JPS6139370B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to the production of fine alloy powder, and more specifically, the invention relates to the production of fine alloy powder, and more specifically, the invention relates to the production of fine alloy powder.
This invention relates to an apparatus for manufacturing the following alloy fine powder.

PRIOR TECHNOLOGY Fine powders of pure metals and alloys used as dispersants in sintered materials and particle-dispersed composite materials are generally produced by mechanically crushing solid metals, by spraying molten metal, or by impinging on other objects at low temperatures. The particle size of the fine powder produced by these methods is about 10 to 500 μm.

In general, the smaller the particle size of the fine metal powder, the higher the density of the sintered body, and the better the mechanical properties of the particle-dispersed composite material. efforts are being made vigorously. For example, when a metal is heated in a vacuum, it becomes atoms and evaporates, and when cooled on the surface of a low-temperature object, it becomes a solid. This phenomenon is known as vacuum evaporation, and attempts have been made to utilize this phenomenon to produce fine metal powder. Also, instead of a vacuum atmosphere,
When a metal is evaporated in an inert gas at 1000 atmospheres, the metal vapor is cooled by the inert gas, becomes supersaturated, and condenses into a fine powder in a liquid or solid phase. This method is called evaporation in gas, and fine metal powder has been experimentally produced in small quantities by this method.

Problems to be Solved by the Invention According to these methods, fine metal powder with a particle size of 1 μm or less can be produced, but since all of these methods utilize a slow evaporation-condensation phenomenon, , productivity is extremely low. In order to increase productivity in these methods, it is necessary to quickly and continuously take out the generated metal vapor from the metal vapor chamber and cool it. Therefore, the metal vapor is taken out from the metal vapor chamber in a plasma airflow. Methods such as colliding with a water-cooled copper plate and absorbing metal vapor into dripping oil have been proposed, but the former method requires expensive and large-scale equipment.
It is difficult to efficiently and inexpensively mass-produce fine metal powder with a uniform particle size using these methods because the absorption efficiency is not necessarily sufficient in the latter method.

In view of the above-mentioned various problems in conventional methods and devices for producing fine metal powder, the inventors of the present application,
We considered improving productivity by rapidly and continuously passing the generated metal vapor through a nozzle to quench it. Initially, we conducted experimental production of fine metal powder using a normal nozzle (tapered nozzle).
We succeeded in producing 100g of metal fine powder per hour. As a result of further intensive study, the inventors of this application found that by using a wide-spread nozzle (also called a Laval tube) used in rocket propulsion devices as a cooling nozzle, metal particles with finer and more uniform particle size could be produced. We have discovered that powder can be efficiently mass-produced.

In addition, the inventors of the present application have proposed a method for rapidly cooling metal vapor by self-adiabatic expansion through a nozzle, in which metal vapor is mixed with an inert gas such as argon or helium, and the mixed gas is passed through a nozzle to rapidly cool the metal vapor. For example, the inert gas functions as a carrier gas, and the metal vapor generated from the surface of the molten metal is guided to the nozzle more quickly by the inert gas, and grain growth due to aggregation of metal vapors is suppressed. This makes it possible to produce metal fine powder with even more uniform particle size even more efficiently, and furthermore, it is possible to easily control the pressure and pressure ratio before and after the nozzle, so the cooling rate of the mixed gas and the metal fine powder can be easily controlled. It has been found that the grain size of the powder can be easily controlled.

According to the results of various experimental studies conducted by the present inventors, fine metal powder with a particle size of several hundred angstroms or less can be efficiently mass-produced, but metals generally consist of two or more elements. It is often used as an alloy, and as for metal fine powder, alloy fine powder is preferable to pure metal fine powder, and the actual demand for alloy fine powder is much greater. FIG. 6 shows the vapor pressure of various metals, and it can be seen from FIG. 6 that the vapor pressure of metals varies greatly depending on the type. For example, the vapor pressures of Al, Cu, and Ni at 1800°C are 12 Torr, 5.6 Torr, and 0.3 Torr, respectively. The boiling points of metals also vary greatly depending on their type. Therefore, an Al-Ni alloy of a certain composition can be prepared under reduced pressure.
When heated to 1800°C, only aluminum vapor is produced at first, and nickel vapor is produced only after a while.

