JPS62269743A - Method and device for producing isolated or short-chain ultra-fine particle - Google Patents

Abstract

PURPOSE:To efficiently produce isolated ultra-fine particles by providing many thin tubes with the front end opened to a vaporization source and the rear end communicat ing with a high-vacuum chamber in parallel in the chamber for forming the vapor of an ultra-fine particle by an in-gas vaporization method, and increasing the degree of vacuum in a vacuum chamber to a value higher than that in the formation chamber. CONSTITUTION:When vacuum vaporization is carried out in the formation chamber 1, evacuation is performed so that the degree of vacuum in the high-vacuum chamber 10 is made higher than that in the formation chamber 1. Consequently, the vapor of a material vaporized from a crucible 4 reaches the lower surface of a large-bore group 8 of thin tubes above the crucible, however, strong suction is generated in the thin tube 7, since the rear end of each thin tube 7 is opened to the high-vacuum cham ber 10. As a result, the vapor (ultra-fine particles) is sucked from the lower suction port, and rapidly drawn into the high-vacuum chamber 10 along with the inert gas in the formation chamber 1. The isolated ultra-fine particles are then accumulated in a collecting chamber 13 and collected. Since the vaporized ultra-fine particles are then sucked by the many thin tubes 7, mass production is made possible.

Description

Detailed Description of the Invention V. Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method and apparatus for producing isolated or short chain-shaped ultrafine particles.

(Prior art) Conventional production of ultrafine powder involves evaporation in gas. Since it is obtained as an aggregate of long chain-shaped ultrafine particles with a length of 50 pieces or more, when applied to a substrate as a magnetic recording material, it may not be easily dispersed or a high-density magnetic coating may be formed. I also worried about the inconvenience of not being able to get it. An invention for solving the drawbacks of this conventional manufacturing method is a method for producing isolated ultrafine particles, and a production apparatus is known in Japanese Patent Application Laid-open No. 71635/1983.

(Problems to be Solved by the Invention) In view of the above, it is desirable to increase the productivity of ultrafine powder made of isolated ultrafine particles based on the above proposed invention. or,
For example, isolated ultrafine particles or short chain-like ultrafine particles are ideal for coating on substrates as magnetic recording materials.
It is desirable that an ultrafine powder consisting of an aggregate of short-chain ultrafine particles of μ Torihodeka can be produced as needed.

Means for Solving Problem C) The present invention provides a method for producing isolated ultrafine particles that satisfies the above requirements, and includes an ultrafine particle generation chamber that generates ultrafine particle vapor by an in-gas evaporation method; A thin tube is provided with a tip opening facing the evaporation waste source in the generation chamber and a rear end communicating with a high vacuum chamber, and increasing the degree of vacuum in the vacuum chamber to generate a pressure difference. In this method for producing isolated ultrafine particles, the vapor in the generation chamber is drawn into the vacuum chamber through the capillary, and the method is composed of a large number of capillaries, and the particles are generated in the production chamber via a group of capillary tubes. It is characterized by making sure that ultrafine particle vapor is drawn into the vacuum chamber.

The 8g2 invention provides a method for producing the short chain-shaped ultrafine particles described above, 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 is opposite to the evaporation source. 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, so that the degree of vacuum in the vacuum chamber is higher than the degree of vacuum in the generation chamber. No pressure difference is generated, so that the vapor in the generation chamber is drawn into the vacuum chamber through the group of capillary tubes, and the ultrafine particles are passed through the magnetic field generated by the magnetization device in each capillary. It is characterized by a remembrance.

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

(Example) FIGS. 1 and 2 show an example of an apparatus for implementing the method of the present invention. +11 indicates a generation chamber in which ultrafine particles are evaporated and generated, and the generation chamber (1) has a gas introduction pipe (2+
having a crucible (4) containing an evaporation material (3) in its lower interior and a dielectric heating filter (5) around its outer periphery,
An exhaust port (6) connected to an external vacuum evacuation device is provided on the edge wall of the generation chamber +11.

