JP3661211B2 - Manufacturing method and manufacturing apparatus for tubular body with film formed on inner peripheral surface - Google Patents

Description

[0001]
[Industrial application fields]
The present invention relates to a method and an apparatus for forming a predetermined film on the inner surface of a tube body such as various glass pipes, a cooling water thin tube of a nuclear power device, and a medical catheter for the purpose of protecting the peripheral surface of the tube body.
[0002]
[Prior art]
In general, film formation on the peripheral surface of a pipe body is performed by vacuum deposition.
The apparatus shown in FIG. 2 will be described as an example of such an apparatus for performing vacuum vapor deposition. This apparatus has a vacuum vessel 10 in which a film-forming tube body S2 is installed supported by a holder (not shown), A linear or rod-like vapor deposition material 9 having a length substantially the same as that of the tube S2 is disposed in the tube S2, and a DC power source 60 is connected to both ends of the vapor deposition material 9. Further, an exhaust device 80 is connected to the container 10 by piping.
[0003]
According to this apparatus, the tube body S2 is carried into the container 10 and supported by a holder (not shown), and after the vapor deposition material 9 is disposed in the tube body S2, the inside of the container 10 is kept in a predetermined state by the operation of the exhaust device 80. While the degree of vacuum is established, DC power is applied to both ends of the vapor deposition material 9 by the DC power source 60, whereby the vapor deposition material 9 is heated and vacuum-deposited on the inner peripheral surface of the tube S 2, and a desired value is applied to the inner peripheral surface of the tube S 2. A film is formed.
[0004]
[Problems to be solved by the invention]
However, in the film formation using the vacuum evaporation apparatus, when the inner diameter of the tube body S2 is small, the diameter of the vapor deposition material 9 must be small accordingly. Easy to cut along the way. In this case, since the film cannot be formed on the inner surface of the tube body, it must be replaced with a new vapor deposition material. At the time of this replacement, after the inside of the container 10 is temporarily returned to atmospheric pressure and a new vapor deposition material is installed, the container is again formed. The inside of 10 must be set to a predetermined degree of vacuum, which is troublesome and productivity is poor.
[0005]
In addition, a plasma CVD method is conceivable as a method for supplying a film forming raw material without breaking a vacuum. In this case, if the inner diameter of the tube is small, a power application electrode for generating plasma cannot be disposed in the tube. Cannot be generated in the tube, and no film can be formed on the peripheral surface of the tube. Further, even if plasma is generated outside the tube, it cannot be sent into the tube.
[0006]
Therefore, the present invention can form a film evenly or uniformly on the inner peripheral surface of a tubular body having a small inner diameter, and can be formed as needed without breaking the vacuum in the container for film formation. It is an object of the present invention to provide a method and an apparatus capable of adding a membrane raw material and thereby obtaining a tube having a film formed on the inner peripheral surface with high productivity.
[0007]
[Means for Solving the Problems]
The method for obtaining a tube formed with a film on the inner peripheral surface of the present invention that solves the above-mentioned problem is that a rod-shaped electrode is placed in a vacuum vessel and a ring-shaped electrode is disposed around the rod-shaped electrode at a predetermined interval from the electrode. The film-forming tube is connected to the ring-shaped electrode, the inside of the vacuum vessel is set to a predetermined film-forming vacuum degree, a film-forming raw material gas is introduced between the electrodes, Applying electric power for converting the gas into plasma and applying a magnetic field, the magnetic field acting together with an electric field generated between the two electrodes by applying the electric power, and generating an electromagnetic force for directing the plasma into the tube It is characterized in that a generated magnetic field is sent into the tubular body by the electric field and the magnetic field, and a film is formed on the inner surface of the tubular body under the plasma.
[0008]
Further, the manufacturing apparatus for a tubular body having a film formed on the inner peripheral surface of the present invention that solves the above problems surrounds the periphery of the vacuum container, a rod-shaped electrode installed in the container, and a predetermined distance from the electrode. A ring-shaped electrode, a holder that is connected to the ring-shaped electrode and supports the film-forming tube, a means for introducing a film-forming gas between the electrodes, and a plasma for converting the gas between the electrodes. Means for applying electric power, and means for applying a magnetic field to the plasma generated between the two electrodes, the magnetic field applying means together with the electric field between the electrodes generated by the application of electric power by the electric power applying means. A magnetic field having a direction to generate an electromagnetic force that acts to generate a plasma generated between the two electrodes into a tube supported by the holder is applied to the plasma .
[0010]
[Action]
According to the method and apparatus of the present invention, the film-forming tube is carried into the vacuum vessel and is arranged continuously with the ring electrode. Thereafter, the inside of the container is brought to a predetermined film-forming vacuum, and a film-forming source gas is introduced between the rod-shaped electrode and the ring-shaped electrode installed at a predetermined interval so as to surround the electrode. Electric power for plasma generation is applied between the electrodes, and the gas is turned into plasma. A magnetic field is applied inside the ring electrode. The magnetic field acts together with the electric field generated by the applied electric power to move the plasma generated by the application of electric power in the direction of the film-forming tube arranged continuously to the ring-shaped electrode. Enter and diffuse inside the body. In this way, film formation is performed continuously or uniformly on the peripheral surface of the tubular body under the plasma. In addition, the film forming material gas can be supplied as needed without breaking the vacuum inside the vacuum container for film formation.
[0011]
【Example】
Embodiments of the present invention will be described below with reference to the drawings.
