WO2022181433A1

WO2022181433A1 - Horizontal-type powder surface film forming device

Info

Publication number: WO2022181433A1
Application number: PCT/JP2022/006347
Authority: WO
Inventors: 智弘丸子
Original assignee: 株式会社フルヤ金属
Priority date: 2021-02-26
Filing date: 2022-02-17
Publication date: 2022-09-01
Also published as: JP2022131217A

Abstract

The purpose of the present invention is to provide a horizontal-type powder surface film forming device which improves dry stirring efficiency of powder and continuously produces a powder covered on the surface with a fine film and which further achieves high productivity by suitably controlling the film forming speed so as to have an even amount of film formed on the raw powder. This horizontal-type powder surface film forming device 100 comprises: a horizontally inclined barrel 1; a rotation mechanism 7 which rotates the barrel 1 with the primary axis thereof as the rotation axis 2; a pressure regulating mechanism 23 which maintains the pressure of the barrel 1 at a prescribed pressure less than or equal to atmospheric pressure; and a film forming mechanism 43 which is installed inside of the barrel 1; while the barrel 1 is rotated, the horizontal-type powder surface film forming device 100 forms a thin film on the surface of a raw powder 42 which has been inserted into the barrel 1. The barrel 1 has a passage 45 that extends spirally around the rotation axis 2; the bottom surface 44 of the passage 45 is the inside surface on the side wall of the barrel 1, and the top surface of the passage 45 is open.

Description

Horizontal powder surface coating equipment

The present disclosure relates to a powder surface film forming apparatus for forming a thin film on the surface of each powder particle.

In some cases, a thin film is formed on the surface of the particles in order to add new functions to the powder. For example, a wet method such as a plating method or a sol-gel method has been widely used to form a thin film on the surface of particles. While the wet method has the advantage of mass production, it is difficult to form a thin film containing multiple elements on the complex surfaces of particles. Moreover, since it is a wet method, the solvent remains on the surface of the powder, inside the thin film, and further on the surface of the thin film, and there is a problem that the intended function cannot be exhibited.

Therefore, a powder surface thin film formation technology using a dry method was desired. There is a sputtering method as a film forming technique using a dry method, and a powder film forming apparatus using the sputtering method has been proposed (see, for example, Patent Document 1).

There have also been proposals for a technology that achieves multi-element simultaneous film formation, which is a conventional problem, and a technology that improves powder agitation (see, for example, Patent Documents 2 and 3).

Patent Literatures

2 and 3 disclose an apparatus in which a stirring plate and a scraper are installed in a powder surface film-forming apparatus to promote agitation of the raw material powder so that the raw material powder is evenly sputtered. In addition, a powder surface film forming apparatus has been proposed which enables the formation of a multi-element thin film on the powder surface, guides the powder to a region where film can be formed effectively, and has a jig for agitating the powder.

Japanese Patent No. 3068947 Japanese Patent No. 6789217 Japanese Patent No. 6715003

It is clear that forming a film on the powder surface by the dry method is an effective means of adding high functionality to the powder. However, in the techniques disclosed in Patent Documents 1 to 3, a barrel-shaped container is arranged horizontally, powder is put inside it, it is rotated to achieve stirring, and a stirring jig is installed at the powder contact part. Although the agitation is improved by doing so, if the rotation speed of the barrel is high, the powder sticks to the barrel due to centrifugal force and rises to a position where the angle of repose is high, and the powder falls beyond the angle of repose. Occasionally, the powder may scatter in the barrel and adhere to the film forming apparatus, or the discharge during film formation may become unstable. In addition, considering problems such as peeling of the coating powder from the coating powder, the stirring jig cannot be moved quickly, so the stirring efficiency cannot be said to be sufficiently good. In addition, the powder cannot be fed continuously, and the batch system has a structure that significantly impairs productivity.

Therefore, the object of the present disclosure is to improve the stirring efficiency of the powder by the dry method, to continuously produce the powder whose surface is coated with a thin film, and to form an even amount of film with respect to the raw material powder. Another object of the present invention is to provide a horizontal powder surface film-forming apparatus that achieves high productivity by properly controlling the film-forming speed.

As a result of intensive studies, the present inventors found that by providing a passage extending spirally around the rotation axis of the barrel on the inner surface of a horizontal rotating barrel, the powder placed in this passage is automatically displaced by the rotation of the barrel. It is conveyed from one end of the barrel to the other end while being agitated, or is conveyed from one end of the barrel to the other end and then conveyed from the other end to the other end of the barrel in the reverse direction, and further during conveyance. The inventors have found that a uniform thin film can be formed on the surface of the raw material powder by forming a film in , and completed the present invention. That is, the horizontal powder surface deposition apparatus according to the present invention comprises a laterally tilted barrel, a rotating mechanism for rotating the main axis of the barrel as a rotation axis, and a pressure in the barrel to a predetermined pressure below atmospheric pressure. and a film forming mechanism installed in the barrel, and a horizontal powder surface film forming mechanism for forming a thin film on the surface of the raw material powder put in the barrel while rotating the barrel. The apparatus is characterized in that the barrel has an inner surface of the side wall as a bottom surface, a passage extending spirally around the rotation axis, and a top surface of the passage that is open.

