JP2004238701A - Ion-plating apparatus and deposition method using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an ion-plating apparatus which stabilizes the evaporation of a deposition material, performs uniform deposition and enables effective use of the deposition material, and a deposition method using the same. <P>SOLUTION: The ion-plating apparatus is equipped with at least a vacuum chamber wherein a deposition target is located, a plasma gun, a revolver for revolving the deposition material located inside the vacuum chamber so that it is uniformly exposed to plasma beam discharged from the plasma gun and a heating means for heating the deposition material. The deposition method using the ion-plating apparatus comprises a step wherein the deposition material is heated by the heating means to remove moisture and a step wherein the deposition material is exposed to the plasma beam discharged from the plasma gun and evaporated to form a thin film on the deposition target while revolved by the revolver. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an ion plating apparatus capable of forming a stable and uniform film, and a film forming method using the same.
[0002]
[Prior art]
[Patent Document 1] Japanese Patent Application Laid-Open No. 2000-144390 Japanese Patent Laid-Open Publication No. 2000-144390 A plasma beam generated by a plasma gun is converged and drawn into a vacuum chamber, and this plasma beam is irradiated on a film forming material by a magnetic field to evaporate the film forming material. Conventionally, an ion plating apparatus that forms a thin film by being ionized when passing through the above-described plasma beam and colliding with a film-forming object has been conventionally used. Such an ion plating apparatus has an advantage that a film forming material can be evaporated and ionized by a plasma gun, and that the formed thin film has high adhesion strength.
[0003]
[Problems to be solved by the invention]
However, for example, a sintered body of an inorganic material such as silicon oxide used as a film-forming material of an ion plating apparatus easily absorbs moisture, and a film-forming material provided in a vacuum chamber absorbs moisture. In the case of absorption, there are problems that the time until the start of evaporation by the plasma gun becomes longer and that the power supplied to the plasma gun needs to be increased.
Further, in a conventional ion plating apparatus, since a plasma beam is irradiated to a film forming material from a certain direction, only a portion or a surface to which the plasma beam is applied is partially reduced, and the plasma beam is irradiated as the film forming material evaporates. The surface of the film-forming material hit by the surface becomes rough and irregular. For this reason, there is also a problem that the variation in the flying direction of the evaporated film-forming material becomes large and the film-forming property is reduced.
[0004]
Furthermore, when the film-forming material is used in a sandwiched state, a part of the film-forming material is irradiated with the plasma beam from a certain direction as described above. There is also a problem in that the film-forming material is dropped and the utilization efficiency of the film-forming material is reduced.
The present invention has been made in view of such circumstances, and has an ion plating apparatus capable of stably evaporating a film forming material, forming a uniform film, and effectively using the film forming material. It is another object of the present invention to provide a film forming method using the same.
[0005]
[Means for Solving the Problems]
In order to achieve such an object, an ion plating apparatus of the present invention includes a vacuum chamber in which a film-forming target is disposed, a plasma gun, and a film-forming material disposed in the vacuum chamber. The apparatus is configured to include at least a rotating device for rotating in a plasma beam irradiated from the plasma gun and a heating unit for heating a film-forming material.
As a preferred embodiment of the present invention, the rotating device is configured to rotate the film-forming material on an axis forming an angle in a range of 80 to 100 ° with respect to a plasma beam applied to the film-forming material. .
As a preferred embodiment of the present invention, the rotating device includes a pair of holding members rotatable coaxially in a state where the film forming material is held, and the heating unit is configured to rotate the film forming material held by the holding member. The configuration was such that it was arranged to heat from the outside.
[0006]
As a preferred embodiment of the present invention, the rotating device has a rod-shaped body or a cylindrical body that can hold a film-forming material on a peripheral surface and is rotatable around an axial direction, and the rod-shaped body and the cylindrical body are The resistance heating element was formed, or the resistance heating element was provided.
Further, the present invention provides a film forming method using any one of the above ion plating apparatuses, wherein a step of heating the film forming material by the heating means to remove moisture contained in the film forming material, A step of irradiating the film-forming material with a plasma beam from the plasma gun and evaporating the film-forming material while the film-forming material is rotated by the rotating device to form a thin film on the film-forming target.
