JPH0434448B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method and apparatus for producing ultrafine particles in the form of arcuate or short chains.

(Prior art) Conventional ultrafine powder is produced by evaporation in gas, but the ultrafine particles adhere in the collection chamber and are collected into an agglomerated state. Since it is obtained as an aggregate of long chain-like ultrafine particles with a length of 1 μm or more, it is not easily dispersed or a high-density magnetic coating cannot be obtained when applied to a substrate as a magnetic recording material. This caused such inconvenience. An invention for solving the drawbacks of this conventional manufacturing method, a method and a device for producing erect ultrafine particles, is known in Japanese Patent Application Laid-Open No. 78635/1983.

(Problems to be Solved by the Invention) In view of the above, it is desirable to increase the productivity of ultrafine powder made of vertical ultrafine particles based on the above proposed invention. In addition, for example, arcuate ultrafine particles or short chain-like ultrafine particles are suitable for coating on substrates as magnetic recording materials, for example, about 5 to 10 ultrafine particles are connected and short particles with a length of about 0.15 to 0.3 μm are used. It is desirable that ultrafine powder consisting of an aggregate of chain ultrafine particles can be produced as needed.

(Means for Solving the Problems) The present invention provides a method for producing vertical ultrafine particles that satisfies the above-mentioned needs. A thin tube is provided at the tip facing the evaporation source in the generation chamber and whose rear end communicates with the high vacuum chamber, and the degree of vacuum in the vacuum chamber is made higher than the degree of vacuum in the generation chamber to generate a pressure difference. In a method for producing erect ultrafine particles in which the vapor in the generation chamber is drawn into the vacuum chamber through the thin tubes, the thin tubes are composed of a large number of tubes with air space between them. The lower end area of the capillary tube group is made larger than the area of the evaporation source, and the distance between the lower end of the capillary tube group and the evaporation source is configured to be adjustable, and the ultrafine particle vapor generated in the generation chamber is transferred through the capillary tube group to the evaporation source. It is characterized by being drawn into the vacuum chamber side.

The second invention provides a method for producing the above-mentioned short chain-shaped ultrafine particles, and includes an ultrafine particle generation chamber that generates ultrafine particle vapor generated by an evaporation method in a gas, and an evaporation source in the generation chamber that faces the ultrafine particle vapor. A large number of thin tubes each having an open tip and a rear end communicating with a high vacuum chamber are provided, and a magnetization device is provided around the outer periphery of the group of thin tubes, and the degree of vacuum in the vacuum chamber is higher than the degree of vacuum in the generation chamber. A pressure is generated, thereby drawing the vapor in the generation chamber into the vacuum chamber through the group of capillary tubes, and causing the ultrafine particles to pass through the magnetic field generated by the magnetization device in each capillary tube. It is characterized by what it did.

Furthermore, the third invention provides an apparatus for producing the above-mentioned vertical or short chain-shaped ultrafine particles, which includes an ultrafine particle generation chamber for generating ultrafine vapor produced by an in-gas evaporation method, and It consists of a large number of thin tubes each having an open tip facing the evaporation source and a rear end communicating with a high vacuum chamber, and a magnetization device provided on the outer periphery of the group of thin tubes, and is a part of the high vacuum chamber. is configured in an ultrafine particle surface treatment chamber.

