JP3617711B2 - Stirrer for deaeration of liquid, vacuum deaerator using the stirrer, and vacuum deposition apparatus - Google Patents

Description

表１から、撹拌子１のポーラス状非磁性体１２と容器の接触面２３ａの材質の組み合わせは、ステンレスとステンレスのように同種材質の組み合わせの場合は勿論、ステンレスとハードクロムメッキのように異種材質の組み合わせの場合も摩耗量が多いが、どちらか一方の材質が焼結金属またはセラミックスのような多孔質であると摩耗量は少ないことが分かった。
【００２７】
表２は、図１の真空脱気装置１００において、撹拌子１と容器２間に接触がある場合とない場合の脱気効果への影響を示したものである。
【００２８】
【表２】

表２から判るとおり、撹拌脱気中に容器内底部で浮遊するタイプの撹拌子では、何時までたっても脱気できず、容器底部との接触脱気が必要であることが分かる。
【００２９】
【発明の効果】
請求項１ないし４の液体の脱気用撹拌装置においては、容器と撹拌子との接触部分のいずれか一方の材質を多孔質材料で構成したことにより、撹拌中において微小孔部分に液体が入って液体による潤滑が可能となり、両部材間の接触摩擦による摩耗を防ぐことができる。したがって、撹拌子と容器とが接触しても摩耗しにくいため、この分だけ強力に撹拌でき、液体の比重、粘度等に関係なく強力な撹拌脱気ができる。
【００３０】
請求項５及び６の真空脱気装置においては、撹拌子と容器とが接触する部分で液体を連続的に剪断できるため、より一層短時間で効率的に真空脱気ができる。請求項７及び８の真空蒸着装置においては、チャンバ内に予め脱気済みの液体を供給するので、チャンバ内を真空雰囲気にしてもチャンバ内で液体を発泡させずに蒸着することができる。
【図面の簡単な説明】
【図１】本発明に係る撹拌装置の一実施例の概略図である。
【図２】図１の装置に用いられている撹拌子の斜視図である。
【図３】本発明に係る真空脱気装置及び真空蒸着装置の一実施例の概略図である。
【図４】従来の撹拌装置の概略図である。
【図５】従来の真空脱気装置の概略図である。
【符号の説明】
１ 撹拌子
２ 脱気タンク（容器）
３ 撹拌モータ（回転磁界発生手段）
４ 液体供給装置
５ 真空排気装置
１０ 撹拌装置
１１ 永久磁性体
１２ ポーラス状非磁性体
２１ タンク上板
２２ 筒
２３ａ 接触面
４１ ヘッドタンク
Ａ 液体
Ｂ キャリア液
Ｃ 保護液
Ｄ 液体
Ｅ オイルマスク用マージンオイル
Ｆ フィルム
１００ 真空脱気装置
１０１ 真空チャンバ
１１０ 真空ポンプ
２００ 真空蒸着装置[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a stirrer capable of sufficiently degassing a gas dissolved in a liquid as well as stirring a liquid, a vacuum deaerator using such a stirrer, and a vacuum deposition apparatus. Is.
[0002]
[Prior art]
As a conventional liquid stirring apparatus, one described in JP-A-3-229630 shown in FIG. 4 is known. As is well known, this apparatus is widely used in physics and chemistry experiments, etc., and generates a rotating magnetic field in a stator 204 provided outside the container with respect to a rotor 202 introduced into the container 201 into which liquid A has been injected. Then, by rotating the rotor 202, the liquid A is stirred by a pair of stirring blades 202b provided at both ends of the rotor 202. That is, the rotor 202 is provided with a through hole 202a at the center thereof, and the liquid A flows from the through hole between the rotor 202 and the bottom surface 201a of the container 201 by the rotation of the rotor as indicated by an arrow. The liquid A moves in the outer circumferential direction of the rotor 202 by centrifugal force, gives buoyancy to the rotor, and balances with the suction force by the stator 204. Therefore, the liquid is agitated by continuously rotating the rotor without contacting the bottom surface 201a.
[0003]
Japanese Utility Model Publication No. 4-48531 proposes the apparatus shown in FIG. 5 in order to promote degassing from the liquid during the stirring.