According to the present invention, a plurality of thin tubes (7) extend vertically and parallel to each other at a required interval above the evaporation source, that is, the crucible (4), and the upper end of the production chamber (1) A group of thin tubes (8) is provided which hermetically penetrates the wall. These thin tube groups (8) may be arranged in a bundle with the thin tubes (7) in contact with each other, but as shown in the figure and as described below, each thin tube (7) is cooled or heated by a cooling or heating medium. They can be placed side by side with a desired gap (9) between them so as to receive each of 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 located in a high vacuum chamber al maintained at a higher vacuum level than the vacuum level of the production chamber (1), as described later. The opening communicates with the The high vacuum chamber α is a vacuum exhaust pipe α connected to an external vacuum pump.
The high vacuum chamber aQ is maintained at a required degree of vacuum through a control valve 13 which is provided with a pressure υ and a control valve 13 interposed between the valves υ and υ. The end side of the high vacuum chamber (1G) is an ultrafine particle collection chamber α3. That is,
A partition valve α4 that can freely partition the interior into two is provided in a part of the earthen wall of the high vacuum chamber (1 (I) so as to be movable forward and backward in the vertical direction, and a space on the end side of the high vacuum chamber a1 is provided. The inside is designated as the collection chamber αJ.

The lower end KFi of the collection chamber (13) is provided with an evacuation pipe α9 of the evacuation device connected to the atmosphere via a control valve U.Inside the collection chamber 0, a dish-shaped collection container or a substrate is installed as necessary. etc. may be accommodated in advance.The end wall of the collection chamber αl is configured as an airtight closing/opening door.

α in the drawing? ) indicates a viewing window. The group of capillary tubes (8) in the illustrated embodiment is arranged so as to occupy as little height space as possible.
It was constructed into a group of bent thin tubes that bend from the middle and extend horizontally. The high vacuum chamber αlFi, if necessary, has an evaporation chamber 0 located below the horizontal thin tube group (7) and housing a heating evaporation device α♂ for evaporation material for ultrafine particle footing.
The surface treatment chamber for ultrafine particles can be constructed by providing the following.

In addition, if necessary, the high vacuum chamber α1 can be connected with a gas inlet pipe (2) for surface treatment of the surface of ultrafine particles such as oxygen and nitrogen by gas phase reaction, etc., which communicates with the high vacuum chamber α1. It can be configured in a processing chamber. As shown in the figure, both the evaporation chamber 0 and the gas introduction pipe (■) are provided, or although not shown,
A surface treatment chamber can be configured with only one of them.

In the drawing, there is a generation chamber (1) in the middle of the tubule group (8).
A jacket Qυ is provided on the outer periphery of the capillary tube group (8) so as to enclose the tube group (8) in an air-liquid tight manner.

A refrigerant or heat medium supply pipe @ is connected to the lower part of the Jiken Qυ, and a discharge pipe thereof is connected to the upper part thereof.

Furthermore, if necessary, a magnetization device (c) 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 magnetized bag fiff: 12
4 is the height of the lIm device (with moisture) interposed between the arm member (c) fixed on the inner wall of the generation chamber (1) and the 7 langes (2) protruding from the outer periphery of the magnetization device (24). The height position can be adjusted.

That is, the height adjustment device @ consists of an elastic member (27a) such as a bellows or a spring, and an adjustment screw (27b), and the height of the solenoid (2IO from the upper end of the crucible) is adjusted by rotating the screw (27b). The position can be adjusted, for example, from 50 to 100 degrees, and the height position of the magnetic field generated in one tube group (7) when the magnetizer C is activated can be set in advance.The jacket Qυ is set on the cylinder wall ( 21a) and the cylinder wall (21a)
It consists of a closing plate (2l b) and (21b) at both ends. The closing plate (2l b) inserts each capillary tube (7) of the capillary group (8) at a predetermined position and fixes it by welding, and closes the space between these capillary tubes (7) to keep the internal space free of water, etc. The cooling or heating medium is arranged in the circulation space of the cooling or heating medium. Furthermore, the closing plate (2l b) is provided with a 7-rung part (2) that protrudes outward from the cylindrical wall (21 m) of the jacket υ, and this and the production chamber [
A height adjustment device similar to that described above was provided between the top wall and the mouth edge of No. 11. The height adjustment bag #4 for the thin tube consists of a telescopic member (29a) and a screw (29b). This makes it possible to adjust the height distance between the lower end of the thin tube group (8) and the evaporation source (3) within a range of, for example, 80 to 150 tin.