(Example) Figures 1 and 2 show an example of the method and apparatus of the present invention. Reference numeral 1 indicates a generation chamber in which ultrafine particles are evaporated, and the generation chamber 1 has a gas introduction pipe 2 on its bottom wall, a crucible 4 containing an evaporation material 3 in the lower part thereof, and a dielectric heating on its outer periphery. The generation chamber 1 has a coil 5 and an exhaust port 6 connected to an external evacuation device on the edge wall of the generation chamber 1. According to the present invention, above the evaporation source, that is, the crucible 4, a plurality of thin tubes 7 extend vertically and parallel to each other at a required interval, and penetrate the upper end wall of the production chamber 1 in an airtight manner. A group of thin tubes 8 is provided. These thin tube groups 8 may be arranged in a bundle with the thin tubes 7 in contact with each other. They are placed side by side so that a desired gap 9 exists between them. The outer end of the group of capillary tubes 8 led out to the outside, that is, the outer end of each capillary tube 7, is in open communication with a high vacuum chamber 10 that is maintained at a higher vacuum level than the vacuum level of the production chamber 1, as described later. . The high vacuum chamber 10 is equipped with an evacuation pipe 11 connected to an external evacuation pump, and the interior of the high vacuum chamber 10 is maintained at a desired degree of vacuum via a control valve 12 interposed therein. The rear end side of the high vacuum chamber 10 is an ultrafine particle collection chamber 13. That is, a partition valve 14 is provided on a part of the upper wall of the high vacuum chamber 10 to freely partition the interior into two parts, and is movable forward and backward in the vertical direction. is defined as the collection chamber 13. At the lower end of the collection chamber 13,
Vacuum exhaust pipe 15 of the vacuum exhaust device connected to the atmosphere
is provided via the control valve 16. In the collection chamber 13, a dish-shaped collection container, a substrate, etc. may be stored in advance, if necessary. The end wall of the collection chamber 13 is configured as an airtight opening/closing door. In the drawing, 17 indicates a viewing window. The thin tube group 8 in the illustrated embodiment is formed into a bent thin tube group that is bent from the middle and extends horizontally so as to take up as little height space as possible. If necessary, the high vacuum chamber 10 is provided with an evaporation chamber 19 located below the horizontal thin tube group 8 and housing a heating evaporation device 18 for evaporation material for ultrafine particle coating. It can be configured as a surface treatment chamber.

The high vacuum chamber 10 also has a gas introduction pipe 20 for surface treatment of ultrafine particles of oxygen, nitrogen, etc. by gas phase reaction, etc., which is communicated with the high vacuum chamber 10, if necessary.
can be connected to form a surface treatment chamber for ultrafine particles. As shown in the figure, the surface treatment chamber can be configured with both an evaporation chamber 19 and a gas introduction pipe 20, or with only one of them (not shown).

In the drawing, there is a generation chamber 1 in the middle of the thin tube group 8.
These thin tube groups 8 are located above and on the outer periphery of
A jacket 21 is provided by enclosing the jacket in an air-liquid tight manner. A refrigerant or heat medium supply pipe 22 is connected to the lower part of the jacket 21, and a discharge pipe 23 thereof is connected to the upper part.

Furthermore, if necessary, a magnetization device 24 consisting of an annular magnetic field forming solenoid connected to an external DO power source is provided on the lower outer periphery of the thin tube group 8. The magnetization device 24 includes an arm member 2 fixed to the inner wall of the generation chamber 1.
5 and a flange 2 protruding from the outer periphery of the magnetizing device 24.
The height position can be adjusted by a height adjustment device 27 interposed between the height adjustment device 6 and the height adjustment device 27.

That is, the height adjustment device 27 is composed of an elastic member 27a such as a bellows or a spring, and an adjustment screw 27b, and when the screw 27b rotates, the solenoid 24
For example, set the height from the top of the crucible to 50 to 100 mm.
When the magnetizing device 24 is activated, the height position of the magnetic field generated within the thin tube group 8 can be set in advance. The jacket 21 is attached to the cylinder wall 2
1a and closing plates 21b, 21 at both ends of the cylinder wall 21a.
It consists of b. The closing plate 21b inserts each thin tube 7 of the thin tube group 8 at a predetermined position and fixes it by welding, closes the space between these thin tubes 7, and makes the internal space a circulation space for a cooling or heating medium such as water. Configure. Furthermore, the closing plate 21b has a flange portion 2 that protrudes outward from the cylindrical wall 21a of the jacket 21.
8, and a height adjustment device 29 similar to that described above was provided between this and the edge of the top wall of the generation chamber 1. The height adjustment device 29 for the thin tube consists of a telescopic member 29a and a screw 29b. As a result, the thin tube group 8
The height distance between the lower end and the evaporation source is, for example, 80 to 150 mm.
It can be adjusted within a range of In the drawing, the thin tube group 8 is arranged so that the outer periphery is approximately circular, and the outer peripheral diameter of the lower end surface is larger than the diameter of the opening that accommodates the evaporation material 3 of the crucible 4, for example, at least approximately twice as large. It is preferable to do so. In this way, the upward flow of vapor generated by heating the evaporative material 3 was sufficiently received at the lower surface of the large-diameter thin tube group 8. Furthermore, it is preferable that the lower end surface of the capillary tube group 8 be made into a concave surface with a high center as shown in the figure to prevent the evaporated ultrafine particles from escaping to the outside as much as possible. An evaporated ultrafine particle receiving wall 30 is provided on the upper wall of the generation chamber 1 so as to protrude from the outer periphery of the thin tube group 8, and a discharge port 31 is provided on the lower surface of the receiving wall 31. Excess evaporated ultrafine particles that are not sucked into the receiving wall 3
0 and from the exhaust port 31, the exhaust port 31
It was designed to be collected externally via a discharge pipe 32 connected to the .