In a preferred embodiment of the present invention, the film forming material is configured to use a material containing a conductive material in a range of 10% by weight or less.
[0007]
In the present invention, since the moisture contained in the film-forming material is removed by the heating means, and the film-forming material is exposed to the plasma beam irradiated from the plasma gun while being rotated by the rotating device, The film forming material is uniformly reduced without any irregular surface.
[0008]
BEST MODE FOR CARRYING OUT THE INVENTION
Next, embodiments of the present invention will be described with reference to the drawings.
FIG. 1 is a drawing showing the configuration of an embodiment of the ion plating apparatus of the present invention. In FIG. 1, an ion plating apparatus 1 of the present invention is a take-up hollow cathode type ion plating apparatus, in which a vacuum chamber 2 partitioned by a partition plate 3 into a deposition object transfer chamber 2A and a deposition chamber 2B. And a pressure gradient type plasma gun 10 disposed at a predetermined position of the film forming chamber 2B (left side wall of the film forming chamber in the illustrated example). A supply roll 4a, a take-up roll 4b, a coating drum 5, and a vacuum exhaust port 6 for a long object S are disposed in the object transfer chamber 2A. A rotating device 7 for the film forming material T, a heating device 8 for the film forming material T, and an anode magnet 9 are provided below. The pressure gradient type plasma gun 10 provided in the film forming chamber 2B has a converging coil 11, a sheet magnet 12, and an inert gas (carrier gas) such as an argon gas to the pressure gradient type plasma gun 10. A valve 13 for adjusting the supply amount is provided, and a vacuum exhaust port 14 and a reaction gas supply port 15 are provided in the film forming chamber 2B.
[0009]
FIG. 2 is a diagram for explaining the rotating device 7 and the heating device 8 of the film forming material T described above. 2, the rotating device 7 includes driving bases 7a, 7a and a pair of rotating arms 7b, 7b rotatably projecting from the driving bases 7a. The driving bases 7a, 7a are separated in the direction of arrow a. The rotating arms 7b, 7b are rotatable coaxially. Then, by moving the drive bases 7a, 7a, the film forming material T (in the illustrated example, having a cylindrical shape) can be mounted between the rotary arms 7b, 7b. In this state, the film forming material T can be rotated by rotating the rotary arms 7b, 7b in the same direction. The rotation axis of the film-forming material T by the rotating arms 7b, 7b is set so as to form an angle in the range of 80 to 100 ° with respect to the plasma beam applied to the film-forming material T. The heating device 8 heats the rotating film-forming material T sandwiched by the rotating device 7 from the outside, and is disposed near the lower portion of the film-forming material T. As the heating device 8, a resistance heating body such as an electric heating heater or an infrared lamp can be used.
[0010]
FIG. 3 is a diagram for explaining another example of a rotating device and a heating device for the film forming material T. In FIG. 3, the rotating device 7 'has driving bases 7'a, 7'a, and the heating device 8' has a cylindrical resistance heating element 8'a, which is connected to the driving base 7 '. 'A, 7'a is rotatable by being bridged between rotation engaging portions (not shown). Wiring (not shown) for supplying electricity to the installed resistance heating element 8a is provided on the driving bases 7'a and 7'a. Then, a cylindrical resistance heating element 8'a is inserted into a hollow portion of the film-forming material T formed into a cylindrical shape, and both ends of the resistance heating element 8'a are illustrated by driving bases 7'a and 7'a. The film-forming material T is rotatable by mounting the film-forming material T between the rotation engaging portions not to be mounted. The rotation axis of such a film forming material T is set so as to make a degree in the range of 80 to 100 ° with respect to the plasma beam irradiated on the film forming material T. Further, by supplying a current to the resistance heating element 8'a, the film-forming material T can be heated from the inside. The resistance heating element 8'a can be formed using a high melting point material such as tungsten, tantalum, molybdenum, and platinum. Further, the resistance heating body 8'a may be one in which the above-described resistance heating material is disposed in a cylindrical body formed of another material. The shape of the resistance heating element 8'a may be a rod shape or the like in addition to the cylindrical shape.