In the horizontal powder surface deposition apparatus according to the present invention, the passages are preferably provided with partitions between adjacent passages. The raw material powder placed in the passage can be moved along the main axis direction of the barrel while being reliably and efficiently stirred by the rotation of the barrel. can be deposited over a wider area in a wider state, resulting in higher deposition efficiency.

In the horizontal powder surface deposition apparatus according to the present invention, the partition may be a continuous spiral partition, a continuous spiral step partition, or a plurality of partitions arranged in a spiral step shape with portions facing each other. It is preferable that the partition is an intermittent spiral stepped partition, or a partition that is a combination of at least two of these three kinds of partitions. The boundary between the passages has a shape extending spirally around the rotation axis of the barrel on the inner surface of the side wall of the barrel. can take

In the horizontal powder surface deposition apparatus according to the present invention, the passage preferably has a projection on the bottom surface. After the raw material powder passes through the projections, it acts like a fluid and forms a Karman vortex, thereby obtaining a stirring effect.

The horizontal powder surface deposition apparatus according to the present invention preferably has a knocker for impacting the barrel or a vibrator for vibrating the barrel. The impact or vibration applied to the barrel agitates the raw material powder, making it easier to form a film over the entire powder.

In the horizontal powder surface deposition apparatus according to the present invention, there is provided a powder supply mechanism that supplies the raw material powder into the barrel from one end surface of the barrel, and a thin film formed on the surface from the other end surface of the barrel. a powder recovery mechanism for recovering the coated powder, the powder supply mechanism having a first preliminary chamber capable of adjusting pressure and atmosphere, the first preliminary chamber having a powder inlet and a and is connected to one end face of the barrel via a first opening/closing mechanism, the powder recovery mechanism has a second preliminary chamber capable of adjusting pressure and atmosphere, and the second preliminary chamber It is preferable that the chamber is connected to the other end surface of the barrel via a second opening/closing mechanism, and is also connected to the powder recovery port. The raw material powder is continuously introduced from one side of the barrel, and the introduction of the raw material powder can be performed in a vacuum atmosphere or at a predetermined gas pressure. It is a structure that allows the powder surface to be deposited during the movement, and furthermore, the coated powder that has completed the deposition is continuously discharged, and the inside of the barrel is a vacuum atmosphere or a predetermined gas pressure. The structure can be such that the coating powder can be discharged to the atmosphere while maintaining the

In the horizontal powder surface deposition apparatus according to the present invention, it is preferable that the rotating mechanism has a regulator for the number of rotations of the barrel and a switch for forward/reverse rotation of the rotation direction. The motion of the barrel can be diversified, thereby more efficiently stirring the raw material powder in the barrel, and as a result, the raw material powder can be uniformly coated.

In the horizontal powder surface deposition apparatus according to the present invention, there is provided a powder supply mechanism for supplying the raw material powder into the barrel from one end surface of the barrel, and a thin film formed on the surface from one end surface of the barrel. a powder recovery mechanism for recovering the coated powder, wherein the powder supply mechanism has a first preliminary chamber capable of adjusting pressure and atmosphere, and the first preliminary chamber includes a powder inlet. and is connected to one end face of the barrel via a first opening/closing mechanism, the powder recovery mechanism has a second preliminary chamber capable of adjusting pressure and atmosphere, and the second The preliminary chamber is connected to one end face of the barrel via a second opening/closing mechanism and is connected to the powder recovery port, and the rotating mechanism includes a regulator for the number of rotations of the barrel and a positive rotation direction. It is preferable to have a reverse/reverse switch. The raw material powder is continuously introduced from one side of the barrel, and the introduction of the raw material powder can be performed in a vacuum atmosphere or at a predetermined gas pressure. It is a structure in which the powder can be moved dynamically and a film can be formed on the surface of the powder during the movement, and the powder can be moved back and forth along the rotation axis direction of the barrel to ensure the thickness of the film. Furthermore, by rotating the barrel in reverse, the powder for which film formation has been completed is discharged from the powder input side, and the powder is discharged to the atmosphere while maintaining a vacuum atmosphere or a predetermined gas pressure in the barrel. It can be a structure that can be done. Furthermore, the motion of the barrel can be diversified, thereby more efficiently agitating the powder in the barrel, and as a result, forming a uniform film on the raw material powder.

The horizontal powder surface deposition apparatus according to the present invention preferably has an angle adjustment mechanism for adjusting the inclination of the main axis of the barrel. The slanting angle of the barrel facilitates the movement of the powder, making introduction, movement and discharge more reliable.

In the horizontal powder surface film-forming apparatus according to the present invention, the film-forming mechanism preferably has a film-forming source using a sputtering method, an ion plating method, an ion beam method, or an atom beam method. A variety of deposition mechanisms can be selected, all of which can provide a uniform coating powder.

According to the present disclosure, the powder stirring efficiency by the dry method is improved, the powder whose surface is coated with a thin film is continuously produced, and the film thickness is uniform with respect to the raw material powder. It is possible to provide a horizontal powder surface film-forming apparatus that achieves high productivity by properly controlling the film-forming speed.