The vacuum chamber side of this device is supported by upper and lower support arms 33 protruding from a fixed wall (not shown) via a telescoping device 34 such as a height adjustment device similar to the height adjustment device 29 described above. I made it.

Next, the operation of the above device of the present invention will be explained. When performing evaporation in gas by setting the high degree of vacuum in the production chamber 1 to, for example, 1×10 ^-4 Torr, the degree of vacuum in the high vacuum chamber 10 is set to a degree higher than the vacuum degree in the production chamber 1, for example, 5×.
Evacuate to 10 ^-2 torr. In this case, the vapor of the evaporated material, such as a metal or alloy material, evaporated from the crucible 4 reaches the lower surface of the group of large-diameter thin tubes 8 facing above, but each of the thin tubes 7 has a rear end that is high. Since it opens into the vacuum chamber 10, the high vacuum of the high vacuum chamber 10 produces a strong suction action in each of the capillary tubes 7, and the vapor (ultrafine particles) in the previous air is discharged from the lower end suction port of each capillary tube 7. It is sucked in and flows at a rapid speed (several tens of meters per second) together with the inert gas in the generation chamber 1, and is drawn into the high vacuum chamber 10.
In this way, the erect ultrafine particles are accumulated in the collection chamber 13. In this case, in the device of the present invention,
Since the evaporating ultrafine particles are collected by suction through a large number of thin tubes 7, mass production becomes possible. The particle size of the obtained arcuate ultrafine particles is determined by the conditions used in the normal gas evaporation method (molten temperature of the evaporation material, type of gas (molecular weight), degree of vacuum), as well as the lower end inlet of the capillary group 8 and the evaporation material. The distance can be changed within the range of 10 to 500 Å by appropriately changing the vertical movement of the thin tube group 8 or the vertical movement of the evaporation surface (not shown).

In the above operation, a coating material such as a synthetic resin is prepared as an evaporation material stored in a heating device 18 in an evaporation chamber 19 provided in advance in a high vacuum chamber 10, and is heated and evaporated. In such a case, the countless erect ultrafine particles discharged from the thin tube group 8 into the high vacuum chamber 10 are each coated with synthetic resin vapor to obtain an aggregate of erect ultrafine particles coated with synthetic resin. It will be done.

For example, in order to coat Cu instead of the synthetic resin described above, Ni
Preferably, the ultrafine particle stream is heated to 400-500°C. In this case, each thin tube 7 is heated by passing a heating medium such as heating oil into the jacket 21, and the Ni ultrafine particles passing through the tube are heated to 400 to 500°C and released into the high vacuum chamber 10. This is coated with Cu ultrafine particles evaporated from the evaporation source 18 to obtain an aggregate of Cu-coated Ni arcuate ultrafine particles.

In addition, when producing arcuate ultrafine particles in which the arcuate ultrafine metal particles discharged from the capillary tube group 8 are subjected to a gas phase reaction with oxygen, nitrogen, etc. to form a coating such as oxidation or nitridation on the surface, the gas introduction tube 20 is used. Introduce the desired gas such as oxygen or nitrogen. In this case, the desired reaction temperature is obtained by passing a heated medium to the required temperature through the jacket 21 mentioned above. The temperature of the ultrafine particles in each thin tube 7, which is normally conveyed by gas, is 200 to 300°C, but if a temperature lower than that is desired, for example, 100°C or less, a cooling medium such as cold water may be passed through the jacket 21. This is achieved by Tube group 8
Since it is composed of a large number of thin tubes 7 with an empty space, the ultrafine particles passing through each thin tube 7 are heated or cooled as described above. By heating, the ultrafine particles in the capillary tube 7 can be aggregated and coalesced to grow, and in the case of short chain-like ultrafine particles described below, the strength of the connections between the particles can be improved. Furthermore, the growth of ultrafine particles within the thin tube 7 can be suppressed by cooling.