In the drawing, the thin tube group (8) is arranged so that the outer circumference is approximately circular, and the outer circumference diameter of the lower end surface is equal to the evaporation material (2) of the crucible (3).
), and preferably has a diameter larger than the nominal diameter, for example, preferably at least approximately twice the diameter. In this way, the upward flow of steam generated by heating the evaporative material (2) is sufficiently received by 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. On the upper wall of the generation chamber (1), there is a group of capillary tubes (8) outside r! A protruding evaporated ultrafine particle receiving wall ■ is provided at the RK position, and an outlet Gυ is provided at the lower surface of the receiving wall ω, so that the excess evaporated ultrafine particles that are not sucked into the thin tube group (7) are The exhaust pipe G connected to the exhaust port C311 is received by the receiving wall (to) of the exhaust port (from 3υ).
3 to be collected externally.

The vacuum chamber side of this device is provided with a telescopic device (such as a height adjustment device similar to 2! ).

Next, the operation of the above device of the present invention will be explained.

When performing evaporation in gas with the degree of vacuum in the production chamber (1) set to, for example, 1×10, the degree of vacuum in the high vacuum chamber (1
10-") - vacuum evacuation. When doing so, the vaporized material evaporated from the crucible (4), such as the vapor of metal or alloy material, is transferred to the lower surface of the large-diameter thin tube group (8) attached above. However, each of the thin tubes (71K) has its rear end open to the high vacuum chamber (1), so the high vacuum of the high vacuum chamber (IG) exerts a strong suction action inside each of the thin tubes (7). The vapor (ultrafine particles) in the previous air is sucked in from the lower end suction port of each thin tube (7) and flows at a rapid rate (several tens of meters per second) together with the inert gas in the generation chamber (1). The particles are drawn into the high vacuum chamber uI.In this way, isolated ultrafine particles are accumulated in the collection chamber a3.

In this case, in the apparatus of the present invention, the evaporating ultrafine particles are collected by suction through a large number of thin tubes (7), so that mass production is possible. The particle size of the isolated ultrafine particles obtained depends on the conditions of the usual gas evaporation method (molten temperature of the evaporation material, type of gas (
(molecular weight), degree of vacuum), and by appropriately changing the distance between the lower end inlet of the capillary group (8) and the evaporation material by the vertical movement of the capillary group (8) or the vertical movement of the evaporation surface (not shown).
It can be varied in the range of 10-500A.

In the above operation, a coating material such as a synthetic resin is prepared as an evaporation material stored in a heating device aB in an evaporation chamber α3 provided in advance in a high vacuum chamber α1, and is heated and evaporated. In such a case, the countless isolated ultrafine particles discharged from the thin tube group (8) into the high vacuum chamber αQ are each coated with synthetic resin vapor to obtain an aggregate of isolated ultrafine particles coated with synthetic resin. It will be done.

In order to coat Ou instead of the above-mentioned synthetic resin, for example, it is preferable to heat the M1 ultrafine particle flow passing through each capillary tube (7) of the capillary group (8) to 400 to 500° C. in advance. In this case, each thin tube (7) is heated by passing a heating medium such as heating oil into the jacket (21), and the N1 ultrafine particles passing through the tube are heated to 400 to 400 to s o 'c and placed in a high vacuum. chamber (released into the IG, to this,
By coating the Ou ultrafine particles evaporated from the evaporation source αa, an aggregate of O-enclosed M1 isolated ultrafine particles is obtained.

In addition, oxygen,
When producing isolated ultrafine particles by performing a gas phase reaction with nitrogen or the like to form a coating such as oxidation or nitridation on the surface, a desired gas such as oxygen or nitrogen is introduced from the gas introduction pipe (2).

In this case, the desired reaction temperature is 12υ
It is obtained by passing a medium heated to the required temperature. The ultrafine particles in each capillary (7), usually transported by gas, are 20
0 to sOO°C, but if a lower temperature is desired, e.g. 100°C or less, this can be achieved by passing a cooling medium such as cold water through the jacket Qυ. When manufacturing an assembly of Create a state in which a magnetic field is formed in the range, and apply 20~
IF @ passing at high speed of S Oys / 3, 00.
The evaporated ultrafine particles of magnetic materials of transition metals such as Ni or alloys thereof are magnetized while passing within the predetermined region of the magnetic field after the temperature drops below the Curie point,
Individual particles are oriented and, for example, about 5 to 10 particles are connected to form short chain-like ultrafine particles with a length of α15 to α3 μm, which are transported from each capillary (7) to a high vacuum chamber α [
An aggregate of short chain ultrafine particles, that is, powder, is obtained in the collection chamber αJ.

K to obtain the above-mentioned short chain-shaped ultrafine particles depends on the length and height of the solenoid of the magnetization device, 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. Measure the distance to 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 σ
This can be achieved by using 1 or gas introduction pipe 2.