Therefore, even if each metal vapor is generated by heating an alloy with a desired composition, it is difficult to produce alloy fine powder with a uniform composition from the start of the process to the end of the process, and the resulting alloy The composition of a fine powder is determined by the vapor pressure ratio of the metals that constitute it, and it is difficult to set the composition to a desired ratio depending on the use of the fine alloy powder.
In view of this, the inventors of the present application have conducted various experimental studies and found that two or more types of metal vapor and a gas such as an inert gas are mixed to form two or more types of mixed gas, and the mixed gas It has been found that fine alloy powder having a desired and uniform composition can be easily produced by passing the two through separate nozzles and quenching them by adiabatic expansion, and then mixing the quenched gas mixture.

Generally, the finer the alloy powder, the larger the ratio of surface area to mass, and the stronger its activity.It is often observed that when alloy powder is taken out into the atmosphere under reduced pressure, it ignites even at room temperature. be done. For this reason, post-treatment has traditionally been carried out to form an oxide film on the surface of fine alloy powder under controlled conditions before it is taken out into the atmosphere. And in equipment, deterioration in quality of fine alloy powder and increase in cost are unavoidable.

The inventors of the present application have conducted various experimental studies on this point, and have found that liquids that have fluidity and evaporate in a small amount even under vacuum, such as vacuum oil and electrical insulation oil, are placed directly under the nozzle. By setting up a liquid bath consisting of The metal particles are very efficiently collected and dispersed, and because they exist in isolation from each other in the liquid, there is almost no aggregation of the metal particles, resulting in extremely fine alloy powder with a more uniform particle size. In addition, the fine alloy powder introduced into the liquid forms a colloid solution with the liquid, so even if it is taken out into the atmosphere, it will not come into contact with oxygen, so there is no risk of ignition. Handling such as transportation becomes much easier than when using only fine powder. Furthermore, since the fine powder is stabilized by the substances that make up the liquid, such as oil, there is little risk of it catching fire even if the fine powder is left in the atmosphere after being separated from the liquid by vacuum distillation. I discovered something. The liquid constituting the liquid bath may be, for example, an organic solvent whose evaporation is suppressed by being cooled with liquid nitrogen or the like.

The present invention is based on the knowledge obtained as a result of various experimental studies conducted by the inventors of the present invention as described above, and the present invention provides an alloy that allows mass production of extremely fine alloy powder with uniform particle size efficiently and inexpensively. The purpose is to provide a fine powder manufacturing device.

Means for Solving the Problems According to the invention, the above-mentioned object is achieved by providing a first metal vapor chamber 5 in which a first metal vapor is generated.
, a first heating means 7 for heating the first metal vapor chamber, a first gas introduction means 3 for introducing gas into the first metal vapor chamber, and communication with the first metal vapor chamber. a second metal vapor chamber 5' for generating a second metal vapor therein; and a second heating means 7' for heating the second metal vapor chamber. , a second gas introduction means 3' for introducing gas into the second metal vapor chamber, a second outlet passage means 2a' communicating with the second metal vapor chamber, and a second gas introduction means 3' for introducing gas into the second metal vapor chamber; an alloy fine powder recovery zone 11 communicating with the first and second metal vapor chambers via outlet passage means; The fluid of the jet 14,1
first and second nozzles 13, 13' that inject the particles 4' so as to mix them with each other; a forced cooling plate 15 or a liquid bath 22 for collecting fine alloy powder, and a pressure reducing means 20 for reducing the pressure in the fine alloy powder collection zone.
This is achieved by a fine alloy powder manufacturing apparatus including:

According to the present invention, the first and second metal vapors are generated in the first and second metal vapor chambers, respectively, and the inert gases are introduced into each metal vapor chamber through the first and second gas introducing means, respectively. By introducing the gas, grain growth due to aggregation of the metal vapor is suppressed by the inert gas, and the metal vapor is quickly and continuously guided to the nozzle by the inert gas.
The metal vapor is rapidly cooled by adiabatic expansion by the nozzle, and it is possible to mix two types of metal vapor in any ratio and combine them with each other, so it is possible to
It is possible to efficiently and inexpensively mass-produce the following fine alloy fine powders with uniform particle sizes and arbitrary and uniform composition. In particular, according to the alloy fine powder manufacturing apparatus in which the alloy fine powder collecting means is a liquid bath, the increase in particle size due to collective growth of the metal fine particles after being ejected from the nozzle is effectively suppressed, and the alloy fine powder is Since it is stabilized, it is possible to mass-produce stable fine alloy powder that is even finer and has a more uniform particle size more efficiently and at a lower cost.

Further, according to the present invention, it is possible to pass a mixed gas of metal vapor and inert gas through the nozzle, so that
The pressure and pressure ratio of the mixed gas before and after the nozzle can be controlled relatively easily by controlling the flow rate of inert gas introduced into the metal vapor chamber and the flow rate of gas discharged from the alloy fine powder recovery zone to the outside of the device. This makes it possible to easily control the cooling rate of the mixed gas and the particle size of the fine alloy powder.

The cooling nozzle used in the present invention may be either a wide-spread nozzle or a tapered nozzle, but the cooling rate of the mixed gas can be increased as much as possible by increasing the flow rate of the mixed gas passing through the nozzle. However, in order to efficiently produce fine, high-quality alloy fine powder with uniform particle size, it is preferable to use a wide-divergent nozzle.

The pressure of the mixed gas upstream of the cooling nozzle,
The temperature is P ₁ (Torr) and T ₁ (〓), respectively, and the pressure and temperature downstream from the nozzle are P ₂ respectively.
(Torr) and T ₂ (〓), the following equation holds true from the relationship of adiabatic expansion.

T ₂ = T ₁ × (P ₂ /P ₁ )K-1/K (K = Specific heat ratio of gas body) As can be seen from this formula, the larger the pressure ratio P ₁ /P ₂ , the more downstream from the nozzle The temperature of the mixed gas can be lowered. Especially when the nozzle is a tapered nozzle, when the pressure ratio P ₁ /P ₂ reaches approximately 2.
The flow velocity of the gas passing through the nozzle reaches the sonic velocity, and even if the pressure ratio is increased further, the degree of expansion cannot be increased, and therefore the temperature of the gas cannot be lowered any further. In some cases, when the pressure ratio is increased to 2.1 or more, the degree of expansion of the gas also increases, and the gas flow velocity becomes supersonic. Therefore, by increasing the pressure ratio, the temperature of the gas can be further lowered. can do.

Furthermore, in the present invention, a metal vapor chamber, a heating means,
Three or more sets of gas introduction means, outlet passage means, and nozzles may each be provided, and the apparatus for producing fine alloy powder with such a configuration can easily and efficiently produce fine powder of an alloy having any composition of ternary or higher. can be manufactured. In addition, in the apparatus for producing fine alloy powder of the present invention, the gas introduced into the metal vapor chamber through the gas introducing means, such as nitrogen gas or ammonia gas, is at high temperature with the metal constituting the metal vapor. It may be a reactive gas that reacts to alloy the metal, and the metal charged into the metal vapor chamber and evaporated may be an alloy, and these may also be used to form a ternary or higher alloy. fine powder can be efficiently produced.

The invention will now be described in detail by way of example embodiments with reference to the accompanying drawings.