1 is a schematic diagram showing a first example of a horizontal powder surface deposition apparatus according to this embodiment; FIG. Fig. 2 is a schematic perspective view of the barrel and partition of the first example; Fig. 2 is a schematic cross-sectional view showing the barrel and partition of the first example; It is a schematic diagram showing a second example of a horizontal powder surface deposition apparatus according to the present embodiment. FIG. 11 is a schematic perspective view of a second example barrel and partition; It is a schematic diagram showing a third example of a horizontal powder surface deposition apparatus according to the present embodiment. FIG. 11 is a schematic perspective view of a third example barrel and partition; It is the schematic which shows the state which tilted the 1st example to the lower right. It is the schematic which shows the state which tilted the 1st example to the upper right. It is a schematic diagram showing a fourth example of a horizontal powder surface deposition apparatus according to the present embodiment. FIG. 11 is a schematic perspective view of a fourth example barrel and partition;

Hereinafter, the present invention will be described in detail by showing embodiments, but the present invention is not interpreted as being limited to these descriptions. Various modifications may be made to the embodiments as long as the effects of the present invention are achieved. In the figure, the parts with the same name are given the same reference numerals regardless of the shape.

Next, a horizontal powder surface deposition apparatus according to this embodiment will be described with reference to FIGS. 1 to 3. FIG. A horizontal powder surface deposition apparatus 100 according to this embodiment includes a barrel 1 tilted sideways, a rotation mechanism 7 that rotates the main shaft of the barrel 1 as a rotation axis 2, and a and a film forming mechanism 43 installed in the barrel 1, and a thin film is formed on the surface of the raw material powder 42 put in the barrel 1 while rotating the barrel 1. The barrel 1 has a bottom surface 44 on the inner surface of the side wall and a passage 45 extending spirally around the rotating shaft 2. The top surface of the passage 45 is open. .

The barrel 1 preferably has a tubular shape, more preferably a cylindrical shape or a polygonal tubular shape. Moreover, it is preferable that the end face of the barrel 1 has an opening. For example, as shown in FIG. 2, the end face of the barrel 1 may have an annular flat surface with an opening 46 in the center, or may have an opening 47 with no surface at all. The barrel 1 is tilted sideways and has a rotation mechanism 7 that rotates around the main axis of the barrel 1 as the rotation axis 2 . The rotating mechanism 7 has a drive motor 3, a drive shaft 4 rotated by the drive motor 3, a drive roll 5 rotated by the drive shaft 4, and a slave roll 6 freely rotating. The drive roll 5 and follower roll 6 are in contact with the outer surface of the side wall of the barrel 1 . When the drive motor 3 rotates, the drive roll 5 also rotates, causing the barrel 1 to rotate around the rotating shaft 2 . At this time, the subordinate roll 6 also rotates, and the weight balance of the barrel 1 is adjusted. The rotation mechanism 7 preferably has a regulator (not shown) for the number of revolutions of the barrel 1 . The adjuster is, for example, a rotation adjuster or gearbox of the drive motor 3 . It is preferable that the rotation mechanism 7 further has a switch for forward/reverse rotation of the rotation direction of the drive shaft 4 . The changeover is, for example, a geared rotation converter or a rotation converter of the drive motor 3 .

The barrel 1 has at least the

openings

46 and 47 of the barrel 1 covered by the vacuum chamber 24 . FIG. 1 shows a form in which a portion of the side wall of the barrel 1 is covered with the heating/cooling mechanism 48 and both ends of the barrel including the

openings

46 and 47 of the barrel 1 are covered with the vacuum chamber 24. It may be covered by chamber 24 . The pressure adjusting mechanism 23 is connected to the vacuum chamber 24 . The pressure adjustment mechanism 23 is, for example, an exhaust pump. Preferably, the pressure adjusting mechanism 23 further includes a pipe 21 connected to the vacuum chamber 24 and a first gas system 18 connected to the pipe 21 . The pressure regulating mechanism 23 can maintain the pressure in the barrel 1 at a predetermined pressure below the atmospheric pressure and replace it with a predetermined gas atmosphere by means of exhaust by the exhaust pump and gas supply by the first gas system 18 . The heating/cooling mechanism 48 heats the raw material powder 42 by heating the barrel 1, and cools the barrel 1 after the film is formed on the raw material powder 42. may have

The film forming mechanism 43 is preferably installed inside the barrel 1 . In FIG. 1, the film-forming mechanism 43 has illustrated the form which has the film-forming apparatus 25 and the film-forming material 26. As shown in FIG. A film-forming material is discharged from the film-forming material 26 toward the raw material powder 42 in the barrel 1 by the film-forming device 25 . The raw material powder 42 is gathered on the vertically lower side of the inner surface of the side wall inside the barrel 1 by gravity. Therefore, it is preferable that the film forming mechanism 43 discharges the thin film forming substance downward as shown in FIG. More specifically, the film forming mechanism 43 preferably has a film forming source using a sputtering method, an ion plating method, an ion beam method, or an atom beam method. A variety of deposition mechanisms can be selected, all of which can provide a uniform coating powder.

The passage 45 has the inner surface of the side wall of the barrel 1 as the bottom surface 44 and extends spirally around the rotating shaft 2 . The top surface of the passage 45 is open. Since the film-forming mechanism 43 discharges the thin-film-forming substance downward, the top surface of the passage 45 is open, so that the inside surface of the side wall in the barrel 1 is discharged vertically downward in the passage 45 . A film-forming material can be applied to the surface of each particle of the gathering raw material powder 42 .