[0011]
In the ion plating apparatus 1 of the present invention as described above, the film forming material T can be heated by the heating device 8, whereby the moisture contained in the film forming material T can be removed. Further, the plasma beam generated by the pressure gradient plasma gun 10 is converged by the converging coil 11, guided to the magnetic field formed by the sheet magnet 12 and the anode magnet 9, and irradiated to the film forming material T. Since the film forming material T is rotated by the rotating device 7 with a rotation axis forming an angle in the range of 80 to 100 ° with respect to the irradiated plasma beam, the film formation material T is uniformly exposed to the plasma beam, and the reduction due to evaporation is uniform. As a result, the surface irradiated with the plasma beam is always in a regular state.
[0012]
Next, a film forming method using the above-described ion plating apparatus 1 of the present invention will be described.
First, the film forming material T mounted on the rotating device 7 is heated by the heating device 8 to remove moisture contained in the film forming material T. The heating temperature of the film forming material T by the heating device 8 is preferably set to a temperature at which moisture is removed by evaporation, for example, about 120 to 150 ° C. This heating of the film forming material T is preferably performed while rotating the film forming material T by the rotating device 7. The film forming material T to be used, silicon oxide _{(SiO x (1 ≦ x ≦} 2)), magnesium oxide, indium tin oxide (ITO), silicon nitride _(Si x _{N y)} silicon oxynitride _{(Si x O} y N _z ) and the like. Further, it is preferable to use a material containing a conductive material in a range of 10% by weight or less as the film-forming material T, because the evaporation of the evaporation material by the plasma gun becomes easy. B (boron), P (phosphorus), and the like can be given as examples of the conductive material contained in the film forming material T. The rotation speed of the film-forming material T by the addition rotation device 7 can be set, for example, in a range of about 0.5 to 50 rpm.
[0013]
Next, the air in the chamber 2 is exhausted from the vacuum exhaust ports 6 and 14 to reduce the pressure to a predetermined ultimate vacuum degree, and then a predetermined reaction gas is introduced from the reaction gas supply port 15 into the film forming chamber 2B. The inside of the chamber 2 is maintained at a predetermined pressure, and the object S is run. Next, while the film forming material T is being rotated by the rotating device 7, electric power for plasma generation is supplied to the pressure gradient plasma gun 10 into which an inert gas such as an argon gas is introduced, and the anode magnet 9 is turned on. The film material is evaporated by converging and irradiating the plasma beam on the film material T located in the upper vicinity. As a result, the evaporated molecules of the film forming material are ionized by the high-density plasma and adhere to the film-forming target S to form a thin film.
[0014]
In such a film forming method, since the moisture of the film forming material T is removed before the evaporation of the film forming material T by the plasma beam, the time from the start of the plasma beam irradiation to the start of the evaporation of the film forming material T is increased. Can be shortened, and there is no need to increase the power supplied to the pressure gradient plasma gun 10 in order to continue evaporation. Furthermore, since the film-forming material T rotated in the plasma beam irradiated from the pressure gradient plasma gun 10 is uniformly exposed to the plasma beam, the reduction by evaporation becomes uniform, and the surface irradiated with the plasma beam is The surface is always in a regular state, whereby the flying direction of the film-forming material T after evaporation is stabilized, and the film-forming property on the film-forming object is stabilized. Further, even if the rotating device has a structure in which the film forming material T is sandwiched as shown in FIG. 2, since the local decrease of the film forming material T is prevented, the film forming material T may be cracked during use. , Destruction and the like are greatly reduced, and the film forming material T can be effectively used.
Note that the present invention is not limited to the above embodiments.
[0015]
【Example】
Next, the present invention will be described in more detail with reference to examples.
[Example]
As an ion plating apparatus of the present invention, a winding hollow cathode type ion plating apparatus equipped with a pressure gradient plasma gun as shown in FIG. 1 was prepared. As shown in FIG. 2, the ion plating apparatus includes a rotating device for rotating the film-forming material while holding the film-forming material therebetween, and a resistance heating device for heating the rotating film-forming material from near below. It was taken. Then, a cylindrical (diameter 200 mm, length 400 mm) silicon monoxide (SiO) having a sintering density of 90% was mounted as a film forming material on a rotating device.
