JPH09155177A - Liquid stirring apparatus and vacuum degassing apparatus and vacuum deposition apparatus using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To strongly stirr a liquid regardless of the kind thereof by using a stirring element hard to abrade and to also efficiently perform vacuum degassing by strong stirring. SOLUTION: A stirring element 1 stirring a liquid A is disposed in a container 2 formed from a non-magnetic material and housing the liquid A and rotated by the rotary magnetic field generating means 3 attached to the bottom surface of the container 2. The material quality of either one of the stirring element 1 and the container 2 at the contact part of the stirring element 1 with the bottom surface 23a of the container 23 is formed from a porous material 12 having a large number of pores.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field 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, and a vacuum degasser using such a stirrer. The present invention relates to an apparatus and a vacuum vapor deposition apparatus.

[0002]

2. Description of the Related Art As a conventional liquid stirring device, a device described in Japanese Patent Laid-Open No. 3-229630 shown in FIG. 4 is known. As is well known, this device is often used in physics and chemistry experiments and the like, and generates a rotating magnetic field in a stator 204 provided outside the container with respect to a rotor 202 put in a container 201 in which liquid A is injected. Then, by rotating the rotor 202, the liquid A is stirred by the 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 in the center thereof, and the liquid A is supplied from the through hole to the rotor 202 as indicated by an arrow by the rotation of the rotor.
And the bottom surface 201a of the container 201. Liquid A
Moves to the outer peripheral direction of the rotor 202 due to the centrifugal force to give buoyancy to the rotor, and balances with the suction force by the stator 204. Therefore, the liquid is agitated by the rotor continuing to rotate smoothly without contacting the bottom surface 201a.

Further, Japanese Utility Model Publication No. 4-48531 discloses that
In order to promote degassing from the liquid during the above stirring, the device of Fig. 5 is proposed.

This device, as shown in FIG.
After injecting a predetermined carrier liquid B into the liquid tank 308 so that a is opened and a space S is left in the upper part, the tight stopper 308a is again placed on the receiving table 301, and liquid such as water or oil is placed on the receiving table 301. When the preparation for injecting D is completed, the switching valve 312 is switched to the vacuum pump 311 side to operate the vacuum pump 311 and simultaneously operate the heater 302, the high frequency oscillator 303 and the motor 305. As a result, the upper space S of the tank 308 is decompressed by the vacuum pump 311, while the carrier liquid B receives heat from the heater 302 and its temperature rises, and the solubility of gases such as oxygen dissolved therein decreases. To do. At the same time, carrier liquid B
Is a stirring bar 309 due to the rotating magnetic field from the permanent magnet 306.
And the vibration from the ultrasonic oscillator 304 via the liquid L, the mixture is vigorously stirred, and the discharge of the dissolved gas inside is accelerated.

[0005]

However, in the above-mentioned conventional stirring device, in order to avoid abrasion due to contact rotation between the stirring bar and the container, the buoyancy force due to the rotation of the stirring bar and the attractive force of the magnet are adjusted by the rotation speed. It had to be balanced and it was not possible to stir with a stir bar equipped with a large and powerful magnet in order to perform strong stirring. Also,
Since the balance position from the bottom of the container varies depending on the specific gravity and viscosity of the liquid, there is also a problem that the rotation speed of the stirrer must be adjusted depending on the type of liquid. Therefore, the vacuum deaerator using this agitator has a problem that it takes time to deaerate because the liquid in the agitator is insufficiently agitated. In order to solve this drawback, the device described in Japanese Utility Model Publication No. 4-48531 has a heating device and an ultrasonic vibration device added to compensate for insufficient stirring, but it is a complicated and expensive device. was there.

The present invention has been made in view of the above problems, and by using a stirrer that is less likely to wear, it is possible to strongly stir regardless of the type of liquid, and this strong stirring allows efficient vacuum degassing. An object of the present invention is to provide a liquid stirring device, a vacuum degassing device using this stirring device, and a vacuum vapor deposition device.

[0007]

In order to achieve the above object, a liquid stirring device of the present invention is provided with a magnetic stirrer for stirring a liquid in a container formed of a non-magnetic material. A stirring device for a liquid that rotates the stirring bar by means of a rotating magnetic field generating means provided on the bottom surface of the container, wherein one of the stirring bar or the container at the contact portion between the stirring bar and the bottom surface of the container is either It is characterized by being 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 outer shape.

The vacuum deaerator of the present invention comprises: a container for the liquid stirring device; a device for supplying the liquid; a vacuum exhaust device for maintaining the inside of the container at a predetermined degree of vacuum; and a device for discharging the liquid. It is characterized by connecting. in this case,
It is preferable that the liquid supply device has 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.