When producing an aggregate of short-chain ultrafine particles using the above-mentioned apparatus, a DC current is passed through the magnetic field forming solenoid of the magnetization device 24, and a DC current is applied to the internal space of the magnetic field forming solenoid, that is, into each capillary tube 7 of the capillary group 8. Fe passes through each thin tube 7 at a high speed of 20 to 30 m/s, creating a state in which a magnetic field is formed in a predetermined length range,
After the temperature of the evaporated ultrafine particles of magnetic materials of transition metals such as Co and Ni or their alloys falls below the Curie point, they are magnetized while passing within the predetermined region of the magnetic field, and the individual particles are oriented. , for example, particles are connected in a range of about 5 to 10, and the length
Short chain-shaped ultrafine particles of 0.15 to 0.3 μm are formed and discharged from each capillary tube 7 into the high vacuum chamber 10, and an aggregate of short chain ultrafine particles, ie, powder, is obtained in the collection chamber 13.

In order to obtain the short chain-shaped ultrafine particles described above, the length (height) of the solenoid of the magnetization device 24, the pressure difference between the high vacuum chamber and the generation chamber, the degree of vacuum in the high vacuum chamber, and the magnetic field to be formed. Adjust the distance between the evaporation source and the evaporation source. In order to obtain surface-treated short chain ultrafine particles such as coating by vapor phase reaction or vapor deposition, the evaporation source 19 is
This is accomplished by using a gas inlet pipe 20 or the like.

FIG. 3 shows the high vacuum chamber 10 connected to the vacuum device via an intermediate exhaust conduit 36 separated by a perforated plate 35 between the upstream side of the high vacuum chamber 10, that is, the discharge end of the thin tube group 8; During operation, the vacuum level is between the vacuum levels of the generation chamber 1 and the high vacuum chamber 10, for example 1×.
Make sure that the exhaust pressure is reduced to about 10 ^-1 .

In such a case, the carrier gas discharged from each capillary tube 7 is discharged from this evacuation conduit 36. On the other hand, the arcuate or short chain ultrafine particles released from each thin tube 7 travel straight due to inertia and reach the perforated plate 35.
A large number of through holes 35 are provided in advance to face the thin tube 7.
a, enters the high vacuum chamber 10, and reduces or eliminates the influence of excessive carrier gas flowing into the high vacuum processing chamber 10, so that the coating process within the vacuum processing chamber 10 can be performed well. can do.

Although not shown, when coating the vertical or short chain ultrafine particles with one type of substance to increase the thickness of the coating, or when forming a laminated coating of two or more types of substances, Two or more similar surface treatment chambers having the above-mentioned evaporation chamber 19 and gas introduction pipe 20 are configured.

The erect ultrafine particles, short chain ultrafine particles, or aggregates of these surface-treated erect ultrafine particles or short chain ultrafine particles, that is, powder, accumulated in the collection chamber 13 as described above are collected. When taking out the raw material to the outside, after stopping operations such as heating and evaporating the raw material and evacuation, the operation of the evacuation device connected to the evacuation pipe 15 is stopped, and the atmosphere is drawn into the collection chamber 13 through the control valve 16. The high vacuum chamber 10 (including the collection chamber 13) is brought to atmospheric pressure, and the sample is taken out to the outside and collected in a desired container according to a conventional method.

In addition, if you continue driving without completely stopping,
The collection chamber 13 is partitioned by lowering the partition valve 14, and only the collection chamber 13 is brought to atmospheric pressure by the same operation as described above, while the heating is temporarily relayed so that the material in the crucible does not evaporate, or lower the heating temperature. After the powder has been taken out to the outside, the partition valve 14 is moved upward and backward, and the powder is heated to the evaporation temperature again.

Next, more detailed examples will be described.

