adiabatic expansion when passing through the opening 1-1.

The jet stream 7 containing the fine powder of the metal compound thus generated collides with the molten metal 72, 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 pressure in each chamber, the flow rate of the carrier gas and the flow of the reaction gas can be adjusted to change the size of the fine powder of the metal compound produced, and the temperature in the metal vapor generation chamber and the reaction gas can be changed. By adjusting the flow rate, etc., the amount of fine metal compound powder produced per unit time can be changed.

Next, what is shown in Figure 1? Some specific examples of the manufacturing method of the present invention performed using a composite material manufacturing apparatus will be described.

Tadashi-Sumi-1 Silicon molten metal is selected as the molten metal 82, and Mad-1 and 7 are selected.
- Select pure aluminum molten metal as the molten metal, select argon as the carrier gas, select methane gas as the reaction gas, and conduct the heating under the conditions shown in Table 1 below without energizing the heater 56. By operating the apparatus shown in Figure 1, a composite material consisting of pure aluminum in which fine powder of silicon carbide was dispersed was produced.

Table 1 Temperature of Si molten metal + 2000℃ Argon flow rate = 2 no/m1n CH4 gas flow ft: 3 J/min Pressure of metal vapor generation chamber 15 Torr Pressure of reaction chamber, 0 Torr
r Pressure in the composite material manufacturing chamber + 2 Torr As a result, silicon carbide fine powder with an average particle size of 50 OA can be collected in the pure aluminum molten metal at a rate of about 40 g/hr,
Compared to the method described in JP-A No. 60-21346, the production speed of a composite material with the same volume fraction of fine powder could be improved by about 5 to 10 times.

In addition, the composite material could be manufactured for about 100 hours without any trouble in the operation of the apparatus due to carbon accumulation or the like.

Specific example 2 Pure aluminum molten metal is selected as the molten metal 82 and the molten matrix metal, argon is selected as the carrier gas, methane gas is selected as the reaction gas, and the heater 5
By operating the apparatus shown in Figure 1 under the conditions shown in Table 2 below without applying electricity, a composite material made of pure aluminum in which fine powder of aluminum carbide was dispersed was manufactured. .

Table 2 Temperature of A1 molten metal: 1800°C Argon flow rate: 2 no/m1n CH4 gas flow rate: 4 no/min Pressure crab in metal vapor generation chamber 17 Torr Pressure crab in reaction chamber 14 Torr Pressure crab in composite material production room 2. 5 Torr.As a result, fine aluminum carbide powder with an average particle size of 40A can be collected in the pure aluminum molten metal at a rate of about 50 g/hr, using the method described in the above-mentioned Japanese Patent Application Laid-Open No. 60-21346. The manufacturing speed of a composite material with the same volume fraction of fine powder could be improved by about 2 to 3 times compared to the case of . In addition, the composite material could be manufactured for about 110 hours without any troubles such as "operation of the apparatus" due to carbon accumulation or the like.

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

[Brief explanation of the drawing]

FIG. 1 is a longitudinal sectional view showing one embodiment of a composite material manufacturing apparatus according to the present invention. ] 0... 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, 3
4... Gas preheating chamber, 36... Metal vapor generation chamber, 38
... Crucible, 40... Heater, 42... Insulation material,
44...Carrier gas introduction conduit, 46...Metal vapor transport conduit, 48...Reaction chamber section, 50...Reaction chamber,
52... Aperture opening, 54... Composite material manufacturing room, 56
...Heater, 58...Reaction gas introduction conduit, 60...
・Wire mesh, 64... Open/close valve, 66... Conduit, 68...
Vacuum pump, 70... Jet flow, 72... Molten metal of matrix metal, 74... Container, 76... Heater. 78...shaft, 80...propeller, 82...molten metal Figure 1

Claims (5)

[Claims] (1) Introducing the vapor of the metal to constitute the metal compound into the reaction chamber without significantly reducing its temperature, introducing into the reaction chamber a reaction gas containing other elements to constitute the metal compound, and By mixing the metal vapor and the reaction gas, the metal vapor and the other element are caused to react, and the resulting mixed gas of the fine particles of the metal compound and the residual gas is passed through the adiabatic expansion aperture to react with the other element. A method for manufacturing a metal composite material in which metal compound particles are dispersed, the method comprising ejecting the jet from a chamber and colliding the jet with a molten matrix metal. (2) In the method for manufacturing a metal composite material in which metal compound particles are dispersed in claim 1, the reaction gas is introduced into the reaction chamber in a direction radially inward, circumferentially, and inclined toward the aperture opening. A method for producing a metal composite material in which metal compound particles are dispersed. (3) a metal vapor generation chamber, a reaction chamber, a composite material production chamber, and means for heating the metal vapor generation chamber to a predetermined temperature;
passage means for communicating and connecting the metal vapor generation chamber and the reaction chamber and guiding the metal vapor in the metal vapor generation chamber to the reaction chamber without greatly reducing the temperature; and means for supplying a reaction gas into the reaction chamber; a diaphragm opening that communicates and connects the reaction chamber and the composite material manufacturing chamber; a matrix metal molten metal storage means disposed within the composite material manufacturing chamber at a position receiving the jet from the diaphragm opening; and a means for reducing the pressure of the metal compound particle-dispersed metal composite material. (4) In the apparatus for manufacturing a metal composite particle-dispersed metal composite material according to claim 3, the means for supplying the reaction gas into the reaction chamber is configured to supply the reaction gas inward in the radial direction, in the circumferential direction, and through the aperture opening. 1. An apparatus for producing a metal composite material in which metal compound particles are dispersed, characterized in that the apparatus is configured to supply a reactive gas in a direction inclined toward. (5) In the apparatus for manufacturing a metal composite particle-dispersed metal composite material according to claim 3 or 4, the reaction chamber contains a mixture of metal vapor and a reaction gas introduced into the reaction chamber; 1. An apparatus for producing a metal composite material in which metal compound particles are dispersed, characterized in that a means for promoting the reaction is provided.