[0004]
As shown in FIG. 5, this device opens the sealing plug 308a and injects a predetermined carrier liquid B into the liquid tank 308 so as to leave a space S in the upper part, and then closes the sealing plug 308a again and places it on the cradle 301. When the preparation for injecting the liquid D such as water or oil into the cradle 301 is completed, the switching valve 312 is switched to the vacuum pump 311 side to operate the vacuum pump 311, and at the same time, the heater 302, the high-frequency oscillator 303 and the motor 305 are turned on. It is made to operate. As a result, the upper space S of the tank 308 is depressurized by the vacuum pump 311, while the carrier liquid B is heated by the heat from the heater 302, and the solubility of gas such as oxygen dissolved therein is lowered. To do. At the same time, the carrier liquid B is vigorously stirred in response to the rotational stirring of the stirrer 309 by the rotating magnetic field from the permanent magnet 306 and the vibration from the ultrasonic vibrator 304 via the liquid L, and the dissolved gas inside Emissions are promoted.
[0005]
[Problems to be solved by the invention]
However, in order to avoid wear due to contact rotation between the stirrer and the container, the above-described conventional stirrer must balance the buoyancy due to the rotation of the stirrer and the attractive force of the magnet by adjusting the rotation speed, and strong agitation. It was impossible to stir using a stirrer equipped with a large and powerful magnet to perform the above. In addition, since the balance position from the bottom of the container differs depending on the specific gravity and viscosity of the liquid, there is also a problem that the rotational speed of the stirring bar must be adjusted depending on the type of liquid. Therefore, the vacuum degassing apparatus using this stirring device has a problem that it takes time to degas because the liquid in the stirring device is insufficiently stirred. In order to eliminate this drawback, the device described in the above Japanese Utility Model Publication No. 4-48531 is supplemented with a heating device and an ultrasonic vibration device in order to compensate for insufficient stirring. was there.
[0006]
The present invention has been made in view of the above problems, and by using a stirrer that does not easily wear, the liquid can be stirred strongly regardless of the type of liquid, and vacuum degassing can be efficiently performed by this powerful stirring. It is an object of the present invention to provide a liquid deaeration stirrer, a vacuum deaerator using the stirrer, and a vacuum vapor deposition apparatus.
[0007]
[Means for Solving the Problems]
In order to achieve the above object, the liquid degassing stirrer of the present invention is provided with a stirrer made of a magnetic material for stirring the liquid in a container formed of a non-magnetic material, on the outside of the bottom surface of the container. a stirring device for degassing liquid rotating the stirrer by the rotating magnetic field generating means provided, the stirrer rotates while in contact with the bottom surface of said container, said stirrer or the container at the contact portion Any one of these is formed of a porous material having a large number of pores. In this case, the porous material is preferably an aggregate of particles having a particle size of 0.01 to 100 μm, and is preferably a ceramic or a sintered metal. The stirrer preferably has a rectangular parallelepiped shape.
[0008]
The vacuum degassing apparatus of the present invention includes a container for the liquid degassing stirrer, a liquid supply device, a vacuum exhaust device for maintaining the inside of the container at a predetermined degree of vacuum, and a liquid discharge device. It is characterized by connecting. In this case, it is preferable that the liquid supply device includes a flow rate adjusting device that can supply the liquid at a predetermined flow rate in a state where the inside of the container is maintained at a predetermined vacuum degree.
[0009]
The vacuum vapor deposition apparatus of the present invention has a film running means and a vapor deposition material evaporation source for the film in a vacuum chamber, and a vacuum vapor deposition apparatus in which a pressure reducing means for making the inside of the chamber a reduced pressure atmosphere is connected to the chamber. The vacuum degassing apparatus according to claim 6 is connected to the chamber. The vacuum evaporation apparatus includes an input / output device that detects a deaeration state of the liquid by the vacuum deaeration device and outputs an operation command to the vacuum deaeration device so as to maintain a predetermined degree of vacuum. What has is preferable.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
DESCRIPTION OF EXEMPLARY EMBODIMENTS Hereinafter, preferred embodiments of the invention will be described with reference to the drawings illustrating an example thereof.
[0011]
FIG. 1 is a schematic explanatory diagram of a vacuum degassing apparatus 100 of the present invention in which a liquid degassing stirring apparatus 10 of the present invention is incorporated.
[0012]
First, the stirrer 10 will be described. The stirrer 10 has a liquid A inside, a deaeration tank 2 in which the stirrer 1 is charged at the bottom, and a stirrer motor that rotates the stirrer 1 by a rotating magnetic field. 3. As shown in FIG. 2, the stirrer 1 is formed by laminating a nonmagnetic body 12 having a large number of holes on the lower surface of a permanent magnetic body 11, and the nonmagnetic body 12 has a thickness of 0.01 to 100 μm. What is an aggregate | assembly of particle | grains is preferable, and specifically, a well-known zirconia type | system | group, an alumina type ceramic, and a copper-type sintered metal are mentioned. The holes on the surface of the non-magnetic body 12 are not required to penetrate, and any holes may be used as long as there are holes on the surface. As the outer shape of the stirring bar, for example, a rectangular parallelepiped or a cube having a shape having many contact surfaces with the bottom of the container and having a stirring effect is preferable. In addition, the permanent magnetic body 11 itself may be porous. In this case, a sintered magnet such as summarium cobalt or neodymium is preferable.
