JP5436198B2 - Fine particle forming apparatus and method thereof - Google Patents

Description

  The present invention relates to a fine particle forming apparatus and a method for attaching nano fine particles to a carrier.

In recent years, catalysts for exhaust gas have become more advanced, and are made to be nanosize of binary and ternary alloys such as rhodium and palladium based on platinum and are attached to a carrier such as alumina powder.
The loading of these catalytic metals is currently carried out mainly by a wet process, and this method has a problem that when a nanoparticle catalyst is used for a long period of time, it tends to aggregate due to heating, resulting in poor performance.
In the wet process, considering the inferiority, a large amount of catalyst is supported in the initial stage, the precious metals are soaring and the resources are scarce, and this is a bigger problem than the number of cars in the future.
In this regard, dry support, in which nanoparticles are deposited in a vacuum using a recently developed coaxial vacuum arc deposition source, is excellent in adhesion, and thus hardly changes over time. In this method, a single metal such as platinum, rhodium or palladium or a target of an alloy thereof is used, and these metal materials are converted into plasma by a vacuum arc (Patent Documents 1 and 2 below) to support atomic powder such as alumina. It is sprayed onto the body and carries nanoparticles of platinum, rhodium, palladium, etc., or alloys thereof on powder such as aluminum.
Also in the photocatalyst, improvement of the photocatalytic effect is recognized only by supporting 0.3% to 1% of nanoparticles such as gold or platinum as a cocatalyst on titania powder for photocatalyst, and various kinds of nanoparticles are supported on the photocatalyst. The production method of supporting the powder in a vacuum in the future may be changed from a conventional wet process in a specific field.

  A conventional fine particle forming apparatus irradiates a catalyst metal plasma generated from above using a vacuum arc plasma generator while stirring a carrier such as alumina powder stored in a cylindrical container in a vacuum. The catalyst metal is supported on the catalyst.

JP 2007-204810 A JP 2007-254762 A

However, in the conventional fine particle forming apparatus, when the stirring vessel is continuously rotated in the vacuum by the conventional stirring method, the titania powder is aggregated as shown in the example in which gold is supported on the titania powder shown in FIG. As the container rotates, it grows in the shape of a snowman, and the gold nanoparticles adhere only to the surface of the dama and degrade the performance of the titania powder carrying the catalyst metal.
This is because the gold nanoparticles attached to the surface of the titania powder act as an adhesive, and the nanoparticles in the vacuum easily adhere to each other even with a weak mechanical pressure. Once a small dama is formed, the dama that rolls with the movement of the rotating container grows into a big dama by sprinkling titania powder like a snowball. In such a dama, gold particles adhere only to the dama surface and hardly adhere to the titania powder inside.

  The present invention has been made in view of such circumstances, and an object of the present invention is to provide a fine particle forming apparatus and a method for attaching a vapor deposition material without forming a lump on the surface of the vapor deposition target. It is to be.

In order to solve the above-mentioned problems of the prior art and achieve the above-described object, the fine particle forming apparatus of the present invention is a vapor deposition source that flies a vapor deposition material, and is opposed to the vapor deposition source, and is a deposition target. A container for containing a powder carrier, a stirring means for stirring the powder carrier in the container, and a stamp head for crushing the lump of the powder carrier generated in the stirring process by the stirring means A first operation for causing the stamp head to collide with the bottom surface of the container, a second operation for holding the stamp head in contact with the bottom surface, and a third operation for separating the stamp head from the bottom surface are sequentially repeated. A circular edge portion of the upper open portion of the container becomes a slope inclined in a direction in which the central axis of the container extends, and has a step at a predetermined position, and the pulverizing means has the bottom surface While being urged towards An arm portion that contacts an edge portion, and when the arm portion falls toward the bottom surface at the step, the stamp head is brought into contact with the bottom surface, and the arm portion is in a predetermined position along the slope. When reached, the stamp head is moved away from the bottom surface.

In the fine particle formation method of the present invention, the vapor deposition material flying from the vapor deposition source is supported on the vapor deposition target while stirring the powdery carrier that is the vapor deposition target in a container disposed opposite to the vapor deposition source. In the fine particle forming method, in the process of stirring the powder carrier in the container, the bottom of the container is beaten with a pulverizing means, and the lump of the powder carrier generated by the stirring is crushed, The rotational speed of the container is increased as the amount of the vapor deposition material deposited on the powder carrier increases.