The vacuum vapor deposition apparatus of the present invention has a film running means and a vapor deposition source of vapor deposition material for the film in a vacuum chamber, and a depressurizing means for connecting the chamber to a depressurized atmosphere is connected to the chamber. A vacuum vapor deposition apparatus, wherein the vacuum degassing apparatus according to claim 6 is connected to the chamber. The vacuum vapor deposition apparatus includes an input / output device that detects a degassing state of the liquid by the vacuum degassing device and outputs an operation command to the vacuum degassing device so as to maintain a predetermined degree of vacuum. Those having are preferred.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION A preferred embodiment of the present invention will be described below with reference to the drawings showing an example thereof.

FIG. 1 is a schematic explanatory view of a vacuum degassing apparatus 100 of the present invention incorporating a liquid stirring apparatus 10 of the present invention.

First, the stirrer 10 will be described.
The stirrer 10 includes a degassing tank 2 that holds the liquid A therein and has a stirrer 1 at its bottom, and a stirrer motor 3 that rotates the stirrer 1 by a rotating magnetic field. As shown in FIG. 2, the stirrer 1 is formed by laminating a non-magnetic body 12 having a large number of holes on the surface on the lower surface of a permanent magnetic body 11, and the non-magnetic body 12 has a thickness of 0.01 to 100 μm. It is preferably an aggregate of particles, and specific examples thereof include known zirconia-based or alumina-based ceramics and copper-based sintered metals. The holes on the surface of the non-magnetic body 12 are not required to be penetrated, and it is sufficient that at least the surface has holes. As the outer shape of the stirrer, a shape having a large contact surface with the bottom of the container and having a stirring effect, such as a rectangular parallelepiped or a cube, is preferable. The permanent magnetic body 11 itself may be porous, and in this case, a sintered magnet such as Samaleumu cobalt or Neody is preferable.

The deaeration tank 2 is constructed by integrally assembling the upper and lower sides of a cylindrical body 22 with a tank upper plate 21 and a tank lower plate 23, respectively. The tank upper plate 21 has a liquid A injection pipe 42 and an exhaust gas. The 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 it retains its shape even when the inside of the tank is depressurized to vacuum and does not allow air to permeate into the tank. The tank upper plate 21, the tank lower plate 23 and the cylinder 2 are also configured.
It may be integrated with 2, and may be made of glass or synthetic resin. In order to see bubbles generated inside by the rotation of the stirrer 1, a transparent one is preferable. The agitation motor 3 is a known one that includes a magnet 31 and a motor 32 that rotates the magnet 31.
It is composed of a magnet 31 made of cobalt sintered metal and a motor 32 for rotating the magnet 31. The vacuum degassing device 100 is different from the stirring device 10 described above in that the head tank 41 for the liquid A, the liquid supply pipe 42, and the flow rate adjustment valve 43 are provided.
A liquid supply unit 4 including a vacuum pump 51, a leak valve 52, an exhaust unit 5 including an exhaust pipe 53, and a drainage pump 6.
1. Connected with the exhaust part 6 composed of the drain pipe 62,
The tank upper plate 21 includes a liquid supply pipe 42 of the liquid supply unit 4.
And the exhaust pipe 53 of the exhaust unit 5 are connected to each other, and the tank lower plate 2
An exhaust pipe 62 of the exhaust unit 6 is connected to the unit 3. The flow rate adjusting valve 43 adjusts the injection amount of the liquid A into the degassing tank 2 while the degassing tank 2 is maintained at a predetermined vacuum degree, and the leak valve 52 is the vacuum pump 5.
By introducing a predetermined amount of outside air into the deaeration tank 2 when 1 is stopped, the degree of vacuum inside the deaeration tank 2 is always kept constant. The degassing tank 2
An optical liquid level sensor (not shown) is provided in the vicinity of.

Next, the stirrer 1 configured as described above
0 and the operation of the vacuum deaerator 100 will be described.

First, the stirring device 10 rotates the magnet 3 from below the tank lower plate 23 with respect to the stirrer 1 submerged in the degassing tank 2 to generate a rotating magnetic field. The stirrer 1 rotates while the non-magnetic body 12 portion is in contact with the contact surface 23a,
Stir Liquid A. At this time, although the reason is not clear, when the bottom surface of the stirring bar 1 rotates while contacting with the contact surface 23a,
Unlike the conventional stirring device, a very active foaming phenomenon occurs from the contact point, and the defoaming of the liquid A is promoted as the liquid A is stirred. In this case, the stirrer 12 and the contact surface 23a
Although there is concern that the stirrer may wear due to contact with the stirrer, the non-magnetic member 12 of the stirrer is made of a porous material, so that liquid can enter the micropores during stirring and be lubricated by the liquid. Therefore, wear due to contact friction with the bottom of the container is prevented. Therefore, the stirring can be strengthened without being affected by the stirring conditions such as the above-described number of revolutions by this amount,
A strong stirring action is obtained.