Example 1 (Manufacture of arcuate ultrafine particles) 8.5 kg of electrolytic Ni shot was filled into a refractory crucible with an inner diameter of 150 mm provided inside a generation chamber, and the mixture was first placed in a high vacuum of 1 x 10 ^-4 Torr. After exhausting to
Introduce He gas. On the other hand, it is heated with 1KHz38KW of power supplied from a high frequency power source to melt the Ni in the crucible and maintain the molten metal temperature at 1800℃. He gas is supplied from the bottom of the generation chamber at a flow rate of 10/min, the vacuum level of the generation chamber is set to 2 Torr, and the evaporating Ni ultrafine particles (observed as black smoke) are transported. Above the crucible, a large number of thin tube groups were provided in advance at a distance of 130 mm from the upper end of the crucible, with the suction ports facing each other. The diameter of the circular outer periphery of the group of thin tubes is approximately 200 mm, and each of the thin tubes is
Consists of a circular copper tube with an inner diameter of 2 mm and a wall thickness of 0.5 mm.
The 150 tubes constitute a group of tubules. The thin tubes are arranged so that they are juxtaposed with a gap of 13 mm between them. One side, the high vacuum chamber is evacuated using an exhaust system that combines an oil rotary pump and a mechanical booster.
5 × 10 ^-2 Torr, and with a pressure difference between the vacuum level of the generation chamber and the vacuum level of 2 Torr, the smoke of Ni vapor rising from the lower end suction surface of the group of capillary tubes and He gas is inside each capillary tube. and then forcefully suck it into the high vacuum chamber at a high speed of 400 m/s.

In this way, the Ni ultrafine particles evaporated in the generation chamber and the countless standing ultrafine Ni particles released from the group of capillary tubes fly as they are and accumulate in the collection chamber. Alternatively, it adheres to the substrate surface and is collected. Obtained Ni
The average particle diameter of the erect ultrafine particles was 200 Å, and the half-width was 30 Å, showing a sharp particle size distribution.

The Ni ultrafine particle evaporation generation rate in the actual operation was 120g/
The production rate of Ni arcuate ultrafine particles obtained in the collection chamber was 49 g/hr. This is approximately 41% of the evaporation amount.
% indicates that it can be produced as vertical ultrafine particles.

Incidentally, ultrafine Ni particles with a particle size of 100 Å were obtained by carrying out the same procedure as above, with a distance of 100 mm from the lower end of the capillary group and the upper end of the crucible.

Example 2 (Manufacture of coated arc-shaped ultrafine particles) The initial stage of the crucible, Ni raw material, and production chamber were the same as in Example 1, and then He gas was introduced and the temperature was increased to 1.5
Toll. Power supply from high frequency power supply 1KHz
Heating with 32kw to melt the Ni in the crucible to 1750℃
Maintain the molten metal temperature. He gas is supplied from the bottom of the generation chamber at a flow rate of 0.6/min, and the Ni evaporated ultrafine particles are transported to a group of thin tubes fixed at a position 100 mm from the top of the crucible. The tubule group consists of 150 tubules,
Each tube has an inner diameter of 2 mm, a wall thickness of 0.5 mm, and a length of 200 mm. On the other hand, in the evaporation chamber installed in the high vacuum chamber, 100 g of polystyrene filled in an alumina crucible in advance is heated from the outside of the crucible with a nichrome wire heater and kept at a temperature of 250℃, and the high vacuum chamber is equipped with an oil diffusion pump. The vacuum pumping system is a combination of an oil rotary pump and a mechanical booster, and the vacuum is maintained at 1×10 ^-3 Torr, and 0.35 g/min of polystyrene is evaporated. A perforated plate is interposed between the high vacuum chamber and the introduction end of a group of thin tubes communicating therewith, and an intermediate exhaust chamber provided between the introduction end of the group of thin tubes and the perforated plate is connected to the oil evacuation chamber. The vacuum is maintained at 1×10 ^-1 Torr using an exhaust system that combines a rotary pump and a mechanical booster. Thus, due to the pressure difference between the high vacuum on the high vacuum chamber side and the low vacuum in the generation chamber, the vaporized Ni ultrafine particle smoke is sucked into the capillary group from the lower end suction port group of the capillary tube group together with the carrier gas, and the flow rate is 350 m/sec. is first drawn into the intermediate exhaust chamber at a high speed, and the carrier gas is removed by a screw, while the Ni ultrafine particle flow goes straight and is sucked into the high vacuum chamber through the holes in the perforated plate. At this time, the flying Ni arcuate ultrafine particles pass through the polyethylene vapor zone and are coded. In order to perform the coating process well, the arcuate ultrafine particles are released from the thin tube group into the intermediate exhaust chamber. While passing through the group of thin tubes before being heated, the He gas and the Ni arcuate ultrafine particles are cooled to below 100°C by cooling water flowing into the jacket around the outer periphery. Thus, film thickness 30-50 Å, average
A 40 Å polyethylene vapor deposited film is made of Ni with an average grain size of 100 Å.
A product whose surface is coated with vertical ultrafine particles is obtained in the collection chamber. A substrate may be set in advance in the collection chamber and the substrate may be adhered thereto. The Ni ultrafine particle evaporation generation rate in the actual operation was 82 g/h.
The production rate of polyethylene-coated Ni arcuate ultrafine particles obtained in the collection chamber was 7.2 g/hr (4.4 g/hr for Ni arcuate ultrafine particles only). This means that approximately 5.4% of the evaporated amount was produced as Ni arcuate ultrafine particles.