  ADVANTAGE OF THE INVENTION According to this invention, the fine particle formation apparatus which can adhere a vapor deposition material, without forming a dama on the surface of a to-be-deposited body, and its method can be provided.

FIG. 1 is a schematic view of a fine particle forming apparatus according to an embodiment of the present invention. FIG. 2 is a view for explaining the function of the scraper of the fine particle forming apparatus shown in FIG. FIG. 3 is a diagram for explaining a TEM observation image showing a state on the titania surface when gold is deposited on the titania powder. FIG. 4 is a view for explaining a scraper and a stamp of the fine particle forming apparatus shown in FIG. FIG. 5 is an external view of the stirring container of the fine particle forming apparatus shown in FIG. FIG. 6 is a diagram for explaining a part of the structure of the stamp shown in FIG. FIG. 7 is a diagram for explaining the change in the distance between the stamp according to the embodiment of the present invention and the bottom surface of the stirring vessel in time series. FIG. 8 is a partial cross-sectional view of the stamp shown in FIG. FIG. 9 is an external view of the stirring container as viewed from above. FIG. 10 is an external view of a dama generated in the stirring process. FIG. 11 is an external view of a dama generated in the stirring process. FIG. 12 is a diagram of a state where a dama is crushed by the stamp head according to the embodiment of the present invention. FIG. 13 is a view for explaining the result of grinding the powder before and after stirring with gold supported on titania powder by the fine particle forming apparatus of the embodiment of the present invention.

Hereinafter, a fine particle forming apparatus according to an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is a schematic view of a fine particle forming apparatus 1 using a coaxial vacuum arc vapor deposition source 5.
The fine particle forming apparatus 1 shown in FIG. 1 uses, for example, a vacuum arc plasma generator 3 while stirring alumina powder (deposited body 7) that is a carrier housed in a stirring container 73 that is a cylindrical container in a vacuum. Then, the ionized plasma, which is the catalytic metal generated in this way, is irradiated from above, and nanoparticles are formed on the surface of the alumina powder to carry the catalytic metal.
A vacuum chamber 2 shown in FIG. 1 has a cylindrical shape.
In the vacuum chamber 2, a stirrer 3 and a coaxial vacuum arc deposition source 5 are accommodated.

[Agitator 3]
The stirrer 3 includes a stirring vessel 73 for containing the deposition target 7, scrapers 75 a and 75 b that are fixed blades for stirring the deposition target 7, and lumps (lumps) of the deposition target 7 generated during the stirring process. And a stamp 85 for crushing.
The vapor-deposited body 7 is, for example, titania powder that is a powder having a particle size of 0.1 μm to 1 mm.

A rotation mechanism 72 that rotates the stirring vessel 73 about its central axis 80 is connected to the center of the lower surface of the stirring vessel 73.
The rotation mechanism 72 is disposed below the fixed table 71.
The material of the stirring vessel 73 is, for example, stainless steel, and the inner wall (inner side surface and bottom surface 73a) is buffed. The diameter of the upper opening of the stirring vessel 73 is, for example, 60 to 300 mm. The upper opening may be oval.
The inner wall of the stirring vessel 73 is coated with alumina or Teflon (registered trademark). The coating method may be any of CVD, sputtering, and arc methods. If it is Teflon (registered trademark), the container itself may be made of Teflon (registered trademark).

FIG. 2 is a diagram for explaining the functions of the scrapers 75a and 75b of the fine particle forming apparatus 1. FIG. 2A is a diagram for explaining the arrangement of the scrapers 75a and 75b in the planar direction as viewed from the upper open side of the stirring vessel 73, and FIG. 2B is an illustration of the arrangement as viewed from the side of the scraper 75a. It is a figure for doing.
As shown in FIG. 2A, scrapers 75 a and 75 b are fixed around the stirring vessel 73.
The scrapers 75a and 75b are made of stainless steel, for example. The scrapers 75a and 75b are formed of a rod having a diameter of about 1 mm to 5 mm, and the outside is covered with a Teflon (registered trademark) tube.

The scraper 75a extends from the upper open portion of the stirring vessel 73 into the stirring vessel 73, contacts the vicinity of the inner peripheral surface of the bottom surface 73a of the stirring vessel 73, and extends inward while contacting the bottom surface 73a from the contacted portion. Yes.
The scraper 75b extends from the upper open portion of the stirring vessel 73 into the stirring vessel 73, contacts the vicinity of the central axis of the bottom surface 73a, and extends toward the inner peripheral surface while contacting the bottom surface 73a. .
Further, a gap 76 is formed between the tip of the scraper 75b and the scraper 75a.