[0013]
The deaeration tank 2 is integrally formed in a liquid-tight state with a tank upper plate 21 and a tank lower plate 23 on the upper and lower sides of the cylindrical body 22. The tank upper plate 21 includes a liquid A injection pipe 42 and an exhaust pipe 53. Is connected. The material of the tank upper plate 21, the tank lower plate 23, and the cylinder 22 is not particularly limited as long as the tank maintains its shape even when the inside of the tank is depressurized to a vacuum and does not transmit air into the tank. As for the configuration, the tank upper plate 21, the tank lower plate 23, and the cylinder 22 may be integrated, or may be made of glass or synthetic resin. In order to see the bubbles generated inside by the rotation of the stirring bar 1, a transparent one is preferable. The agitating motor 3 is a known motor composed of a magnet 31 and a motor 32 that rotates the magnet 31, and is composed of a magnet 31 made of a sintered metal made of Samarium Cobalt and a motor 32 that rotates the magnet 31. ing. The vacuum deaerator 100 is different from the agitator 10 described above in that a liquid supply unit 4 including a liquid A head tank 41, a liquid supply pipe 42, and a flow rate adjustment valve 43, a vacuum pump 51, a leak valve 52, and an exhaust pipe 53. Are connected to an exhaust unit 6 composed of a drain pump 61 and a drain pipe 62. The tank upper plate 21 includes a liquid supply pipe 42 of the liquid supply unit 4 and an exhaust unit 5 of the exhaust unit 5. An exhaust pipe 53 is connected, and an exhaust pipe 62 of the exhaust unit 6 is connected to the tank lower plate 23. The flow rate adjusting valve 43 adjusts the injection amount of the liquid A into the deaeration tank 2 while the deaeration tank 2 is maintained at a predetermined degree of vacuum. The leak valve 52 stops the vacuum pump 51. In this case, a predetermined amount of outside air is introduced into the deaeration tank 2 to keep the degree of vacuum inside the deaeration tank 2 constant. An optical liquid level sensor (not shown) is provided in the vicinity of the deaeration tank 2.
[0014]
Next, the operation of the stirring device 10 and the vacuum deaeration device 100 configured as described above will be described.
[0015]
First, the stirring device 10 rotates the magnet 3 from below the tank lower plate 23 to generate a rotating magnetic field with respect to the stirring bar 1 submerged in the deaeration tank 2. The stirrer 1 rotates while the non-magnetic body 12 portion is in contact with the contact surface 23a to stir the liquid A. At this time, although the reason is not clear, when the bottom surface of the stirring bar 1 rotates while contacting the contact surface 23a, unlike the conventional stirring device, a very active foaming phenomenon occurs from the contact point, and the liquid A is stirred. Defoaming from the liquid is promoted. In this case, there is a concern about abrasion of the stirrer due to contact between the stirrer 1 12 and the contact surface 23a. However, since the nonmagnetic body 12 of the stirrer is made of a porous material, its minute amount during stirring is reduced. Liquid enters the hole and lubrication with the liquid becomes possible, and wear due to contact friction with the bottom of the container is prevented. Therefore, stirring can be strengthened by this amount without being influenced by the stirring conditions such as the rotational speed described above, and a strong stirring and deaeration action can be obtained.
[0016]
Next, the vacuum degassing device 100 is such that the leak valve 52, the adjustment valve 43, and the drainage pump 61 are first closed with respect to the stirring device 10, and the vacuum pump 51 is operated to start depressurization in the degassing tank 2. To do. When the pressure reduction is completed, the flow rate adjustment valve 43 is opened and the liquid A is supplied into the deaeration tank 2. When a predetermined amount of liquid A enters the degassing tank 2, the flow rate adjusting valve is closed and the agitation motor 3 is rotated, and the agitator 1 in the tank is rotated by the rotating magnetic field to agitate the liquid A. At this time, the stirring action by the rotor 1 and the defoaming action by the foaming phenomenon are as described above. When no bubbles are generated from the liquid A, the rotation is stopped. After opening the leak valve 52 and releasing the deaeration tank 2 to the atmosphere, the drainage pump 61 is operated to send defoamed stirring liquid A to a device that requires defoamed margin oil such as a vacuum vapor deposition apparatus. . That is, the vacuum deaerator of the present invention can add sufficient agitation to the liquid to be supplied to the next step and can also deaerate by using the agitation device.