As shown in FIGS. 2 and 3, the raw material powder 42 collected on the vertically lower side in the passage 45 tends to remain on the bottom surface on the vertically lower side when the barrel 1 rotates around the rotating shaft 2. , move in a spiral direction in the passage while being automatically stirred. At this time, as long as the barrel 1 rotates in the same direction, the raw material powder 42 is moved from one end face side of the barrel 1 to the other end face side. Further, when the barrel 1 rotates in the opposite direction, the raw material powder 42 is moved from the other end surface side of the barrel 1 to the one end surface side, that is, moved in the opposite direction. In FIG. 1, when the bottom surface 44 on the vertically lower side of the barrel 1 is rotated in the direction of moving away from the plane of the paper, the raw material powder 42 is moved from left to right. By activating the film forming mechanism 43 while the raw material powder 42 is moving, a thin film can be formed on the surface of the raw material powder 42 that is being automatically stirred.

The shape of the passage 45 is not particularly limited as long as it extends spirally around the rotation axis. For example, a form in which grooves are provided on the inner surface side of the side wall of the barrel 1 is exemplified. The groove has, for example, a semi-circular, V-shaped or U-shaped cross-section.

In this embodiment, the passages 45 are preferably provided with partitions 40 between adjacent passages 45 . The raw material powder 42 placed in the passage 45 can be moved along the main axis direction of the barrel 1 while being reliably and efficiently stirred by the rotation of the barrel 1 . Further, since the partition 40 itself has a small end surface area, the raw material powder 42 can be formed into a film over a wider area, thereby increasing the film formation efficiency. The partition 40 may be, for example, a partition wall formed by processing the inner surface of the side wall of the barrel 1, or a fence-like plate formed into a spiral shape and fixed to the inner surface of the side wall of the barrel 1. There is a form of partition plate. The fixing of the partition plate includes a form of mechanical fixing or a form of joining and fixing. The height of the partition 40 from the bottom surface 44 is, for example, 1 to 20 mm. It is preferable that the raw material powder 42 is supplied in such an amount that it does not climb over the partition 40 . The distance between the partition 40 and the adjacent partition is preferably 50 to 100 mm, for example. The thickness of the partition 40 is preferably 1 mm or less for the purpose of reducing film formation on the end faces of the partition.

Various forms of the partition 40 will be described. In this embodiment, the partition 40 is a continuous spiral partition (illustrated as the partition 40 in the horizontal powder surface deposition apparatus 100 in FIGS. 1 to 3), a continuous spiral step partition (FIGS. (illustrated as partition 40 in horizontal powder surface deposition apparatus 200 in FIG. 5) or intermittent spiral step partitions in which partitions are arranged in a spiral step pattern with portions facing each other (FIGS. 6-7). ), or a combination of at least two of these three types of partitions. The boundary between the passages has a shape extending spirally around the rotation axis 2 of the barrel 1 on the inner surface of the side wall of the barrel 1. can take various forms. Any partition 40 can guide the raw material powder 42 along the spiral direction. Combinations of partitions 40 include a combination of a continuous spiral partition and a continuous spiral step partition, a combination of a continuous spiral partition and an intermittent spiral step partition, and a continuous spiral step. A combination of a spiral stepped partition and an intermittent spiral stepped partition, or a combination of a continuous spiral stepped partition, a continuous spiral stepped partition and an intermittent spiral stepped partition.

In this embodiment, the passage 45 preferably has a protrusion 41 on the bottom surface 44. After the raw material powder 42 passes through the projections 41, it acts like a fluid and forms a Karman vortex, thereby obtaining a stirring effect. 1 to 7 illustrate the projection 41 having a conical shape, but it may be a columnar projection, a cylindrical projection, a polygonal prismatic projection, a polygonal cylindrical projection, or a polygonal pyramidal projection. The height of the protrusion 41 is preferably lower than the height of the partition 40 . Also, the width of the protrusion 41 is preferably 1 to 20% of the width of the passage 45 . It is preferable that the protrusions 41 are evenly arranged at predetermined angles with respect to the rotating direction of the rotating shaft 2 . For example, they are arranged every 90°. Moreover, it is preferable to arrange them evenly along the direction of the rotating shaft 2 . For example, as shown in FIG. 1, it is preferable to arrange for each passage.

In this embodiment, as shown in FIG. 1, it is preferable to have a knocker 50 that gives impact to the barrel 1 or a vibrator 50 that gives vibration. The raw material powder 42 is agitated by the impact or vibration applied to the barrel 1, making it easier to form a film over the entire powder. Both the knocker and the vibrator may be provided. Also, a plurality of knockers may be provided, and a plurality of vibrators may be provided. Although the knocker 50 or vibrator 50 is arranged under the barrel 1 in FIG. The knocker may be mechanical, electric, or pneumatic.

In this embodiment, as shown in FIG. 1, a powder supply mechanism that supplies raw material powder into the barrel 1 from one end face side of the barrel 1 and a thin film is formed on the surface from the other end face side of the barrel 1. The powder supply mechanism has a first preliminary chamber 13 capable of adjusting pressure and atmosphere, and the first preliminary chamber 13 is connected to the powder inlet 9. and is connected to one end face of the barrel 1 via the first opening/closing mechanism 15, and the powder recovery mechanism has a second preliminary chamber 28 capable of adjusting pressure and atmosphere. 28 is preferably connected to the other end surface of barrel 1 via second opening/closing mechanism 27 and to powder recovery port 30 .