Next, the vacuum degassing apparatus 100 is different from the stirring apparatus 10 in that the leak valve 52 and the adjusting valve 4 are first provided.
3. The drainage pump 61 is closed and the vacuum pump 51 is operated to start depressurizing the deaeration tank 2. When the pressure reduction is completed, the flow rate adjustment valve 43 is opened to remove the liquid A from the degassing tank 2
Supply within. When a predetermined amount of liquid A enters the degassing tank 2, the flow rate adjusting valve is closed and the stirring motor 3 is rotated.
The stirrer 1 in the tank is rotated by the rotating magnetic field,
Stir Liquid A. The stirring action by the rotor 1 at this time and the defoaming action due to the foaming phenomenon occur as described above. The rotation is stopped when no bubbles are generated from the liquid A. Open leak valve 52 and degas tank 2
After releasing the air to the atmosphere, the drainage pump 61 is operated to send the defoamed agitated liquid A to a device requiring defoamed margin oil such as a vacuum vapor deposition device.
That is, the vacuum degassing apparatus of the present invention can perform sufficient stirring and degassing the liquid to be supplied to the next step by using the above stirring apparatus.

FIG. 3 is a schematic diagram of a vacuum vapor deposition apparatus 200 using the vacuum degassing apparatus 100 described above. In the figure,
Two units denoted by reference numeral 100 are the above-described vacuum deaeration devices, and in each head tank 41, a protective liquid C for protecting the vapor deposition material 103 vapor-deposited on the surface of the film F in the vacuum chamber 101 described later. Margin oil E for the oil mask is injected. The vacuum deaerator 100 of these two units is connected to the vacuum chamber 101 by each supply pipe 62, and each supply port 108.
It can be supplied to the surface of the film F from a and 108b.

Vacuum chamber 101 of vacuum deposition apparatus 200
The interior is partitioned by a wall 102 into two chambers 101a and 101b. Inside the chamber 101a, there are provided an unwinding device 107 for the film F, a can 105 that is a guide roller for the unwound film and is also a cooling device, and a winding device 109 for the film F. Can 105
Is a part of the outer peripheral surface from the gap of the wall 102 to the chamber 101a.
Is rotatably provided at a position overhanging from the room to the chamber 101b,
A coolant liquid such as cooling water can be circulated in the inside thereof.

On the other hand, in the chamber 101b, for example, zinc,
Crucible furnace 104 containing the vapor deposition material 103 such as copper
Are provided in a positional relationship facing the lower peripheral surface of the can 105. The crucible furnace 104 is configured to melt and vaporize the vapor deposition material 103 by a resistance heating device (not shown). The means for melting and evaporating the vapor deposition material 103 may be, for example, a high frequency dielectric heating device or a heating device such as an electron beam, in addition to the resistance heating device. Further, although one crucible furnace 104 is provided in the present embodiment, it is possible to provide two or more crucible furnaces 104.

Reference numeral 110 denotes a vacuum pump for creating a reduced pressure atmosphere in the vacuum chamber 101, such as a rotary pump, a mechanical booster pump, a turbo pump,
It is composed of a combination of an oil diffusion pump and a cryopump.

Although not shown, the vacuum chamber 101 is provided with an opening / closing door with a close contact sealing mechanism for loading and unloading the film F so that the vacuum degree in the chamber can be maintained during operation. Has become.

According to this vacuum vapor deposition device, the unwinding device 10
The film F unwound from 7 is provided with the oil mask oil E, which has been sufficiently degassed from the supply port 108a, on both end surfaces thereof to be subjected to the oil mask, and then the can 1
While being cooled by 05, the vapor deposition material 103 evaporated from the crucible furnace 104 is vapor-deposited on the surface thereof, and then the protective liquid C for protecting the vapor deposition material 103 vapor-deposited is supplied to the supply port 1
08b is applied and applied, and is wound by the winding device 109.

The vapor deposition control device 220 for controlling the vacuum vapor deposition device 200 is provided with a program controller (not shown), which controls the vacuum vapor deposition device. The vapor deposition control device 220 is provided with an input / output device 221 which issues a liquid sending command after confirming that the vacuum degassing device 100 is completely degassed. The input / output device 221 controls the entire vacuum degassing device 100 according to the state of the vacuum vapor deposition device 200 by the vapor deposition control device 220.

[0024]

EXAMPLE In the vacuum degassing apparatus 100 of FIG. 2, zirconia-based ceramics was used as the porous non-magnetic body 12 of the stirrer 1, the tank lower plate 23 was made of stainless steel, and the cylinder 22 was made of transparent polycarbonate. It was made. Further, the contact surface 23a of the tank lower plate 23 that comes into contact with the stirrer 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 having a length of 2 cm and a width of 2 cm, and a rectangular parallelepiped shape was used. As the adjusting valve 43, one which can be remotely adjusted in the range of 0 to 500 CC / min while the degassing tank 2 is depressurized is used. The vacuum pump 51 is a rotary pump and the liquid discharge pump 61 is a plunger pump. It was used. Fluorine oil was used as the oil E for the oil mask.