[0017]
FIG. 3 is a schematic view of a vacuum deposition apparatus 200 using the vacuum degassing apparatus 100 described above. In the figure, two units denoted by reference numeral 100 are the vacuum deaeration device described above, and in each head tank 41, protection for protecting the vapor deposition material 103 deposited on the surface of the film F in the vacuum chamber 101 described later. Liquid C and margin oil E for oil mask are injected. These two units of the vacuum degassing apparatus 100 are connected to the vacuum chamber 101 by respective supply pipes 62 and can be supplied to the surface of the film F from the respective supply ports 108a and 108b.
[0018]
The inside of the vacuum chamber 101 of the vacuum deposition apparatus 200 is divided into two chambers 101a and 101b by a wall 102. In the chamber 101a, a film F unwinding device 107, a can 105 that is a guide roller for the unwound film and is also a cooling device, and a film F winding device 109 are provided. The can 105 is rotatably provided at a position where a part of the outer peripheral surface of the can 102 protrudes from the chamber 101a to the chamber 101b through the gap of the wall 102, and a coolant such as cooling water can be circulated therein. Yes.
[0019]
On the other hand, in the chamber 101b, for example, a crucible furnace 104 in which the vapor deposition material 103 such as zinc or copper is accommodated is provided in a positional relationship facing the lower peripheral surface of the can 105. In this crucible furnace 104, the vapor deposition material 103 is melted and evaporated by a resistance heating device (not shown). As a means for melting and evaporating the vapor deposition material 103, for example, a high-frequency dielectric heating device or a heating device such as an electron beam may be used in addition to the resistance heating device. In addition, one crucible furnace 104 is provided in this embodiment, but two or more crucible furnaces 104 may be provided.
[0020]
110 is a vacuum pump for making the inside of the vacuum chamber 101 into a reduced pressure atmosphere, and is constituted by a combination of, for example, a rotary pump, a mechanical booster pump, a turbo pump, an oil diffusion pump, a cryopump and the like.
[0021]
Although not shown, the vacuum chamber 101 is provided with an opening / closing door with a close seal mechanism for loading and unloading the film F into the chamber so that the vacuum in the chamber can be maintained during operation. .
[0022]
According to this vacuum vapor deposition apparatus, the film F unwound from the unwinding apparatus 107 is provided with oil mask oil E that has been sufficiently degassed from the supply port 108a on the surface of both ends thereof. After that, while being cooled by the can 105, the vapor deposition material 103 evaporated from the crucible furnace 104 is vapor-deposited on the surface, and then a protective liquid C for protecting the vapor deposition material 103 deposited is applied from the supply port 108b and applied. And wound by the winding device 109.
[0023]
The vapor deposition control apparatus 220 that controls the vacuum vapor deposition apparatus 200 is provided with a program controller (not shown), thereby controlling the vacuum vapor deposition apparatus. The vapor deposition control device 220 is provided with an input / output device 221 for issuing a liquid sending command after confirming that the degassing is completed with respect to the vacuum degassing device 100. The input / output device 221 performs overall control of the vacuum degassing device 100 by the vapor deposition control device 220 according to the state of the vacuum vapor deposition device 200.
[0024]
【Example】
In the vacuum degassing apparatus 100 of FIG. 2, zirconia ceramics are used as the porous nonmagnetic body 12 of the stirrer 1, the tank lower plate 23 is made of stainless steel, and the cylinder 22 is made of transparent polycarbonate. The contact surface 23a of the tank lower plate 23 that is in contact with the stirring bar 1 was plated with 30 μm of chrome. Further, the magnet 31 was made of Samarium Cobalt, which is a sintered magnet, and the contact area with the tank lower plate contact surface 23a was 4 cm 2 with a length of 2 cm and a width of 2 cm, and a rectangular parallelepiped shape was used. And the adjustment valve 43 uses what can be remotely adjusted arbitrarily in the range of 0-500 CC / min in the state where the deaeration tank 2 is decompressed, the vacuum pump 51 is a rotary pump, and the liquid discharge pump 61 is a plunger pump. It was used. Moreover, the oil E for oil masks used the fluorine oil.
[0025]
In the vacuum deaeration device 100 configured as described above, when the oil mask oil E is stirred for a predetermined time by the stirring device 10, the difference in the amount of wear due to the difference in the material combination of the contact portion between the container and the stirring bar is shown. The following is shown in Table 1.