In this embodiment, as shown in FIG. 1, the powder inlet 9 is connected to the valve 11 via the pipe 10, and the valve 11 is connected to the first preliminary chamber 13 via the pipe 12. The first spare chamber 13 is further connected via a pipe 14 to a first opening/closing mechanism 15 which, via a pipe 16 , is connected to an opening 46 at one end face of the barrel 1 in the vacuum chamber 24 . connected with The first spare chamber 13 is also connected to a second gas system 17 via a pipe 20 and to an exhaust pump 19 via a pipe 22 . Preferably, valves are appropriately arranged in the

pipes

20 and 22 . The powder supply mechanism has a powder inlet 9, a first preliminary chamber 13, a valve 11, a first opening/closing mechanism 15, a second gas system 17, an exhaust pump 19, and piping connecting these. Furthermore, the first gas system 18 is connected via a pipe 21 to an opening 46 in one end face of the barrel 1 in the vacuum chamber 24 . It is preferable that a valve is appropriately arranged in the pipe 21 .

The valve 11 can be omitted when the first preliminary chamber 13 and the powder inlet 9 are integrated into a case. The first opening/closing mechanism 15 is a valve or a shutter.

The first gas system 18 releases atmospheric gases such as Ar, O ₂ and N ₂ in the barrel 1 or releases the film-forming gas in the barrel 1 . The second gas system 17 releases a gas for adjusting the pressure of the first preliminary chamber 13, such as Ar. The valve 11 can be opened when the pressure in the first preliminary chamber 13 substantially coincides with the atmospheric pressure.

The exhaust pump 19 evacuates the interior of the first preliminary chamber 13 and adjusts the pressure of the first preliminary chamber 13 . The first opening/closing mechanism 15 can be opened when the pressures in the first preliminary chamber 13 and the pressure in the barrel 1 substantially match.

In this embodiment, as shown in FIG. 1, the powder recovery port 30 is connected to the valve 29 through the pipe 35, and the valve 29 is connected to the second preliminary chamber 28 through the pipe 34. The second preliminary chamber 28 is further connected to a second opening/closing mechanism 27 via a pipe 33 , and the second opening/closing mechanism 27 is connected to the bottom wall of the vacuum chamber 24 on the side of the opening 47 on the other end surface of the barrel 1 . ing. The second spare chamber 28 is also connected to the third gas system 31 via a pipe 36 and to an exhaust pump 32 via a pipe 37 . Valves are preferably arranged in the

pipes

36 and 37 as appropriate. The powder recovery mechanism has a powder recovery port 30, a second preliminary chamber 28, a valve 29, a second opening/closing mechanism 27, a third gas system 31, an exhaust pump 32, and piping connecting these.

When the second preliminary chamber 28 and the powder recovery port 30 are integrated into the case, the valve 29 can be omitted. The second opening/closing mechanism 27 is a valve or a shutter.

The third gas system 31 releases gas for adjusting the pressure of the second preliminary chamber 28 with Ar or the like. The valve 29 can be opened when the pressure in the second preliminary chamber 28 substantially matches the atmospheric pressure.

The exhaust pump 32 evacuates the inside of the second preliminary chamber 28 and adjusts the pressure of the second preliminary chamber 28 . The second opening/closing mechanism 27 can be opened when the pressure in the second preliminary chamber 28 and the pressure in the barrel 1 substantially match.

The pressure adjustment mechanism 23 discharges atmospheric gases such as Ar, O ₂ and N ₂ released from the first gas system 18 inside the barrel 1 . Also, the film-forming gas in the barrel 1 is discharged.

The horizontal powder surface deposition apparatus 100 has a structure in which the raw material powder is continuously introduced from one side of the barrel, and the raw material powder can be introduced in a vacuum atmosphere or under a predetermined gas pressure. It is a structure in which the powder is continuously moved to the opposite side while moving, and a film can be formed on the powder surface during the movement. The structure can be such that the powder can be discharged to the atmosphere while maintaining a vacuum atmosphere or a predetermined gas pressure.

In this embodiment, the horizontal powder surface deposition apparatus 100 preferably has an angle adjustment mechanism 8 that adjusts the inclination of the main axis of the barrel 1. By giving an inclination angle to the barrel 1, the movement of the powder is facilitated, and introduction, movement and discharge can be performed more reliably. In FIG. 1, the main axis which coincides with the rotation axis 2 of the barrel 1 is horizontal, and in FIG. FIG. 9 shows a mode in which the raw material powder 42 is easily moved from right to left when the main shaft is tilted to the upper right and the raw material powder 42 is in the passage 45 of the barrel 1 . It is preferable to adjust the inclination of the main shaft of the barrel 1 by expanding and contracting the angle adjusting mechanism 8 a and the angle adjusting mechanism 8 b as the angle adjusting mechanism 8 . The inclination of the main axis of the barrel 1 when forming a film on the powder is preferably adjusted up to 20° when the horizontal direction is 0°.