The vapor-deposited body 7 in the stirring vessel 73 collides with the scraper 75b, moves toward the gap 76 (toward the inner peripheral surface of the stirring vessel 73), and collides with the scraper 75a through the gap 76 to enter the central axis. Move towards 80. A part of the deposition object 7 collides with the scrapers 75a and 75b, is directed upward, and moves over them.
In this way, by forming the scrapers 75a and 75b, the vapor-deposited body 7 in the stirring vessel 73 is directed from the central axis 80 toward the inner peripheral surface, from the inner peripheral surface toward the central axis 80, and in the depth direction. And can be efficiently stirred.
As a result, when gold is vapor-deposited on the titania powder, as shown in the TEM observation of FIG. 3, gold nanoparticles on the titania surface are several nanometers to 10 nm in size on the titania surface. Supported.

  Further, since the scrapers 75a and 75b are fixed and the stirring vessel 73 is rotated without driving the scrapers 75a and 75b, the driving mechanism can be simplified.

FIG. 4 is a view for explaining the scrapers 75a and 75b and the stamp 85 of the fine particle forming apparatus 1. FIG.
As shown in FIG. 4, a stamp 85 is disposed around the stirring vessel 73 in addition to the scrapers 75a and 75b.
The stamp 85 supports the stamp head 87 which strikes the bottom surface 73a in the stirring vessel 73 and the stamp head in order to pulverize the lumps of the deposition target (powder carrier) 7 generated in the stirring process by the scrapers 75a and 75b. Arm portion 89 for

  The stamp 85 has a first operation in which the stamp head 87 collides with the bottom surface 73a of the stirring container 73 in a process in which the stirring container 73 rotates about the central axis 80, and the stamp head 87 is in contact with the bottom surface 73a. The second operation for holding and the third operation for gradually separating the stamp head 87 from the bottom surface 73a are repeated.

As shown in FIG. 5, the circular edge 90 of the upper opening of the stirring vessel 73 is notched obliquely and forms a slope that smoothly slopes in the direction in which the central axis 80 extends.
The edge 90 of the upper opening of the stirring container 73 has a first edge 90a that is not inclined, a second edge 90b that is smoothly inclined in a direction away from the bottom surface 73a, and a step 90c.
The step 90b is 3 to 20 mm, for example.

  The arm portion 89 has a stamp head 87 fixed to one end on the side disposed in the stirring vessel 73, and the other end is fixed to a stamp head holding portion 93 as shown in FIGS. 4 and 6. The diameter of the arm part 89 is, for example, about 1 mm to 5 mm.

The vicinity of the center of the arm portion 89 in the longitudinal direction is in contact with the edge 90 of the upper opening of the stirring vessel 73. The arm portion 89 is urged toward the bottom surface 73 a of the stirring vessel 73 by a spring 95.
Thereby, the arm part 89 always makes the vicinity of the center part contact the edge part 90 in the process in which the stirring vessel 73 rotates around the central axis 80.
The arm portion 89 is dropped toward the bottom surface 73a at the step 90c of the edge portion 90 described above to cause the stamp head 87 to collide with the bottom surface 73a, and the stamp head 87 is brought into contact with the bottom surface 73a at the first edge portion 90a. Is held for a predetermined period. Thereafter, the stamp head 87c and the bottom surface 73a are brought into a non-contact state at the second edge 90b. This operation is performed while the stirring vessel 73 makes one rotation around the central axis 80, and the first, second, and third operations described above are repeated during the rotation.

FIG. 7 is a diagram for explaining the change over time of the distance between the stamp head 87 and the bottom surface 73a of the stirring vessel 73 during the rotation of the central shaft 80 described above.
As shown in FIG. 7, the stamp head 87 and the bottom surface 73 a of the stirring container 73 periodically contact.
That is, as the arm portion 89 climbs the slope of the edge portion 90, the stamp head 87 gradually rises upward from the bottom surface 73a (floor surface).
The depth of the deposition target 7 in the stirring vessel 73 and the amount of movement of the stamp head 87 in the vertical movement are set so that the stamp head 87 does not come out of the surface of the deposition target 7.
In addition, the rotation speed of the stirring container 73 is 20-100 rpm, for example.