Embodiment 1 FIG. 1 is a schematic diagram showing one embodiment of an apparatus for producing fine alloy powder according to the present invention. In the figure,
Reference numeral 1 designates a furnace shell forming a substantially hermetic container, in which crucibles 2 and 2' are arranged. The crucibles 2 and 2' have gas preheating chambers 4 and 4' with gas introduction ports 3 and 3', respectively;
It has metal vapor chambers 5 and 5' communicating with the gas preheating chamber. Heaters 7 and 7' are arranged around the crucibles 2 and 2' to maintain the gas preheating chambers 4 and 4' and the metal vapor chambers 5 and 5' at predetermined temperatures _T1 and _T1 ', respectively. These heaters 7
and 7', the metal charged into the crucibles 2 and 2' is melted into molten metals 8 and 8', which are further vaporized as metal vapor and introduced into the metal vapor chamber from the gas introduction port. The gas is preheated to a predetermined temperature. A heat insulating material 9 is arranged between the heaters 7 and 7', so that the temperature T ₁ in the gas preheating chamber 4 and the metal vapor chamber 5 of the crucible 2 and the gas preheating chamber 4' and the metal vapor chamber of the crucible 2' are maintained. The temperature T ₁ ' in the chamber 5' can be arbitrarily controlled independently of each other, and the gas is introduced into the gas preheating chamber and the metal vapor chamber from a gas cylinder (not shown) through the gas introduction ports 3 and 3'. By controlling the amount of inert gas, the metal vapor chambers 5 and 5'
The internal pressures P ₁ and P ₁ ' can be arbitrarily controlled independently of each other.

The bottom walls 10 and 10' of the crucibles 2 and 2' have outlet passages 12a and 12a', respectively, which connect the metal vapor chambers 5 and 5' with a recovery zone 11 provided below the crucibles in the furnace shell 1. Conduit 12 defining
and 12' are fixed, and the lower ends of these conduits are provided with diverging nozzles 13 and 13', respectively. The diverging nozzles 13 and 13' are inclined in directions facing each other so that the jets 14 and 14' ejected from them collide and mix with each other. In the recovery zone 11, a sorption plate 15 as a means for collecting fine alloy powder made of a water-cooled copper plate is arranged at a position evenly spaced apart from the diverging nozzles 13 and 13'. A mixed jet 16 formed by the jets 14 and 14' ejected from the diverging nozzles 13 and 13' collide with each other and mix with the sorption plate 15, and as a result, the alloy is deposited on the surface of the sorption plate 15. Fine powder 17 is collected. The recovery zone 11 is also connected by a conduit 18 to a vacuum pump 20 via an on-off valve 19.
1. The pressure inside the metal vapor chambers 5 and 5' is reduced, whereby the pressures P ₂ , P ₁ , and P ₁ ' are respectively reduced to predetermined pressures. Although not shown in the figure, a detection unit is provided for detecting and displaying the temperatures T ₁ , T ₁ ' and the pressures P ₁ , P ₁ ', P ₂ so that they can be accurately controlled.

Next, the operation of the apparatus for producing fine alloy powder constructed as described above will be explained with reference to an actual operation carried out to produce fine Ni--Cu powder.

Operation (1) First, 30 g of metallic copper (99.9% Cu, remainder impurities) and metallic nickel (99.8% Ni, remainder impurities) are charged into the metal vapor chambers 5 and 5', and argon gas is introduced into the gas introduction port 3. The gas is introduced into the metal vapor chambers 5 and 5' through the preheating chambers 4 and 4' from Temperature T ₁ ,
T ₁ ' is set to approximately 1650℃ and approximately 2000℃, respectively, thereby melting metallic copper and metallic nickel to form copper molten metal 8.
Copper vapor and nickel vapor are generated from the respective molten metals, and the vacuum pump 20 is operated to control the amount of argon gas introduced from the gas introduction ports 3 and 3' and the amount of opening of the on-off valve 19. By controlling the pressures P ₁ , P ₁ ' in the metal vapor chambers 5 and 5' and the pressure in the recovery zone 11
_P2 was set to about 10 Torr, about 10 Torr, and 1 to 2 Torr, respectively. In addition, the distance from the center of the tip of the wide-spread nozzles 13 and 13' to the center of the collision point of the jets 13 and 14' and the distance from the center of the collision point to the surface of the sorption plate 15 are set to approximately 15 cm and approximately 5 cm, respectively. did.