Next, a horizontal powder surface deposition apparatus 400 as a modification will be described with reference to FIGS. 10 and 11. FIG. As shown in FIGS. 10 and 11, the horizontal powder surface deposition apparatus 400 includes a powder supply mechanism that supplies powder into the barrel 1 from one end surface of the barrel 1, and a thin film from one end surface of the barrel 1. and a powder recovery mechanism for recovering powder having a film formed on the surface thereof, the powder supply mechanism has a first preliminary chamber 13 capable of adjusting pressure and atmosphere, and the first preliminary chamber 13 is It is connected to the powder inlet 9 and to one end face of the barrel 1 via the first opening/closing mechanism 15. The powder recovery mechanism has a second preliminary chamber 28 capable of adjusting pressure and atmosphere. The second preliminary chamber 28 is connected to one end surface of the barrel 1 via the second opening/closing mechanism 27 and is connected to the powder recovery port 30, and the rotation mechanism adjusts the rotation speed of the barrel 1. It is preferable to have a device and a switch for forward/reverse rotation of the rotation direction.

The description will focus on differences from the horizontal powder surface deposition apparatus 100 shown in FIGS. The horizontal powder surface deposition apparatus 100 and the horizontal powder surface deposition apparatus 400 have the same configuration except for the differences described below.

The horizontal powder surface deposition apparatus 400 has a powder supply mechanism and a powder recovery mechanism similar to the powder supply mechanism and powder recovery mechanism of the horizontal powder surface deposition apparatus 100 . However, the powder supply mechanism of the horizontal powder surface coating apparatus 100 is connected to one end surface of the barrel, and the powder recovery mechanism is connected to the other end surface of the barrel, whereas the horizontal powder surface coating apparatus 400 is connected to the other end surface of the barrel. , both the powder supply mechanism and the powder recovery mechanism are connected to one end face side of the barrel. In the horizontal powder surface deposition apparatus 100, as shown in FIG. 2, one end face of the barrel 1 (the left end face in FIG. 1) has an annular flat surface with an opening 46 in the center. The end face on the other end face side of the barrel 1 (the right end face in FIG. 1) is in the form of an opening 47 with no surface at all on the end face. On the other hand, in the horizontal powder surface deposition apparatus 400, as shown in FIG. 11, one end face of the barrel 1 (the left end face in FIG. 10) is an opening 47 having no surface on the end face. The end face on the other end face side of the barrel 1 (right end face in FIG. 10) has an annular flat surface with an opening 46 in the center. That is, the end face of the barrel 1 on the side for recovering the powder coated with the thin film has an opening 47 with no face at all. The partition 40 restricts the movement of the powder along the direction of the rotating shaft 2 of the barrel 1. Therefore, by controlling the rotation of the barrel 1, the powder can be prevented from spilling into the vacuum chamber 24. Therefore, the end face of the barrel 1 may be unified into a form having an opening 47 with no surface at all, instead of having a form having an annular flat surface with an opening 46 in the center. Further, when the end face of the barrel 1 is configured to have an annular flat surface with an opening 46 in the center, the annular plate forming the annular flat surface may be detachable.

In the horizontal powder surface deposition apparatus 400, the raw material powder is continuously introduced from one side of the barrel, and the raw material powder can be introduced in a vacuum atmosphere or under a predetermined gas pressure. It is a structure in which the powder is continuously moved to the opposite side, and a film can be formed on the powder surface during that movement. In addition, the powder after film formation is discharged from the powder input side by rotating the barrel in the reverse direction, and the inside of the barrel is maintained at a vacuum atmosphere or a predetermined gas pressure. However, the structure can be such that the powder can be discharged to the atmosphere. Furthermore, the motion of the barrel can be diversified, thereby more efficiently agitating the powder in the barrel, and as a result, forming a uniform film on the raw material powder.

(Modified example of spare room)
In FIG. 1, a third preliminary chamber may be provided between the first opening/closing mechanism 15 and the vacuum chamber 24 (not shown). As long as the raw material powder is kept on standby under the same pressure as in the barrel, the raw material powder can be fed into the barrel at any time by adjusting the feeding amount, and new raw powder can be fed into the first preliminary chamber. It can be put in from the powder inlet. A fourth preliminary chamber may be provided between the vacuum chamber 24 and the second opening/closing mechanism 27 (not shown). If the coating powder is kept on standby under the same pressure as in the barrel, the amount of the coating powder to be moved to the second preliminary chamber can be adjusted. This is particularly effective when the amount of coating powder exceeds the capacity of the second preliminary chamber.

Next, a method for manufacturing powder whose surface is coated with a thin film will be described using the horizontal powder surface deposition apparatus according to this embodiment.

(preliminary process of putting raw materials into the barrel)
First, it is preferable to remove moisture from the raw material powder in advance by applying a vacuum atmosphere or further heating. It has the effect of preventing powder agglomeration. A film is formed on these powders by this horizontal powder surface film forming apparatus. Next, the raw material powder is put into the first preliminary chamber 13 which is open to the atmosphere from the powder inlet 9, and the second gas system 17 and the exhaust pump 19 are used with the valve 11 and the first opening/closing mechanism 15 closed. 1 Preliminary chamber 13 is set to a desired pressure and replaced with a gas atmosphere.