[0026]
[Table 1]

From Table 1, the combination of the material of the porous nonmagnetic body 12 of the stirrer 1 and the contact surface 23a of the container is different from the combination of the same kind of materials such as stainless steel and stainless steel, as well as the stainless steel and hard chrome plating. In the case of a combination of materials, the amount of wear is large, but it has been found that the amount of wear is small if either one of the materials is porous such as sintered metal or ceramics.
[0027]
Table 2 shows the influence on the deaeration effect with and without contact between the stirring bar 1 and the container 2 in the vacuum deaerator 100 of FIG.
[0028]
[Table 2]

As can be seen from Table 2, it can be seen that the type of stirrer that floats at the bottom of the container during stirring and deaeration cannot be degassed at any time, and contact deaeration with the bottom of the container is necessary.
[0029]
【The invention's effect】
In the liquid degassing stirrer according to any one of claims 1 to 4, since the material of one of the contact portions between the container and the stirrer is made of a porous material, the liquid enters the micropores during stirring. Therefore, it is possible to lubricate with a liquid and to prevent wear due to contact friction between both members. Therefore, even if the stirrer and the container are in contact with each other, they do not easily wear, and therefore, the stirring can be performed with this much strength, and powerful stirring and deaeration can be performed regardless of the specific gravity, viscosity, etc.
[0030]
In the vacuum deaeration apparatus according to the fifth and sixth aspects, since the liquid can be continuously sheared at the portion where the stirrer and the container are in contact with each other, the vacuum deaeration can be efficiently performed in a shorter time. In the vacuum deposition apparatus according to the seventh and eighth aspects, since the liquid deaerated in advance is supplied into the chamber, the liquid can be deposited without foaming in the chamber even in a vacuum atmosphere.
[Brief description of the drawings]
FIG. 1 is a schematic view of an embodiment of a stirring device according to the present invention.
FIG. 2 is a perspective view of a stirring bar used in the apparatus of FIG.
FIG. 3 is a schematic view of an embodiment of a vacuum degassing apparatus and a vacuum deposition apparatus according to the present invention.
FIG. 4 is a schematic view of a conventional stirring device.
FIG. 5 is a schematic view of a conventional vacuum degassing apparatus.
[Explanation of symbols]
1 Stirrer 2 Deaeration tank (container)
3 Stirring motor (rotating magnetic field generating means)
4 Liquid supply device 5 Vacuum exhaust device 10 Stirrer 11 Permanent magnetic body 12 Porous nonmagnetic body 21 Tank upper plate 22 Tube 23a Contact surface 41 Head tank A Liquid B Carrier liquid C Protective liquid D Liquid E Margin oil F for oil mask Film 100 Vacuum deaerator 101 Vacuum chamber 110 Vacuum pump 200 Vacuum deposition apparatus

Claims (8)

For deaeration of liquid, a stirrer made of a magnetic material that stirs a liquid is provided in a container formed of a non-magnetic material, and the stirrer is rotated by a rotating magnetic field generating means provided outside the bottom surface of the container a stirring device, the stirring bar rotates while in contact with the bottom surface of the vessel, one of the stirrer or the container at the contact portion is formed of a porous material having a large number of pores on the surface A stirrer for deaeration of liquid, characterized in that 2. The liquid degassing stirrer according to claim 1, wherein the porous material is an aggregate of particles having a particle diameter of 0.01 to 100 [mu] m. The liquid degassing stirrer according to claim 1 or 2, wherein the porous material is ceramic or sintered metal. The stirring device for degassing a liquid according to any one of claims 1 to 3, wherein the stirrer has a rectangular parallelepiped shape. 5. The liquid degassing stirrer according to claim 1, wherein the liquid supply device, a vacuum exhaust device for maintaining the inside of the container at a predetermined degree of vacuum, and discharge of the liquid are provided. A vacuum degassing apparatus characterized by being connected to an apparatus. 6. The vacuum degassing apparatus according to claim 5, wherein the liquid supply device includes a flow rate adjusting device capable of supplying the liquid at a predetermined flow rate in a state where the inside of the container is maintained at a predetermined degree of vacuum. A vacuum vapor deposition apparatus having a film running means and a vapor deposition material evaporation source for the film in a vacuum chamber, and a vacuum decompression device connected to the chamber for reducing the pressure in the chamber. Item 7. A vacuum vapor deposition apparatus comprising the vacuum degassing apparatus according to Item 5 or 6 connected thereto. An input / output device that detects a deaeration state of the liquid by the vacuum deaeration device and outputs an operation command so as to maintain a predetermined degree of vacuum with respect to the vacuum deaeration device. 7. Vacuum deposition apparatus.

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