In this case, the copper vapor and nickel vapor generated from the copper molten metal 8 and the nickel molten metal 8' are mixed with argon gas in the metal vapor chambers 5 and 5', respectively, to form a mixed gas, and each mixed gas is passed through the wide-spread nozzle 13, Due to _{self -} adiabatic expansion due to
It is rapidly cooled to about 860℃ (estimated), and during the rapid cooling, the copper vapor and nickel vapor become essentially liquid phase copper particles and nickel particles, and these particles collide with each other to form copper and nickel. After the composite fine particles were agglomerated, they collided with the sorption plate 15 together with argon gas, whereby the Ni--Cu fine powder 17 was collected on the sorption plate 15.

The time required to process all the metallic copper and metallic nickel was about 17 minutes, and the particle size range of the produced Ni-Cu fine powder was 150-400 Å, with an average particle size of about 250 Å. .

Operation (2) Under the same operating conditions as above, the nozzles provided at the lower ends of conduits 12 and 12' were changed to tapered nozzles 13a and 13a' as shown in FIGS. 3 and 4, respectively. When Ni--Cu fine powder was manufactured, the particle size of the manufactured fine powder ranged from 200 to 600.
Å, and the average particle size was about 350 Å, both the variation in particle size and the average particle size were slightly larger than in the case of the above-mentioned operation, and the processing time was also about 20 minutes, resulting in a slight decrease in productivity.

Operation (3) In the same manner as in operation (1) above, 30 g of metallic aluminum (99.9% Al, balance impurities) was charged into the metal vapor chamber 5 of the crucible 2, and 30 g of metallic nickel (99.8% Ni) was charged into the metal vapor chamber 5 of the crucible 2. , remaining impurities) into the metal vapor chamber 5' of the crucible 2', and the metal fine powder manufacturing apparatus was operated under the following conditions to produce Al--Ni fine powder.

Temperature T ₁ : 1650℃ T ₁ ′: 2100℃ T ₂ : 900 to 1100℃ T ₂ ′: 1150 to 1400℃ Pressure P ₁ : 10Torr P ₁ ′: 10Torr P ₂ : 3 to 4Torr In this operation, all The time required to process metal aluminum and metal nickel was approximately 14 minutes, and the particle size range of the Al-Ni fine powder collected on the sorption plate was 200-400 Å, with an average particle size of 280 Å. It was hot.

Operation (4) Same operation as in operation (3) above except that the nozzles provided at the lower ends of conduits 12 and 12' are changed to tip nozzles 13a and 13a' as shown in FIGS. 3 and 4, respectively. When Al-Ni fine powder was produced under the following conditions, the particle size range of the Al-Ni fine powder collected on the sorption plate was 250 to 600 Å, and the average particle size was 300 Å.
Å, both the particle size variation and average particle size are larger than in operation (3) above, and the processing time is approximately
It took 16 minutes, which caused a slight decrease in productivity.

Embodiment 2 FIG. 2 is a schematic diagram similar to FIG. 1 showing another embodiment of the apparatus for producing fine alloy powder according to the present invention. In FIG. 2, parts that are substantially the same as those shown in FIG. 1 are designated by the same reference numerals.

In the apparatus for producing fine alloy powder according to this embodiment, an oil storage tank 21 is arranged in place of the sorption plate in the recovery zone 11, and the fine alloy powder is stored in the tank 21.
The apparatus is constructed in the same manner as the apparatus for producing fine alloy powder of Example 1 described above, except that the oil is collected in the oil 22 stored in the apparatus. In addition, when the amount of alloy fine powder produced is large, it is preferable that the tank 21 is forcedly cooled so that the temperature of the oil does not become excessively high.