The tip 87a of the stamp head 87 is inclined in a direction away from the bottom surface 73a of the stirring vessel 73, for example, as shown in FIG. Thereby, the vapor-deposited body 7 can collide with the stamp head 87a according to the rotation of the stirring vessel 73, and can be efficiently drawn between the stamp head 87 and the bottom surface 73a. For this reason, it is possible to increase the probability of completely crushing the lumps of the deposition object 7.
Further, in the stirring device 3, the scrapers 75 a and 75 b and the arm portion 89 of the stamp 85 are set to have very small diameters and the stamp head 87 is set so as not to come out from the surface of the deposition target 7. The amount of nanoparticles (vapor deposition body) from the vacuum arc deposition source 5 colliding with the scrapers 75a and 75b and the stamp head 87 can be reduced.

In the fine particle forming apparatus 1, discharge is periodically performed with a pulse as a trigger, as will be described later. As the discharge (evaporation) cycle becomes shorter, the amount of lumps is increased. For structural reasons, the collision period of the stamp 85 with the bottom surface 73 a is proportional to the rotational speed of the stirring vessel 73. Note that the rotation speed of the stirring container 73 after the elapse of a predetermined time from the start of rotation of the stirring container 73 may be faster than the rotation speed within the predetermined time.
That is, the rotation speed of the stirring vessel 73 may be increased as the amount of the vapor deposition material deposited on the vapor deposition target increases.
[Coaxial vacuum arc deposition source 5]
The coaxial vacuum arc evaporation source 5 includes a cylindrical evaporation material 11 made of gold attached to a cathode electrode, a hat-like insulator 14 made of alumina (hereinafter referred to as a hat-type insulator), a trigger electrode 13, Have
The vapor deposition material 11, the hat-type insulator 14, and the trigger electrode 13 attached to the cathode electrode are attached in close contact with each other concentrically.

The anode electrode 23 is made of stainless steel and has a cylindrical shape. The anode electrode 23 is concentrically attached to the vapor deposition material 11 attached to the cathode electrode.
The coaxial vacuum arc deposition source 5 is attached to the wall surface of the vacuum chamber 2 via a support column (not shown) and a vacuum flange (not shown).

Moreover, the power supply device 6 is shown by a simple wiring diagram in FIG.
The power supply device 6 includes a trigger power supply 31, an arc power supply 32, and a capacitor unit 33.
The trigger power source 31 is composed of a pulse transformer, and transforms a pulse voltage in units of μS with an input of 200 V to about 17 times, and outputs a trigger pulse with a positive polarity in units of 3.4 kV and several μS.

The arc power supply 32 is a DC power supply with a capacity of 100 V and several A, and charges the capacitor unit 33. Since the charging time requires about 1 second, the discharge cycle is 1 Hz.
The capacitor unit 33 has a voltage of 720 to 1800 μF and a withstand voltage of 100V. The capacitor unit 33 is charged at 100 V by the arc power source 32.

  The positive output terminal of the trigger power supply 31 is connected to the trigger electrode 13, the negative terminal is connected to the same potential as the negative output terminal of the arc power supply 32, and further connected to the cathode electrode. Both terminals of the capacitor unit 33 are connected between the positive and negative terminals of the arc power supply 32.

The vacuum exhaust system 9 includes a turbo molecular pump 51, a partition valve 52, a rotary pump 53, and an adjustment valve 54.
The turbo molecular pump 51 to the rotary pump 53 are connected by a metal pipe, and the vacuum chamber 2 is evacuated. By performing evacuation, the inside of the vacuum chamber 2 is kept at 10 −4 Pa or less.

Hereinafter, an operation example of the fine particle forming apparatus 1 shown in FIG. 1 will be described.
[Operation example of coaxial vacuum arc deposition source 5]
The electric charge is charged at 100 V by the arc power source 32. Here, the capacitor unit 33 is set to 720 to 1800 μF.
By applying a trigger pulse of 3.4 kV from the trigger power supply 31 to the trigger electrode 13 and applying it between the vapor deposition material 11 attached to the cathode electrode and the trigger electrode 13 via the hat-type insulator 14, a hat-type Creeping discharge occurs on the insulator 14 surface, the electric charge stored in the capacitor unit 33 is discharged between the vapor deposition material 11 and the anode electrode 23, a large amount of current flows into the cathode electrode, and it is attached to the cathode electrode made of gold. The deposited material 11 is formed from a liquid phase to a gas phase and further gold plasma.