FIG. 1 is a view showing an embodiment of a tubular body manufacturing apparatus according to the present invention. This apparatus has a vacuum vessel 1 and has a hollow rod-shaped center electrode 2 in the vessel 1 and an outer diameter substantially the same as the inner diameter of the tube to be processed so as to surround it at a predetermined distance from the electrode 2. A ring-shaped electrode 3 is provided. A ring-shaped insulator 4a is fitted between the electrodes 2 and 3. These are supported by the container 1 by a support portion (not shown). The central electrode 2 is connected to a gas supply portion 5 for the film forming raw material gas through a pipe, so that the film forming raw material gas can be blown out from the gas blowing holes 2a provided around the electrode 2 at equal intervals. . The gas supply unit 5 includes one or two or more mass flow controllers 511, 512,... And film sources gas gas sources 531, 532,. It is. A power supply unit 6 is connected to the electrodes 2 and 3. The power source unit 6 is connected to the electrode 2 on the one hand and the DC power source 6a connected to the electrode 3 via the charging switch 6h and the open / close switch 6g on the other hand, and the discharge start connected in parallel to each other in this circuit. A capacitor 6b, a film formation speed control capacitor 6c and a crowbar circuit switch 6d, a discharge start switch 6e in series with the capacitor 6b, and a film formation speed control switch 6f in series with the capacitor 6c. Instead of the power supply unit 6, a power supply circuit including a semiconductor switch such as an inverter may be used. A magnetic field applying solenoid 7 connected to a DC power source (not shown) is arranged on the outer periphery of the vacuum vessel 1 so that a magnetic field can be applied in the direction indicated by B in the figure. Although the solenoid 7 is used here, a permanent magnet may be used instead. Further, an exhaust device 11 is connected to the container 1 by piping. Further, a support holder 12 for the film forming tube body S1 is provided in front of the electrode 3. The support holder 12 is held in the container 1 by a member (not shown).
[0012]
According to this apparatus, a longitudinal magnetic field is applied to the inside of the container 1 by a solenoid 7 in the direction indicated by B in the figure. Initially, all the switches of the power supply unit 6 are opened, and the tube S1 to be processed is loaded into the vacuum vessel 1 and supported by the holder 12 and arranged continuously with the ring-shaped electrode 3. A predetermined degree of vacuum is obtained by operating the exhaust device 8. Next, a film forming source gas is introduced from the gas supply unit 5 and blown between the electrodes 2 and 3 from the gas blowing hole 2a of the center electrode 2, and a discharge start switch 6e, a film forming speed control switch 6f, and a switch 6h is closed and electric power is applied from the DC power source 6a to charge the discharge start capacitor 6b and the film formation speed control capacitor 6c. Charging is completed by opening the switches 6e, 6f and 6h. Next, the switch 6g and the discharge start switch 6e are closed, and direct current power is applied from the center electrode 2 to the ring electrode 3 by the discharge start capacitor 6b, and the introduction of the introduced film forming material gas into plasma starts. . The subsequent plasma holding is performed by applying power with the film formation speed control capacitor 6c while keeping the switch 6g closed and opening the switch 6e and closing the film formation speed control switch 6f. When the plasma discharge is stabilized, the switch 6g is opened and the crowbar circuit switch 6d is closed. After that, the connection of the capacitor 6c by closing the switches 6g and 6f and the closing of the crowbar switch 6d are alternately repeated, so that the raw material gas is continuously turned into plasma. On the other hand, as indicated by J in the figure, the electric field applied from the center electrode 2 toward the ring electrode 3 and the upper half and the lower half of the ring electrode in opposite directions as indicated by B in the figure. Due to the action of the applied magnetic field, an electromagnetic force is generated toward the processed tube body S1. Due to this electromagnetic force, the generated plasma enters and diffuses into the tubular body S1 spirally as shown in the figure, and a desired film is uniformly formed on the inner peripheral surface of the tubular body S1 under the plasma. .
[0013]
Next, a specific example of manufacturing a glass tube having a titanium (Ti) film formed on the inner peripheral surface by the method and apparatus of the present invention will be shown.
Example 1
Glass tube size to be processed, diameter 10mm (inner diameter 9mm) x length 1m
Device size and center electrode 2 Diameter 2mm x Discharge charge length 10mm
・ Ring electrode 3 diameter 8mm x discharge charge length 8mm
・ Gas blowout hole diameter 0.5mm, 4 piece film formation condition ・ Deposition vacuum degree 50mTorr
・ Discharge starting power 1 kV, 180 mA
・ Deposition rate control power 1 kV, 10 mA
・ Magnetic field strength: 100 Gauss
-Deposition source gas Titanium tetrachloride (TiCl ₄ ), 20 sccm
Deposition result / deposition time 2 sec
・ Film thickness (deposition rate) 2μm (1μm / sec)
・ Thickness uniformity ± 10%
Example 2
Glass tube size, diameter 5mm (inner diameter 4mm) x length 50cm
Device size / Center electrode 2 Diameter 1mm x Discharge charge length 10mm
・ Ring-shaped electrode 3 3mm diameter x discharge length 8mm
・ Gas blowout hole diameter 0.2mm, 4 piece film formation condition ・ Deposition vacuum degree 50mTorr
・ Discharge starting power 1 kV, 150 mA
・ Deposition rate control power 1 kV, 10 mA
・ Magnetic field strength: 100 Gauss
・ Deposition source gas Titanium tetrachloride (TiCl ₄ ), 10 sccm
Deposition result / deposition time 2 sec
・ Film thickness (deposition rate) 1.5μm (0.75μm / sec)
・ Thickness uniformity ± 10%
Example 3
Glass tube size, diameter 2mm (inner diameter 1.4mm) x length 10cm
Device size / Center electrode 2 Diameter 0.5mm x Discharge charge length 10mm
・ Ring electrode 3 diameter 1.0mm x discharge charge length 8mm
・ Gas blowout hole diameter 0.2mm, 2 pieces film formation condition ・ Deposition vacuum degree 50mTorr
・ Discharge starting power 1 kV, 120 mA
・ Deposition rate control power 1 kV, 10 mA
・ Magnetic field strength: 100 Gauss
・ Film source gas Titanium tetrachloride (TiCl ₄ ), 5 sccm
Deposition result / deposition time 2 sec
・ Film thickness (deposition rate) 1μm (0.5μm / sec)
・ Thickness uniformity ± 20%
Therefore, the diameter is 10 mm (inner diameter 9 mm) and the length is 1 m, the diameter is 5 mm (inner diameter 4 mm), the length is 50 cm, the diameter is 2 mm (inner diameter 1.4 mm), the length is about 10 cm, and the inner diameter is small. It can be seen that even a long tube can be formed uniformly or uniformly on the inner peripheral surface in a short time.
[0014]
【The invention's effect】
According to the present invention, even a tube having a small inner diameter can be formed uniformly or uniformly on the inner peripheral surface thereof, and the tube can be formed as needed without breaking the vacuum in the film forming container. It is possible to provide a method and an apparatus capable of adding a membrane raw material and thereby obtaining a tubular body having a film formed on the inner peripheral surface with high productivity.
[Brief description of the drawings]
FIG. 1 is a diagram showing a schematic configuration of an apparatus for manufacturing a tubular body having a film formed on an inner peripheral surface, which is an embodiment of the present invention.
FIG. 2 is a diagram showing a schematic configuration of an example of a conventional manufacturing apparatus for a tubular body having a film formed on an inner peripheral surface thereof.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1, 10 Vacuum container 2 Center electrode 2a Gas blowing hole 3 Ring-shaped electrode 4a Insulator 5 Film-forming raw material gas supply part 6 Power supply part 6a, 60 DC power supply 6b Discharge start capacitor 6c Film-forming speed control capacitor 6d For clover circuit Switch 6e Discharge start switch 6f Film formation speed control switch 6h Charge switch 6g Open / close switch 7 Solenoid 11, 80 Exhaust device 9 Vapor deposition material S1, S2 Film formation tube 12 Support holder for tube S1