Next, the operation of the apparatus for producing fine alloy powder constructed as described above will be explained with reference to an actual operation carried out to produce fine Ni--Cu powder.

Operation (5) First, the initial temperature in the oil storage tank 21 is 20℃,
Pour 500 c.c. of vacuum oil (Neopack MR-200 manufactured by Matsumura Sekiyu Co., Ltd.) 22, and then carry out the operation described above.
30g each of metallic copper and metallic nickel with the same composition as the metallic copper and metallic nickel used in (1) and (2)
Charge into the metal steam chambers 5 and 5' and operate as described above (1).
In the same manner as in the case of , the temperatures T ₁ and T ₁ ' in the metal vapor chambers 5 and 5' were set to about 1650°C and about 2000°C, respectively, and the pressures in the metal vapor chambers 5 and 5' were set to P ₁ and P ₁ . ′ and the pressure P ₂ in the recovery zone 11 are approximately 10 Torr, respectively.
Maintain at about 10 Torr, 1 to 2 Torr, wide end nozzle 13
By colliding and mixing the jets 14 and 14' ejected from and 13' with each other, and then colliding the mixed jet 16 with the liquid surface of the vacuum oil 22 to introduce the Ni--Cu fine powder into the vacuum oil, Ni--Cu fine powder was produced.

The time required to process all copper metal and nickel metal in this operation was approximately 17 minutes, and the particle size range of the produced Ni-Cu fine powder was 80 to 150 Å, with an average particle size of 100 Å, and the recovered Ni-Cu
It was observed that the agglomeration of the fine powder and the variation in particle size were lower than in Example 1 described above.

Operation (6) Same operation as in operation (5) above except that the nozzles provided at the lower ends of conduits 12 and 12' are changed to tip nozzles 13a and 13a' as shown in FIGS. 3 and 4, respectively. When Ni-Cu fine powder was manufactured under the following conditions, the particle size range of the manufactured Ni-Cu fine powder was 100 to 200 Å, and the average particle size was about 120 Å. Both operations mentioned above
It was larger than case (5), and the processing time was about 20 minutes, resulting in a slight decrease in productivity.

Operation (7) In the same manner as in operation (5) above, 30 g of metallic aluminum (99.9% Al, balance impurities) was charged into the metal vapor chamber 5 of the crucible 2, and 30 g of metallic nickel (99.8% Ni) was charged into the metal vapor chamber 5 of the crucible 2. , remaining impurities) into the metal vapor chamber 5' of the crucible 2', and the metal fine powder manufacturing apparatus was operated under the following conditions to produce Al--Ni fine powder.

Temperature T ₁ : 1650℃ T ₁ ′: 2100℃ T ₂ : 900 to 1100℃ T ₂ ′: 1150 to 1400℃ Pressure P ₁ : 10Torr P ₁ ′: 10Torr P ₂ : 3 to 4Torr In this operation, all The time required to process metal aluminum and metal nickel was about 14 minutes, and the particle size range of the Al-Ni fine powder recovered in vacuum oil was 100-150 Å, with an average particle size of 120 Å.
It was Å.

Operation (8) Same operation as in operation (7) above except that the nozzles provided at the lower ends of conduits 12 and 12' are changed to tapered nozzles 13a and 13a' as shown in FIGS. 3 and 4, respectively. When Al-Ni fine powder was produced under the following conditions, the particle size range of the Al-Ni fine powder recovered in vacuum oil was 100 to 200 Å, and the average particle size was about 150 Å, and there was no variation in particle size. Both the average particle diameter and the average particle size were larger than those in the above-mentioned operation (7), and the processing time was also about 16 minutes, resulting in a slight decrease in productivity.

Embodiment 3 FIG. 5 is a schematic diagram showing still another embodiment of the apparatus for producing fine alloy powder according to the present invention. In FIG. 5, parts that are substantially the same as those shown in FIG. 1 are designated by the same reference numerals.