Figure 3 shows that an intermediate exhaust chamber AGE may be provided on the upstream side of the high vacuum chamber QG, which is separated by a perforated plate (toward) from the outlet end of the thin tube group (8). . The intermediate evacuation chamber σC1 is connected to a vacuum device via an evacuation conduit (to), and during operation, the intermediate evacuation chamber σC1 is at a vacuum degree intermediate between the respective vacuum degrees of the production chamber (1) and the high vacuum chamber a. For example, the exhaust pressure is reduced to about 1×10 5 .

In such a case, the carrier gas discharged from each thin tube (7) is discharged from this evacuation conduit (to). One side,
Isolated or short-chain ultrafine particles released from each capillary (7) move straight due to inertia and pass through a large number of through holes (35 &) previously provided opposite to the capillary (71) of the perforated plate (end). The influence of excessive carrier gas flowing into the high vacuum processing chamber C10 into the high vacuum processing chamber C10 is reduced or completely eliminated, and coating processing within the vacuum processing chamber Ql can be performed satisfactorily. .

Note that when coating isolated 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, the above-mentioned method (not shown) may be used. Configure two or more similar surface treatment chambers with evaporation chamber canopies and gas introduction pipes.

The isolated ultrafine particles, short chain ultrafine particles accumulated in the collection chamber α3 as described above, or aggregates of these surface-treated isolated ultrafine particles or short chain ultrafine particles, that is, powder, are removed to the outside. When taking out the raw material, heat evaporation of the raw material, main exhaust, etc. are stopped, and then the operation of the vacuum exhaust system connected to the vacuum exhaust pipe α is stopped, and the atmosphere is introduced into the collection chamber α3 through the control valve net. high vacuum chamber αl (collection chamber α3
) to atmospheric pressure, and take it out to the outside and collect it in the desired container according to the usual method.

In addition, when the operation is continued without completely stopping, the partition pulp α4 is moved downward to partition the collection chamber (13), and only the collection chamber a3 is brought to atmospheric pressure in the same manner as described above. Temporarily interrupt the heating or lower the heating temperature so that the material in the crucible does not evaporate. After the powder is taken out to the outside, move the partition pulp (14J up and back) and heat it again to the evaporation temperature.

Next, more detailed examples will be described.

Example 1 (Manufacture of isolated ultrafine particles) A refractory crucible with an inner diameter of 150 as provided inside a generation chamber was filled with shot-shaped electrolytic N1 to a size of 5 mm, and first, 1X
10 After evacuating to a high vacuum of 2 torr, introduce 2 torr of H gas. Combined power IKH from one-way high frequency power supply,
Heating with 38KW, melting Ni in the crucible, 1B, 0
Maintain a melt temperature of 0°C. He gas is supplied from the bottom of the generation chamber at a flow rate of 11017 W, the degree of vacuum in the generation chamber is set to 2 Torr, and the evaporating N1 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 1,301,111 m from the upper end of the crucible, facing above the suction port. The diameter of the circular outer periphery of the thin tube group is approximately 20 Gas, and each of the thin tubes is made of copper circular thin tubes with an inner diameter of 2 mm and a wall thickness of 115 mm, and 150 of them constitute the thin tube group. The thin tubes are arranged side by side with a gap pitch of 150 between them. One side, the high vacuum chamber is evacuated using an exhaust system that combines an oil rotary pump and a mechanical booster.
x 10 torr, and by creating a pressure difference between the vacuum level of the generation chamber and the vacuum level of 2 torr, the N1 vapor smoke rising from below from the lower end suction surface of the capillary group was sucked into each capillary along with He gas. It is vigorously sucked into the high vacuum chamber at a high speed of 4001 seconds.

In this way, the N1 ultrafine particles evaporated in the generation chamber are rapidly drawn into the high vacuum chamber through the capillary group, and the countless isolated N1 ultrafine particles released from the capillary group are collected by their t-flight. Accumulate indoors.

Alternatively, it may be deposited on the substrate surface and collected. Obtained N
The average particle size of 1 isolated ultrafine particles was 200A, and its half width showed a sharp particle size distribution of 30 people.

The N1 ultrafine particle evaporation generation rate in the actual operation was 1209/h.
The production rate of isolated ultrafine particles of N1 obtained in the collection chamber was Fi49 g/hr. This is approximately 41% of the amount of evaporation.
We show that nanoparticles can be produced as isolated ultrafine particles.