(Pressure and atmosphere adjustment in the barrel)
Before supplying the raw material powder to the inside of the barrel 1, the first gas system 18 and the pressure adjusting mechanism 23 are used to set the pressure inside the vacuum chamber 24 and the inside of the barrel 1 to a desired pressure, thereby replacing the inside with a desired gas atmosphere.

(The process of putting raw materials into the barrel)
The first opening/closing mechanism 15 is opened, and raw material powder is supplied to the inside of the barrel 1 in the vacuum chamber 24 . At this time, it is preferable that the pressure in the first preliminary chamber 13, the pressure in the vacuum chamber 24 and the pressure in the barrel 1 are approximately the same. Moreover, it is preferable to supply the raw material powder at a constant speed.

(Movement and film formation of raw material powder in barrel)
By rotating the bottom surface 44 on the vertically lower side of the barrel 1 in a direction to move beyond the plane of the paper, the raw material powder 42 moves along the passage 45 , that is, moves along the rotating shaft 2 of the barrel 1 . At this time, the film forming mechanism 43 is operated to form a film. Moreover, it is desirable to operate the knocker 50 that gives impact to the barrel 1 or the vibrator 50 that gives vibration. When a thin film having a sufficient thickness is formed while the raw material powder 42 moves from one end face of the barrel 1 to the other end face, preparations for directing the raw material powder 42 to the powder recovery port 30 are completed. If the film thickness of the thin film is insufficient, the direction of rotation is reversed to move the bottom surface 44 on the vertically downward side of the barrel 1 toward the front side of the paper, and the film formation is continued. Next, when the raw material powder 42 is returned to one end face side of the barrel 1, the direction of rotation is reversed so as to move the bottom face 44 on the vertically downward side of the barrel 1 to the other side of the paper. In this way, the rotation direction of the barrel 1 is rotated forward and reversed to obtain a desired thickness of the thin film.

(Preliminary process for collecting powder after film formation)
With the valve 29 and the second opening/closing mechanism 27 closed, the third gas system 31 and the exhaust pump 32 are used to set the pressure in the second preliminary chamber 28 to a desired pressure and replace it with a gas atmosphere. At this time, it is preferable that the pressure in the second preliminary chamber 28, the pressure in the vacuum chamber 24 and the pressure in the barrel 1 are approximately the same.

(Step of recovering powder after film formation)
The second opening/closing mechanism 27 is opened, and the film-formed powder is moved to the second preliminary chamber 28 . After the movement is completed, the second opening/closing mechanism 27 is closed. Next, the exhaust pump 32 is stopped, and the inside of the second preliminary chamber 28 is brought to the atmospheric pressure using the third gas system 31 . Next, the valve 29 is opened and the powder formed into a film is taken out from the powder recovery port 30 .

In this embodiment, it is possible to improve the stirring efficiency by adopting a continuous structure and further by adopting a mechanism that provides a spiral passage 45 in the barrel 1 where film formation is performed. Furthermore, the movement of the powder is controlled by the spiral partition 40, and the rotation speed of the barrel 1 can control the deposition time. At that time, by supplying raw material powder 42 evenly and continuously to the powder film-forming portion in the barrel 1, the film-forming efficiency is increased, and furthermore, the barrel length is switched between normal and reverse rotation of the barrel 1. The film formation productivity can be improved by making the length variable, such as by substantially lengthening the length. In addition, the inside of the barrel 1 always maintains a vacuum, and has a structure in which film formation is performed by sputtering, ion plating, ion beam, or atom beam, and the necessary gas is continuously maintained at the necessary gas pressure. . For example, it is a structure in which a pressure of 0.5 Pa is maintained by inserting argon. Further, the raw material powder is charged from atmospheric pressure, a predetermined vacuum atmosphere is created in the first preliminary chamber for holding and supplying the raw material powder, and the gas pressure is adjusted to the same gas pressure as in the barrel 1. can be continuously supplied to The raw material powder 42 put into the barrel 1 spreads according to the interval of the spiral partition 40 and exists at the bottom by gravity. Then, the film-forming component is blown from the film-forming mechanism 43 to reach the surface of the powder, and the film-forming proceeds. Since the stirring of the powder spreading in the space between the spiral partitions 40 is gentle, the powder is stirred more by applying impact or vibration, for example. The knocker vibrates around the barrel and the vibration propagates to vibrate the powder. This vibration agitates the powder and further forms a film over the entire powder. The powder in the barrel 1 gathers at the bottom of the spiral partition and moves, but in the forward rotation in which the barrel rotates in the same direction as the spiral shape, the discharged powder is discharged on the opposite side of the powder introduction. In order to maintain the vacuum in the barrel for powder supply and discharge, a separate chamber is required, but as shown in FIGS. Therefore, it is also possible to return the powder formed by forward rotation to the introduction side and discharge it by reverse rotation. Furthermore, when the raw material powder 42 is formed into a film, the angle adjustment mechanism 8 makes the barrel 1 angled within 20° in the direction in which the powder advances, thereby facilitating the movement of the powder and ensuring the introduction, movement, and discharge of the powder. can be done. If the angle of the barrel 1 exceeds 20° during film formation of the raw material powder 42, the powder may agglomerate in the spiral partition 40 and effective film formation may not be possible. It is necessary to set the angle so that the powder is widely distributed in the passage 45 between the partitions 40 while observing the fluidity of the powder. If the purpose is to discharge powder, there is no problem in making the angle greater than this.