  At this time, since a large amount of current (2000 A to 5000 A) flows in the cathode electrode between 200 μS and 500 μS, a magnetic field is formed in the vapor deposition material 11 attached to the cathode electrode. Electrons in the plasma fly under the coaxial vacuum arc deposition source 5 under the Lorentz force generated by the magnetic field formed by the deposition material 11 attached to the cathode electrode.

  Gold ions, which are vapor deposition materials in the plasma, are polarized and attracted to electrons flying in front of the coaxial vacuum arc deposition source 5 by Coulomb force and fly forward of the coaxial vacuum arc deposition source 5. It becomes like this.

  On the other hand, gold ions, which are vapor deposition materials in the plasma, are polarized and fly forward of the coaxial vacuum arc vapor deposition source 5 by Coulomb force. As a result, gold ions grow using the carbon powder 7a as a nucleus, and gold particles in nanometer units are formed.

  The titania powder is stirred by rotating the stirring container 73 on the scrapers 75a and 75b while irradiating gold ions in this way. This is continued to form gold nanoparticles uniformly in the titania powder.

More specifically, gold ions are irradiated toward the carbon powder 7 in the stirring vessel 73. Here, the stirring container 73 is rotated by the rotating mechanism 72, and the vapor deposition body 7 such as carbon in the stirring container 73 is stirred by the scrapers 75a and 75b.
The vapor-deposited body 7 appears on the stirring vessel 73 and is exposed to gold ions by colliding with the scrapers 75a and 75b. By continuing this one after another, gold fine particles are uniformly formed on all the particles of the vapor-deposited body 7 in the stirring vessel 73.

[Stirring and crushing operation]
The fine particle forming apparatus 1 shown in FIG. 1 uses, for example, a vacuum arc plasma generator 3 while stirring alumina powder (deposited body 7) that is a carrier housed in a stirring container 73 that is a cylindrical container in a vacuum. The catalyst metal generated on the surface of the alumina powder is irradiated from above with plasma of nanoparticles (deposited body) which is the catalyst metal generated.
In this process, the arm portion 89 of the stamp 85 shown in FIG. 4 is cut off obliquely at the edge 90 of the upper opening of the stirring vessel 73 in conjunction with the rotation of the stirring vessel 73 around the central axis 80. Climb the slope (second edge 90b shown in FIG. 5). The stamp head 87 gradually floats upward from the bottom surface 73a of the stirring vessel 73.
At this time, the stamp head 87 is lifted while the arm portion 89 is pulled by the spring 97 to the bottom surface 73 a (downward) of the stirring vessel 73.

  When the final upper stage is reached, the stamp head 87, which is suddenly dropped to a lower level by the level difference 90c shown in FIG. Crush the lump of the deposition object 7 at the bottom.

Since the elastic force of the spring 97 acts on the stamp head 87 even on the bottom surface 73a of the step, the stamp head 87 moves while contacting the bottom surface 73a as the stirring vessel 73 rotates. That is, while the arm portion 89 and the first edge portion 90a shown in FIG. 5 are in contact, the stamp head 87 moves while being in contact with the bottom surface 73a.
At this time, since the fine particles that have entered between the stamp head 87 and the bottom surface 73a pass between the stamp head 87 and the bottom surface 73a, they are crushed like a buckwheat mortar and further broken into powder.
Then, the slope of the edge 90b is gradually climbed from the stamp head 87 or the lower stage again, and when it reaches the position of the uppermost step 90c, it is dropped to the lower stage at once, so that the tension of the spring 97 is released and Crush and then crush. Repeat this.

FIG. 9 is an external view of the stirring container 73 as viewed from above.
FIG. 10 and FIG. 11 are views of the remaining lumps.
FIG. 9 and FIG. 12 are diagrams showing a state where the stamp head 87 is crushed.
Fig. 12 shows a state where the powder after gold is loaded on carbon powder is ground.
FIG. 13 is a view for explaining the result of grinding the powder before and after stirring with gold supported on titania powder by the fine particle forming apparatus of the embodiment of the present invention, and FIG. FIG. 13B shows the state after stirring.

As described above, the fine particle forming apparatus 1 uses the stamp 85 to apply pressure to the surface of the vapor-deposited body 7 in the stirring vessel 73 to crush it, and stir the crushed powder with the stamp head 87 of the stamp 85. According to the rotation of the stirring vessel 73 between the bottom surface 73a of the vessel 73, it is further finely ground.
As a result, when various metals and reactive substances are deposited and supported in a vacuum, it is possible to suppress the formation of powder lumps and to crush the formed lumps, thereby preventing the powder from agglomerating while supporting the catalyst. The catalyst can be supported on the powder while maintaining the particle size as before.