Example 3 (Production of short chain-shaped Fe-CO alloy ultrafine particles) In a fireproof crucible with an inner diameter of 150 mm in the generation chamber, 4.9 kg of electrolytic Fe and 3.6 kg of electrolytic Co were placed as evaporation materials, totaling 8.5 kg.
Kg is charged and first evacuated to a high vacuum of 1×10 ^-4 Torr, then He gas is introduced to a pressure of 2 Torr. Supply power from high frequency power supply 1KHz38Kw
Heating at 1800℃ to dissolve Fe and Co in the crucible,
Hold the molten Fe-Co alloy at ℃. The structure of the capillary group and the height distance between the capillary group and the crucible are the same as in Example 1. The vacuum inside the high vacuum chamber is maintained at 5×10 ^-2 Torr using an exhaust system that combines an oil rotary pump and a mechanical booster. The evaporated Fe-
The Co alloy vapor is sucked in through the suction port group at the lower end of the thin tube group, and in a state where the temperature of the ultrafine particles is lower than the Curie point, it passes through the magnetic field formed by the solenoid and is magnetized.
The upper half of the height of the solenoid (200mm) is magnetized, and the ultrafine particles pass through this zone at a high speed of 10m/sec.
Residence time in that zone is relatively short;
It was 0.02 seconds. As a result, 8 to 12 erect ultrafine particles are formed into short chain-like ultrafine particles, which are drawn into the high vacuum chamber together with the carrier gas through the tube group and accumulated in the collection chamber. . The average grain size of the aggregate of 60Fe−40Co vertical ultrafine particles produced is 200 Å, and its half-width is 30 Å.
It showed a sharp particle size distribution. Regarding the number of short chain particles, approximately 80% of the aggregates were within the range of 8 to 12 particles, and chains outside the range of 5 to 15 particles were hardly observed.

In the actual operation, the evaporation production rate of 60Fe-40Co ultrafine particles was 108 g/hr, and the collection rate of short chain ultrafine particles was 47 g/hr, and approximately 44% of the evaporation amount was produced as short chain ultrafine particles. . When applying conventional long chain-shaped ultrafine particles consisting of dozens of ultrafine particles to the tape base material in the production of magnetic recording tape, it is difficult to disperse and orient the particles, and the magnetic recording properties vary widely. However, the short chain-shaped ultrafine particles produced in this example solved the above-mentioned difficulties, and
Good magnetic recording characteristics were obtained. When the same procedure as described above was carried out with the distance between the lower end of the solenoid and the upper end of the crucible being 50 mm, short chain-shaped ultrafine particles having 5 to 10 pieces connected were obtained.

Example 4 (Production of short chain-shaped ultrafine particles with oxide film) Under the same conditions as in Example 3, oxygen was introduced into the high vacuum chamber from the gas introduction tube at a rate of 4×10 ^-3 /min to form a group of thin tubes. Short chain-like 60Fe released by
-40Co ultrafine particles were exposed to an oxygen gas atmosphere to produce a surface coated with oxide. In the short chain Fe ultrafine particles, an iron oxide (Fe ₃ O ₄ ) film with a thickness of 10 to 20 Å was uniformly formed on the surface of each Fe ultrafine particle.

The flow velocity of the arcuate or short chain ultrafine particles selected within the group of capillary tubes is adjusted to a desired high speed by adjusting the differential pressure and the degree of vacuum in the high vacuum chamber, and is, for example, 20 to 30 m/s. In the case of only the conventional evaporation method in gas, the hardness is generally 1 to 2 m/S.