In addition, the distance is 100- from the lower end of the tube group and the upper end of the crucible,
It was carried out in the same manner as above, and N1 ultrafine particles with a dead particle size of 100A were obtained.

Example 2 (Production of Coated Isolated Ultrafine Particles) The initial conditions in the crucible, N1 raw material, and production chamber are the same as in Example 1, and then H gas is introduced and 1.5 Torr is introduced.

Heated with IKH, 32Kw power supplied from a high frequency power supply,
The N1 in the crucible is melted and the temperature of the molten metal is maintained at 1750"C. H gas (L 61/
It is supplied at a flow rate of HR, and the Ni evaporated ultrafine particles are transported to a group of thin tubes fixed at a position 100M from the upper end of the crucible. The tubule group consists of 15 tubules, each of which has an inner diameter of 21111°, a wall thickness of α5, and a length of 200 fins. On the other hand, an alumina crucible was filled in advance in the evaporation chamber installed in the high vacuum chamber.
00g of polystyrene was heated with a Kalanichrome wire heater outside the crucible and maintained at a temperature of 250'C, and the high vacuum chamber was evacuated using a vacuum pumping system that combined an oil diffusion pump, an oil rotary pump, and a mechanical booster. - to carry out the evaporation of Zarystidine A, 3597m.

1 between the high vacuum chamber and the introduction end of the group of thin tubes communicating therewith.
An intermediate exhaust chamber provided between the introduction end of the thin tube group and the perforated plate was connected to this via a perforated plate, and evacuated using a thorough evacuation system using a combination of a live rotary pump and a mechanical booster.
) - hold in the field. Thus, due to the differential pressure between the high vacuum on the high vacuum chamber side and the low vacuum in the generation chamber, the vaporized N1 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 seams. The M1 ultrafine particle stream is first drawn into the intermediate exhaust chamber at a high speed of 1, and the carrier gas is removed by the drum, while the M1 ultrafine particle flow goes straight and is drawn into the high vacuum chamber through the holes in the perforated plate. . At this time, the flight N1 isolated ultrafine particles pass through the polyethylene vapor zone and are coated with the polyethylene vapor zone.In order to perform the coating process on the vehicle, the isolated ultrafine particles are discharged from the thin tube group to the intermediate exhaust chamber. While passing through the group of thin tubes before the He gas and N1 isolated ultrafine particles are cooled to below 100°C by cooling water flowing through the outer jacket.

A product in which the surface of N1 isolated ultrafine particles having an average particle size of IQOA is coated with a lithidine vapor-deposited film is obtained in the collection chamber. A substrate may be set in advance in the collection chamber and adhered thereto. The ML ultrafine particle evaporation generation rate in this operation was 829/h, and the generation rate of the obtained polyethylene-coated N1 isolated ultrafine particles in the collection chamber was 7.29/hr.
(Fe44 g/hr for only 14 isolated ultrafine particles). This is about the amount of evaporation! ;', 5c'x means that it was produced as N1 isolated ultrafine particles.

Example 3 (Production of short chain-shaped Fe-0o alloy isolated ultrafine particles) Electrolytic Fe49 J and electrolytic Oo56 a were placed in a refractory crucible with an inner diameter of 150 III m in the generation chamber as evaporation materials.
sIKg +-y-di, first lX10 )-/I/
After evacuating to a high vacuum, 2 torr of He gas was introduced. Heating with M138Kw using power supplied from a high frequency power supply 1 melts Fe and ao in the crucible, and heats the crucible to 1800°C.
Holds the e-Oo alloy molten metal. 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 high vacuum chamber is maintained at a vacuum level of 5×10″ffi torr by an exhaust system that combines an oil rotary pump and a mechanical booster. The evaporated 1.-Oo alloy vapor is sucked in through the suction port group at the lower end of the thin tube group, but in the next state when the temperature of the ultrafine particles becomes lower than the Curie point, it passes through the magnetic field formed by the solenoid and becomes magnetized. In this example, the length region (200ms) of the upper half of the solenoid height (
zone), and the ultrafine particles are magnetized at 10
Since it passes through this zone at a high speed of s/saw, the residence time in that zone is relatively short (102 seconds).

As a result, 8 to 12 isolated ultrafine particles are formed into short chain-shaped ultrafine particles, which are then drawn into the high vacuum chamber together with the carrier gas through the tube group and accumulated in the collection chamber. .