[0016]
Next, while rotating the film-forming material mounted on the rotating device at a rotation speed of 2 rpm, a heating treatment was performed by the heating device so that the temperature of the film-forming material became 120 ° C. (15 minutes). The water content of the film-forming material before the heat treatment was 1% by weight, and the water content after the heat treatment was 0.5% by weight or less.
Next, a rolled biaxially stretched polyethylene terephthalate film (PET film A4100 manufactured by Toyobo Co., Ltd., thickness 100 μm) having a width of 30 cm was prepared as a film-forming body, and the corona-untreated surface side of the base film was prepared. It was mounted in a film-forming body transfer chamber as a film-forming surface. The distance (TS distance) between the base film and the film-forming material was set to about 60 cm.
Next, oxygen gas (manufactured by Taiyo Toyo Oxygen Co., Ltd. (purity: 99.9995% or more)) and nitrogen gas (manufactured by Taiyo Toyo Oxygen Co., Ltd. (purity: 99.9999% or more)) are used as additive gases during film formation. ) And argon gas (manufactured by Taiyo Toyo Oxygen Co., Ltd. (purity: 99.9999% or more)).
[0017]
Next, the pressure in the chamber was reduced to the ultimate degree of vacuum of 5.0 × 10 ⁻⁵ Pa. Next, nitrogen gas was introduced into the film formation chamber at a flow rate of 200 sccm, and oxygen gas was introduced at a flow rate of 10 sccm, while the pressure in the chamber was kept at 0.1 Pa, the substrate film was run, and argon gas was introduced at a flow rate of 15 sccm. An electric power for plasma generation was applied to the pressure gradient type plasma gun at 10 kW, and a plasma beam was converged and irradiated onto the film forming material rotating near and above the anode magnet. This plasma beam was applied at an angle of about 90 ° with respect to the rotation axis of the film-forming material. About 20 minutes after the start of the plasma beam irradiation, evaporation from the rotating film-forming material started. After that, the evaporation of the film-forming material in the rotating state was continued, the evaporated molecules were ionized by high-density plasma, and a barrier layer made of a silicon oxynitride film was formed on the base film to obtain a barrier film. The traveling speed of the base film was set so that the thickness of the silicon oxynitride film formed at the start of film formation was 100 nm. Note that sccm is an abbreviation for standard cubic centimeter per minute, and is the same in the following comparative examples.
[0018]
After such a silicon oxynitride film was continuously formed on a 100-m substrate film, the film-forming material was reduced to a diameter of about 130 mm. It was a shape.
[0019]
Further, the thickness of the silicon oxynitride film was measured for the barrier film, which is the final part of the above continuous film formation, and was found to be about 100 nm, indicating that the same film formability as that immediately after film formation was maintained. Was. Further, the oxygen permeability and the water vapor permeability of the barrier film were measured under the following conditions. As a result, the oxygen permeability was 0.3 cc / m ² / day · atm or less, and the water vapor permeability was 0.1 g / m ² / day or less, and it was confirmed that the composition had excellent barrier properties.
[0020]
Measurement of oxygen permeability Using an oxygen gas permeability measuring device (OX-TRAN 2/20 manufactured by MOCON), individual zero (Individual) for measuring the temperature at 23 ° C., the humidity at 90% RH and the background removal. (Zero) Measured under conditions with measurement.
Measurement of water vapor transmission rate The water vapor transmission rate was measured at a temperature of 40 ° C and a humidity of 100% RH using a water vapor transmission rate measuring apparatus (PERMATRAN-W 3/31 manufactured by MOCON).
[0021]
[Comparative Example 1]
A barrier film was produced in the same manner as in the example except that the heat treatment was not performed on the film forming material and the film forming material was not rotated.
In this barrier film preparation, it took about 40 minutes from the start of plasma beam irradiation to the start of evaporation of the film-forming material. Further, when a 55 m continuous film was formed on the substrate film, the film-forming material was cracked and dropped off, and the film could not be formed. Then, the thickness of the silicon oxynitride film was measured for the barrier film, which is the final part of the continuous film formation, and was found to be about 70 nm, indicating that the film formability was lower than immediately after the film formation. Further, as a result of measuring the oxygen permeability and the water vapor permeability of this barrier film in the same manner as in the example, the oxygen permeability was 2.3 cc / m ² / day · atm, and the water vapor permeability was 6.0 g / m 2. ² / day, and it was confirmed that the barrier property was inferior to the examples.