This embodiment is suitable for producing fine powder of alloys whose constituent metals have high melting points, and the heat insulating materials 9 and 9' correspond to the heat insulating materials in the embodiments shown in FIGS. 1 and 2. have a box-shaped structure that covers the crucible 2 and the heater 7, and the crucible 2' and the heater 7', respectively. A water-cooled jacket 23 is provided inside the furnace shell 1 to cover the heat insulators 9 and 9', and cooling water is circulated and supplied to the water-cooled jacket so that the area around the heat insulator is forcibly cooled. It's summery. Further, a water-cooled pipe 24 is arranged around the part of the reactor shell 1 that defines the recovery zone 11, and cooling water is supplied into the water-cooled pipe so that the recovery zone 11 is forcibly cooled. It's summery.
This embodiment is otherwise constructed similarly to the embodiment described above.

In addition, in FIG. 5, the crucible 2' and the conduit 12,
Although the internal structure of 12' is not shown in detail,
These are constructed identically to the crucibles and conduits shown in FIGS. 1 and 2. Further, in FIG. 5, conduits 26 and 26' are connected to the gas introduction ports 3 and 3' at one end and have flow control valves 25 and 25' in the middle, and conduits 26 and 26' are connected to the other ends of the conduits 26 and 26'. The connected gas cylinders 27, 27', detection units 28, 28' for detecting the temperature and pressure in the metal vapor chambers 5 and 5', respectively, and the detection unit 29 for detecting the pressure in the recovery zone 11 are schematically shown. has been done.

Next, the operation of the apparatus for producing fine alloy powder constructed as described above will be described with reference to an actual operation carried out to produce fine Ni--Ti powder.

Operation (9) 30g of metallic titanium (99.8% Ti, balance impurities) and Operation (1) were prepared in the same manner as in Operation (1) above.
By charging 30g of the same nickel metal used in the process into the metal vapor chambers in the crucibles 2 and 2', and operating the alloy fine powder manufacturing equipment under the following conditions, Ni-Ti was produced. A fine powder was produced.

Temperature T ₁ : 2500℃ T ₁ ′: 2100℃ T ₂ : 1200 to 1600℃ T ₂ ′: 1000 to 11000℃ Pressure P ₁ : 15Torr P ₁ ′: 15Torr P ₂ : 3 to 4Torr In this operation, all The time required to process titanium metal and nickel metal was approximately 15 minutes, and the particle size range of the Ni-Ti fine powder collected on the sorption plate was 100-300 Å, with an average particle size of 180 Å. It was hot.

Operation (10) Connect the nozzles 13 and 13' to tapered nozzles 13a and 1 as shown in FIGS. 3 and 4, respectively.
3a' under the same conditions as the above operation (9).
-When producing Ti fine powder, the particle size range of the Ni-Ti fine powder collected on the sorption plate was 120 to 400 Å.
The average particle size was 200 Å, and both the variation in particle size and the average particle size were larger than in the case of operation (9) described above, and the processing time was about 17 minutes, resulting in a slight decrease in productivity.

Operation (11) The above operation (9) was carried out by replacing the sorption plate 15 with the same oil bath as in the embodiment shown in FIG. 2 (initial oil temperature 20°C, oil amount 500 c.c.). By operating the alloy fine powder production equipment under the same conditions as
Ni-Ti fine powder was produced.

The time required to process all titanium metal and nickel metal in this operation was approximately 15 minutes, and the particle size of the Ni-Ti fine powder recovered in the oil bath ranged from 60 to 120 Å, with an average The particle size was 80 Å, and it was observed that there was less agglomeration of the fine powder than in operations (9) and (10) above.