The average particle diameter of the generated aggregate of isolated ultrafine particles of 601/-400o was 200A, and the half width was 30A, showing a sharp particle size distribution. The number of particles in the short chain is in the range of 8 to 12 in about 80% of the aggregates, and in the range of 5 to 12.
Chains outside the range of 15 were hardly seen and 9.

In the actual operation, the evaporation production rate of Oo ultrafine particles was 108/hr, and the collection rate of short chain ultrafine particles was 479/hr, and approximately 44% of the evaporation amount was short chain ultrafine particles. was able to be manufactured. When conventional long chain-shaped ultrafine particles made of dozens of ultrafine particles are applied to the tape base material in the production of magnetic recording tape, it is difficult to disperse and orient the particles, resulting in many variations in magnetic recording properties. However, the short chain-shaped ultrafine particles produced in this example solved the above-mentioned problems and provided good magnetic recording properties. In fact, when the distance between the lower end of the solenoid and the upper end of the crucible was set to 504, and the procedure was carried out in the same manner as described above, 5 to 10 short chain-shaped ultrafine particles were obtained.

Example 4 (Production of short chain-shaped ultrafine particles with W1 coating) Under the same conditions as in Example 3, oxygen was introduced into the high vacuum chamber from the gas introduction tube in one layer of 4 x 10, and from the thin tube group. The released short chain-shaped 607e-400o ultrafine particles were exposed to an oxygen gas atmosphere to produce an oxide coating on the surface. For short chain ultrafine particles, a film of iron oxide (70304) with a thickness of 10 to 201 is uniformly formed on the surface of each 70 ultrafine particle.

The flow rate of the isolated or short-chain ultrafine particles transported 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%/S. In the case of conventional evaporation only in gas, the hardness is generally 1 to 211 B/S.

(Effects of the Invention) According to the present invention, the degree of vacuum in the generation chamber for performing evaporation in gas is greater than the degree of vacuum in the high vacuum chamber, and the generated ultrafine particle vapor is generated in the υ generation chamber due to the differential pressure. Since the collection is carried out by suction into the high vacuum chamber through a group of thin tubes, it is possible to obtain aggregates of isolated ultrafine particles at a large proportion to the amount of evaporated material. When ultrafine particles are magnetized by a magnetization device while passing through the tube group at high speed, short chain-shaped ultrafine particles can be collected, and furthermore, a coating material evaporation device or / When a surface treatment chamber is provided with gas introduction holes, isolated or short-chain ultrafine particles emitted from the tube group can be subjected to footing treatment, and a surface-treated product can be obtained. When a refrigerant or a heating medium is passed through a wicket provided in the wick, it is possible to obtain high-quality surface-treated isolated or short chain-shaped isolated ultrafine particles at an appropriate temperature.

[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 partially cut-away side view, and FIG. 3 is a partially cut-away side view of a modified example. +1)... Generation chamber (7)... Thin tube (8
)...tubule group rlal...high vacuum chamber 0
...Evaporation chamber ■...Gas introduction pipe patent applicant: 2 people from outside the New Technology Development Corporation

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. established,
In a method for producing isolated ultrafine particles, the degree of vacuum in the vacuum chamber is increased to create a pressure difference, thereby drawing vapor in the production chamber into the vacuum chamber through the thin tube. . A method for producing isolated ultrafine particles, comprising a plurality of thin tubes, and the ultrafine particle vapor generated in the generation chamber is drawn into the vacuum chamber through the group of thin tubes. 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, A magnetization device is provided around the outer periphery of the group of capillary tubes, and 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, thereby causing the vapor in the generation chamber to flow through the group of tubes into the vacuum. 1. A method for producing short chain-shaped ultrafine particles, characterized in that the ultrafine particles are drawn into a chamber and are caused to pass through a magnetic field generated by the 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. An apparatus for producing isolated or short chain ultrafine particles, which comprises a thin tube and a magnetization device provided on the outer periphery of the group of thin tubes, and a part of the high vacuum chamber is configured as 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 facing the evaporation source in the generation chamber, each having an open front end and a rear end communicating with a high vacuum chamber. a thin tube; a jacket covering the outer periphery of the thin tube group;
An apparatus for producing isolated or short chain-shaped ultrafine particles, which comprises an annular magnetization device provided around the outer periphery of the group of thin tubes, and a part of the vacuum chamber is configured as an ultrafine particle surface treatment chamber.