[0022]
[Comparative Example 2]
In the hollow cathode type ion plating apparatus of the embodiment, a crucible is provided instead of the rotating apparatus and the heating apparatus, and a film-forming material (water content is 1% by weight) which is not subjected to the heat treatment is placed in the crucible. Was placed. Thereafter, in the same manner as in the example, a plasma beam was converged and irradiated on the film-forming material to produce a barrier film.
In this barrier film fabrication, it took about 30 minutes from the start of plasma beam irradiation to the start of evaporation of the film-forming material. Further, the thickness of the silicon oxynitride film of the barrier film which was the last part of the continuous film formation was measured to be about 85 nm, and it was confirmed that the film formability was lower than that immediately after the film formation. The oxygen permeability and the water vapor permeability of this barrier film were measured in the same manner as in the example. As a result, the oxygen transmission rate was 1.2 cc / m ² / day · atm, and the water vapor transmission rate was 0.9 g / m ² / day, and it was confirmed that the barrier properties were inferior to the examples.
[0023]
【The invention's effect】
As described in detail above, according to the present invention, since the film-forming material is heated by the heating means to remove the contained water, the adverse effect of water when the film-forming material is evaporated by the plasma gun is eliminated, and the evaporation starts. It is possible to shorten the time required to perform the operation, and it is not necessary to increase the power of the plasma gun. In addition, since the film-forming material rotated in the plasma beam irradiated from the plasma gun is uniformly exposed to the plasma beam, the reduction by evaporation becomes uniform, and the surface irradiated with the plasma beam is always in a uniform state. In this case, the flying direction of the film-forming material after evaporation is stabilized, and the film-forming property on the film-forming object becomes stable. Further, since the local decrease of the film-forming material is prevented as described above, even when the film-forming material is used in a sandwiched state, cracking of the film-forming material during use is less likely to occur. Thus, the film forming material can be effectively used.
[Brief description of the drawings]
FIG. 1 is a drawing showing a configuration of an embodiment of an ion plating apparatus of the present invention.
FIG. 2 is a diagram for explaining a film forming material rotating device and a heating device.
FIG. 3 is a view for explaining another example of a rotating device and a heating device of a film forming material.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Ion plating apparatus 2 ... Vacuum chamber 7, 7 '... Rotating device 7a, 7'a ... Drive base 7b ... Rotating arm 8, 8' ... Heating device 8'a ... Resistance heating body 10 ... Plasma gun S ... Cover Film forming body T: Film forming material

Claims (6)

A vacuum chamber in which a film-forming object is disposed, a plasma gun, and a rotation device for rotating a film-forming material disposed in the vacuum chamber in a plasma beam irradiated from the plasma gun, An ion plating apparatus, comprising: at least heating means for heating a film forming material. 2. The ion according to claim 1, wherein the rotating device is configured to rotate the film forming material about an axis forming an angle in a range of 80 to 100 ° with respect to a plasma beam irradiated on the film forming material. 3. Plating equipment. The rotating device has a pair of holding members rotatable coaxially while holding the film-forming material, and the heating means is arranged to heat the film-forming material held by the holding member from outside. The ion plating apparatus according to claim 1, wherein the ion plating apparatus is provided. The rotating device has a rod-shaped body or a cylindrical body that can hold a film-forming material on a peripheral surface and can rotate around an axial direction, and the rod-shaped body and the cylindrical body are formed of a resistance heating body. The ion plating apparatus according to claim 1, wherein the ion plating apparatus is provided with a resistance heating element. A film forming method using the ion plating apparatus according to any one of claims 1 to 4,
Heating the film-forming material by the heating means to remove moisture contained in the film-forming material; and, while rotating the film-forming material by the rotating device, applying a plasma beam from the plasma gun to the film-forming material. A step of irradiating and evaporating to form a thin film on a film-forming object, the method comprising using an ion plating apparatus. 6. The film forming method using an ion plating apparatus according to claim 5, wherein a material containing a conductive material in a range of 10% by weight or less is used as the film forming material.

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