[First Modification]
In the embodiment described above, the stamp head 87 is moved up and down by making a slope and a step on the upper edge of the wall of the stirring vessel 73, pulling the arm portion 89 of the stamp 85 downward by the spring 97, and using the rotation of the stirring vessel 73. A mechanism that knocks down at the step portion is used.
The present invention may use, for example, a mechanism that independently drives the stamp 85 up and down without interlocking with the rotation of the stirring vessel 73.

[Second Modification]
In the embodiment described above, the stamp 85 is used to grind lumps, but instead, a mechanism that grinds lumps with a roller or a propeller may be used.

The present invention is not limited to the embodiment described above.
That is, those skilled in the art may make various modifications, combinations, subcombinations, and alternatives regarding the components of the above-described embodiments within the technical scope of the present invention or an equivalent scope thereof.
In the embodiment described above, titania is mainly exemplified. However, the powder is not limited to titania, and the deposited material is not limited to gold, and the lumping mechanism can be applied to all other powders and deposited materials.

  In the above-described embodiment, the cylindrical stirring container 73 is illustrated, but a conical stirring container 73 may be used.

  INDUSTRIAL APPLICABILITY The present invention is used for fuel cell and vehicle exhaust gas metal support, air cleaning catalyst support, gas sensor, magnetic material, and dielectric material.

DESCRIPTION OF SYMBOLS 1 ... Fine particle formation apparatus 3 ... Agitation apparatus 5 ... Coaxial type vacuum arc vapor deposition source 7 ... Deposited body 73 ... Agitation container 75a, 75b ... Scraper 85 ... Stamp 87 ... Stamp head 89 ... Arm part 90 ... Edge

Claims (7)

A deposition source for flying the deposition material;
A container that is disposed opposite to the vapor deposition source and contains a powder carrier that is a vapor deposition target;
Stirring means for stirring the powder carrier in the container;
In order to pulverize the lump of the powdery carrier generated in the stirring process by the stirring means, the first operation of causing the stamp head to collide with the bottom surface of the container, and the stamp head in contact with the bottom surface Crushing means for sequentially repeating a second operation for holding and a third operation for separating the stamp head from the bottom surface;
The circular edge of the upper open part of the container becomes a slope inclined in the direction in which the central axis of the container extends, and has a step at a predetermined location.
The grinding means is
An arm portion that contacts the edge portion while being biased toward the bottom surface, and when the arm portion falls toward the bottom surface at the step, the stamp head is brought into contact with the bottom surface; A fine particle forming apparatus that separates the stamp head from the bottom surface when a predetermined position is reached along the slope. Said grinding means, a plate-like the scan Tanpuheddo, up and down movement relative to said bottom surface, to collide with the punch face of the stamp head to the bottom surface,
End on the side of the deposition target of the stamp surface to penetrate the particle formation apparatus according to claim 1 which is inclined in a direction away from said bottom surface. The container is cylindrical or conical, is rotated around the central axis,
It said stirring means has one end fixed to the periphery of the container, the claims and the other end is inserted into the container and stirred by colliding before Kikotai like carrier which moves in conjunction with the rotation of the pre-SL container The fine particle forming apparatus according to claim 1 or 2. The stirring means includes
A first scraper that contacts the outer periphery of the bottom surface of the container from the upper open portion of the container, and extends inward along the bottom surface from the contacted position;
The contact from the upper opening in the vicinity of the central axis of said bottom surface of said container, particle formation apparatus according to claim 3 and a second scraper extending outwardly the from contact with the portion along the bottom surface. The rotational speed of the container increases as the deposition cycle of the deposition source becomes shorter,
The fine particle forming apparatus according to claim 4, wherein a collision cycle of the stirring unit with the bottom surface of the stamp head increases as a discharge cycle of the vapor deposition source becomes shorter. The fine particle forming apparatus according to claim 1, wherein the powdery carrier is a powder having a particle size of 0.1 μm to 1 mm. A fine particle forming method for supporting a vapor deposition material flying from the vapor deposition source on the vapor deposition source while stirring the powdery carrier that is the vapor deposition target in a container disposed opposite to the vapor deposition source,
In the process of stirring the powdery carrier in the container, the bottom of the container is hit with a pulverizing means to pulverize the lump of the powdery carrier generated by the stirring,
A method for forming fine particles, wherein the rotational speed of the container is increased as the amount of the vapor deposition material deposited on the powder carrier increases.