Operation (12) Ni-Ti was processed under the same conditions as operation (11) above by changing the wide-end nozzles 13 and 13' to tapered nozzles 13a and 13a' as shown in FIGS. 3 and 4, respectively. When the differential powder was produced, the particle size range of the Ni-Ti differential powder recovered in the oil bath was
The average particle size was 80 to 150 Å, and the average particle size was 100 Å. Both the particle size variation and the average particle size were larger than in the case of operation (11) described above. The processing time was also about 17 minutes, and the productivity was slightly lower. did.

Although the present invention has been described above in detail with reference to several embodiments, the present invention is not limited to these embodiments, and various embodiments are possible within the scope of the present invention. This will be clear to those skilled in the art. For example, each of the above-mentioned embodiments is configured to produce fine alloy powder in a batch manner, but in order to enable continuous operation of the apparatus for producing fine alloy powder of the present invention, the solid material in the metal vapor chamber is replaced with liquid raw material metal. may be configured to be charged intermittently or continuously.

[Brief explanation of the drawing]

1 and 2 are schematic configuration diagrams showing one embodiment of a fine alloy powder manufacturing apparatus according to the present invention, FIGS. 3 and 4 are longitudinal cross-sectional views showing a tapered nozzle, and FIG. FIG. 6 is a schematic diagram showing another embodiment of the apparatus for producing fine alloy powder according to the present invention, and FIG. 6 is a graph showing the relationship between vapor pressure and temperature of various metals. 1...furnace shell, 2,2'...crucible, 3,3'...
Gas introduction port, 4, 4'... Gas preheating chamber, 5,
5'...Metal steam chamber, 7, 7'...Heater, 8,
8'... Molten metal, 9... Insulating material, 10,10'...
...Bottom wall, 11...Collection zone, 12, 12'...
Conduit, 12a, 12a'... Outlet passage, 13, 1
3'... wide end nozzle, 13a, 13a... tapered nozzle, 14, 14'... jet stream, 15... sorption plate,
16...Mixed jet stream, 17...Alloy fine powder, 18
... Conduit, 19 ... Opening/closing valve, 20 ... Vacuum pump, 21 ... Oil storage tank, 22 ... Vacuum oil, 23 ... Water cooling jacket, 24 ... Water cooling pipe, 25, 25' ... Flow rate control valve , 26, 26'...
...Conduit, 27,27'...Gas cylinder, 28,2
8', 29...detection unit.

Claims (1)

[Scope of Claims] 1. A first metal vapor chamber that generates a first metal vapor therein, a first heating means that heats the first metal vapor chamber, and a first metal vapor chamber that heats the first metal vapor chamber. a first gas introduction means for introducing gas into the room; a first outlet passage means communicating with the first metal vapor chamber; and a second metal vapor chamber for generating a second metal vapor therein. a second heating means for heating the second metal vapor chamber; a second gas introduction means for introducing gas into the second metal vapor chamber; and a second gas introduction means communicating with the second metal vapor chamber. two outlet passage means; an alloy fines collection zone communicating with said first and second metal vapor chambers via said first and second outlet passage means, respectively; and said first and second outlet passages, respectively. first and second nozzles provided in the means for injecting the fluid in the first and second metal vapor chambers so that the jets mix with each other; and first and second nozzles provided in the alloy fine powder recovery zone for injecting the mixed jet. An apparatus for producing fine alloy powder, comprising: a fine alloy powder collection means for receiving and collecting fine alloy powder contained therein; and a pressure reducing means for reducing the pressure in the fine alloy powder collection zone. 2. The alloy fine powder manufacturing apparatus according to claim 1, wherein at least one of the first and second nozzles is a diverging nozzle. 3. The alloy fine powder manufacturing apparatus according to claim 1, wherein at least one of the first and second nozzles is a tapered nozzle. 4. A fine alloy powder manufacturing apparatus according to any one of claims 1 to 3, wherein the fine alloy powder collecting means is a forced cooling plate. 5. An apparatus for producing fine alloy powder according to any one of claims 1 to 3, wherein the fine alloy powder collecting means is a liquid bath.