In the vacuum degassing apparatus 100 thus constructed, when the oil mask oil E is stirred by the stirrer 10 for a predetermined time, the amount of wear caused by the difference in the combination of the materials of the contact portion between the container and the stirrer The difference is shown in Table 1 below.

[0026]

[Table 1] From Table 1, the combination of the materials of the porous non-magnetic body 12 of the stirrer 1 and the contact surface 23a of the container is not limited to the case of stainless steel and the same kind of material such as stainless steel, but is also different between stainless steel and hard chrome plating. It was found that the amount of wear was large even when the materials were combined, but the amount of wear was small when one of the materials was porous such as sintered metal or ceramics.

Table 2 shows the influence on the degassing effect in the vacuum degassing apparatus 100 of FIG. 1 when the stirrer 1 and the container 2 are in contact with each other or not.

[0028]

[Table 2] As can be seen from Table 2, with a stirrer of the type that floats at the bottom of the container during stirring and degassing, it cannot be degassed at any time,
It can be seen that contact degassing with the bottom of the container is necessary.

[0029]

In the stirrer according to the first to fourth aspects of the invention, since the material of either one of the contact portion between the container and the stirrer is made of a porous material, liquid enters the micropores during stirring. As a result, it becomes possible to lubricate with a liquid and prevent wear due to contact friction between both members. Therefore, even if the stirrer and the container come into contact with each other, they are less likely to be worn, so that strong stirring can be performed correspondingly, and strong stirring can be performed regardless of the specific gravity and viscosity of the liquid.

In the vacuum degassing apparatus of the fifth and sixth aspects, since the liquid can be continuously sheared at the portion where the stirring bar and the container are in contact, the vacuum degassing can be performed more efficiently in a shorter time. In the vacuum vapor deposition apparatus according to the seventh and eighth aspects, since the degassed liquid is supplied into the chamber in advance, the liquid can be vapor-deposited in the chamber even when the chamber has a vacuum atmosphere without being bubbled.

[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 stirrer used in the apparatus of FIG.

FIG. 3 is a schematic view of an embodiment of a vacuum degassing apparatus and a vacuum vapor 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 device.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Stirrer 2 Degassing tank (container) 3 Stirring motor (rotating magnetic field generating means) 4 Liquid supply device 5 Vacuum exhaust device 10 Stirring device 11 Permanent magnetic body 12 Porous non-magnetic body 21 Tank top plate 22 Cylinder 23a Contact surface 41 Head tank A Liquid B Carrier liquid C Protective liquid D Liquid E Margin oil for oil mask F Film 100 Vacuum degassing device 101 Vacuum chamber 110 Vacuum pump 200 Vacuum deposition device

Claims (8)

[Claims] 1. An agitator made of a magnetic material for agitating a liquid is provided in a container formed of a non-magnetic material, and a liquid magnetic element for rotating the agitator by a rotating magnetic field generating means provided on a bottom surface of the container. A stirring device, wherein one of the stirring bar or the container at the contact portion between the stirring bar and the bottom surface of the container is formed of a porous material having a large number of holes on the surface. Liquid stirring device. 2. The porous material has a particle size of 0.01 to 1
The liquid stirring device according to claim 1, which is an aggregate of particles having a diameter of 00 μm. 3. The liquid stirring apparatus according to claim 1, wherein the porous material is ceramics or sintered metal. 4. The liquid stirring device according to claim 1, wherein the stirrer has a rectangular parallelepiped outer shape. 5. The container of the liquid agitating device according to claim 1, wherein the container is a liquid supply device, and a vacuum exhaust device is provided to maintain the inside of the container at a predetermined vacuum degree.
A vacuum deaeration device, characterized in that it is connected to the liquid discharge device. 6. The vacuum degassing device according to claim 5, wherein the liquid supply device has a flow rate adjusting device capable of supplying a predetermined flow rate of the liquid while maintaining a predetermined degree of vacuum inside the container. Qi device. 7. A vacuum chamber is provided with a film traveling means and a vapor deposition material evaporation source for the film,
A vacuum vapor deposition apparatus in which a decompression means for making a decompressed atmosphere in the chamber is connected to the chamber, wherein the vacuum deaerator according to claim 5 is connected to the chamber. Vapor deposition equipment. 8. An input / output device for detecting a degassing state of the liquid by the vacuum degassing device, and outputting an operation command to the vacuum degassing device so as to maintain a predetermined degree of vacuum. The vacuum vapor deposition device according to claim 7, which is characterized in that.