When forming a film by sputtering with the horizontal powder surface film-forming apparatus according to this embodiment, it is preferable that Ar, Kr or Xe is introduced as a plasma generating gas and the gas pressure is between 0.01 and 10 Pa. Furthermore, when performing high-speed film formation of oxides and nitrides with a DC power supply, oxygen gas and / or nitrogen gas is added so that the pressure is 10% or less of the plasma gas pressure to generate plasma, and the powder surface to form a film. Among Ar, Kr and Xe, Ar is more preferably used. Since this has a high sputtering rate and is an inert gas, it is important not to alter the properties of the target. Furthermore, the pressure is set to 10 Pa or less. At high gas pressures exceeding 10 Pa, the atoms sputtered from the target diffuse, and furthermore, the transfer energy of the atoms decreases. Because it does. Furthermore, in normal sputtering, it is often about 0.1 to 10 W/cm ² , but it is preferable to set the cathode output to over 10 W/cm ² .

100, 200, 300, 400 Horizontal powder surface film forming device 1 Barrel 2 Rotating shaft 3 Drive motor 4 Drive shaft 5 Drive roll 6 Follower roll 7

Rotation mechanism

8, 8a, 8b Angle adjustment mechanism 9

Powder input port

10, 12, 14 , 16, 20 to 22, 33 to 37

Piping

11, 29 Valve 13 First spare chamber 15 First opening/closing mechanism 17 Second gas system 18

First gas system

19, 32 Exhaust pump 23 Pressure adjustment mechanism 24 Vacuum chamber 25 Film formation Apparatus 26 Film-forming material 27 Second opening/closing mechanism 28 Second preliminary chamber 30 Powder recovery port 31 Third gas system 40 Partition 41 Projection 42 Raw material powder 43 Film-forming mechanism 44 Bottom surface 45

Passages

46, 47 Opening 48 Heating/cooling mechanism 50 Knocker or vibrator

Claims

A laterally tilted barrel, a rotation mechanism for rotating the barrel around its main axis as a rotation axis, a pressure adjustment mechanism for maintaining the pressure in the barrel at a predetermined pressure below atmospheric pressure, and a pressure adjustment mechanism installed in the barrel. and a film forming mechanism, and a horizontal powder surface film forming apparatus for forming a thin film on the surface of the raw material powder put in the barrel while rotating the barrel,
A horizontal powder surface deposition apparatus, wherein the barrel has an inner surface of a side wall as a bottom surface, has a passage extending spirally about the rotation shaft, and the top surface of the passage is open.
The horizontal powder surface deposition apparatus according to claim 1, characterized in that said passages are provided with partitions between adjacent passages.
Is the partition a continuous spiral step partition, a continuous spiral step partition, or an intermittent spiral step partition in which a plurality of partitions are arranged in a spiral step with portions facing each other? 3. The horizontal powder surface deposition apparatus according to claim 2, wherein the partition is a combination of at least two of the three partitions.
The horizontal powder surface deposition apparatus according to any one of claims 1 to 3, wherein the passage has a projection on the bottom surface.
The horizontal powder surface deposition apparatus according to any one of claims 1 to 4, characterized by having a knocker for impacting the barrel or a vibrator for vibrating the barrel.
A powder supply mechanism that supplies the raw material powder into the barrel from one end face of the barrel, and a powder recovery mechanism that recovers the coated powder on which the thin film is formed from the other end face of the barrel. and
The powder supply mechanism has a first preliminary chamber capable of adjusting pressure and atmosphere. are connected through
The powder recovery mechanism has a second preliminary chamber capable of adjusting pressure and atmosphere, the second preliminary chamber is connected to the other end surface of the barrel via a second opening/closing mechanism, and 6. The horizontal powder surface deposition apparatus according to any one of claims 1 to 5, characterized in that it is connected to the recovery port.
7. The horizontal powder surface deposition apparatus according to any one of claims 1 to 6, wherein the rotation mechanism has a rotation speed adjuster of the barrel and a rotation direction forward/reverse switch. .
A powder supply mechanism that supplies the raw material powder into the barrel from one end face of the barrel, and a powder recovery mechanism that recovers the coated powder having the thin film formed thereon from one end face of the barrel. and
The powder supply mechanism has a first preliminary chamber capable of adjusting pressure and atmosphere. are connected through
The powder recovery mechanism has a second preliminary chamber capable of adjusting pressure and atmosphere, the second preliminary chamber is connected to one end surface of the barrel via a second opening/closing mechanism, and It is connected to the collection port,
6. The horizontal powder surface deposition apparatus according to any one of claims 1 to 5, wherein the rotation mechanism has a rotation speed adjuster of the barrel and a rotation direction forward/reverse switch. .
The horizontal powder surface deposition apparatus according to any one of claims 1 to 8, characterized by having an angle adjustment mechanism for adjusting the inclination of the main axis of the barrel.
10. The horizontal powder surface deposition according to any one of claims 1 to 9, wherein the deposition mechanism has a deposition source by a sputtering method, an ion plating method, an ion beam method or an atom beam method. Device.