(Effects of the Invention) According to the present invention, the degree of vacuum is higher than the degree of vacuum in the generation chamber in which the in-gas evaporation method is performed, and the ultrafine particle vapor generated in the generation chamber is caused by the differential pressure. A group of thin tubes consisting of a large number of thin tubes with air space between them, the lower end area of the thin tube group being larger than the area of the evaporation source, and the distance between the lower end of the thin tube group and the evaporation source being adjustable. Since it was designed to be drawn from the generation chamber to the vacuum chamber via the vacuum chamber and collected,
By heating or cooling the group of thin tubes with a medium flowing through the air, it is possible to control the growth of ultrafine particles, or to improve the connection strength of short chain-shaped ultrafine particles, and to control the amount of evaporation material. It is possible to obtain a large aggregate of erect ultrafine particles, and when the ultrafine particles are magnetized by a magnetization device while passing through the tube group at high speed, it is possible to collect short chain-shaped ultrafine particles. Furthermore, when a coating material evaporation device and/or a surface treatment chamber equipped with a gas introduction hole is provided on the high vacuum chamber side, the arcuate or short chain ultrafine particles emitted from the thin tube group can be coated. A surface-treated product can be obtained, and in this case, when passing the refrigerant or heating medium through the jiket provided on the outer periphery of the tube group, use a high-quality surface-treated arc or short chain superstructure at an appropriate temperature. Fine particles can be obtained.

[Brief explanation of drawings]

FIG. 1 is a partially cut-away side view of an apparatus according to an embodiment of the present invention, FIG. 2 is a cut-away sectional view taken along the - line, and FIG. 3 is a partially cut-away side view of a modified example. 1... Generation chamber, 7... Thin tube, 8... Thin tube group, 1
0... High vacuum chamber, 19... Evaporation chamber, 20... Gas introduction pipe.

Claims (1)

[Scope of Claims] 1. An ultrafine particle generation chamber that generates ultrafine particle vapor generated by an in-gas evaporation method, and a thin tube whose front end is open facing an evaporation source in the generation chamber and whose rear end communicates with a high vacuum chamber. , the degree of vacuum in the vacuum chamber is made higher than the degree of vacuum in the generation chamber to create a pressure difference, and thereby the vapor in the generation chamber is drawn into the vacuum chamber through the thin tube. In the manufacturing method, a large number of thin tubes are formed with holes between them,
The area of the lower end of the group of capillary tubes is made larger than the area of the evaporation source, and the distance between the lower end of the group of capillary tubes and the source of evaporation is adjustable, and the ultrafine particle vapor generated in the generation chamber is transmitted through the group of capillary tubes. A method for producing erect ultrafine particles, characterized in that the particles are drawn into the vacuum chamber. 2. An ultrafine particle generation chamber for generating ultrafine particle vapor generated by in-gas evaporation method, and a large number of thin tubes facing the evaporation source in the generation chamber, each having an open tip and a rear end communicating with a high vacuum chamber, On the outer periphery of the group of tubules,
A magnetization device is provided, and the degree of vacuum in the vacuum chamber is made higher than the degree of vacuum in the generation chamber to generate a pressure difference, thereby drawing the steam in the generation chamber into the vacuum chamber side through the group of capillary tubes. 1. A method for producing short chain-shaped ultrafine particles, characterized in that the ultrafine particles are passed through a magnetic field generated by a nuclear magnetization device in each capillary. 3. An ultrafine particle generation chamber that generates ultrafine vapor generated by in-gas evaporation method, and a large number of tubes each having an open tip and a rear end communicating with a high vacuum chamber, facing the evaporation source in the generation chamber. It consists of a thin tube and a magnetization device provided on the outer periphery of the thin tube group, and one of the high vacuum chambers.
An apparatus for manufacturing ultrafine particles in an arcuate or short chain shape, comprising an ultrafine particle surface treatment chamber. 4. The manufacturing apparatus according to claim 3, wherein the ultrafine particle surface treatment chamber is provided with an evaporation source for a coating material within the vacuum chamber. 5. The manufacturing apparatus according to claim 3, wherein the ultrafine particle surface treatment chamber is provided with a gas introduction pipe communicating with the vacuum chamber. 6. The manufacturing apparatus according to claim 3, wherein the lower end area of the thin tube group is larger than the area of the evaporation source. 7. An ultrafine particle generation chamber that generates ultrafine vapor generated by in-gas evaporation method, and a large number of tubes each having an open tip facing the evaporation source in the generation chamber and a rear end communicating with a high degree of vacuum. An arc structure consisting of a thin tube, a jacket enclosing the outer periphery of the thin tube group, and an annular magnetization device provided on the outer periphery of the thin tube group, and in which a part of the vacuum chamber is configured as an ultrafine particle surface treatment chamber. Or an apparatus for producing short chain-shaped ultrafine particles.