Claims (2)

A rod-shaped electrode is installed in the vacuum container, and a ring-shaped electrode is disposed around the rod-shaped electrode at a predetermined interval from the electrode, and a film-forming tube is arranged on the ring-shaped electrode. The inside is set to a predetermined film-forming vacuum degree, a film-forming raw material gas is introduced between the two electrodes, and a power and a magnetic field are applied between the two electrodes, and the magnetic field is applied with the power. A magnetic field having a directivity for generating an electromagnetic force that works with the electric field generated between the electrodes and directing the plasma into the tube , and the generated plasma is sent into the tube by the electric field and the magnetic field. A method for producing a tube having a film formed on an inner peripheral surface, wherein a film is formed on the inner surface of the tube under the plasma. A vacuum vessel, a rod-shaped electrode installed in the vessel, a ring-shaped electrode surrounding the electrode at a predetermined interval from the electrode, a holder that supports the film-forming tube connected to the ring-shaped electrode, Means for introducing a film-forming gas between the electrodes, means for applying electric power for converting the gas into plasma between the electrodes, and means for applying a magnetic field to the plasma generated between the electrodes. The magnetic field applying means acts together with the electric field between the electrodes generated by the application of electric power by the electric power applying means, and sends the plasma generated between the electrodes into the tube supported by the holder. An apparatus for manufacturing a tubular body having a film formed on an inner peripheral surface, wherein a magnetic field having a direction for generating a force is applied to the plasma .

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