JP2004002928A - 3D hollow container thin film deposition system - Google Patents

Abstract

An apparatus for forming a thin film on the inner surface of a container by a plasma CVD method, wherein the thin film adheres to the surface of a gas introduction pipe installed in the container when forming the thin film on the inner surface of the container. We propose a thin film forming apparatus that solves the problem that the thin film peels off and mixes into the container as the number of times increases.
A gas introduction pipe (3) for introducing a raw material gas is disposed in a vacuum chamber (2) accommodating a cylindrical three-dimensional hollow container (1), and the raw material gas is introduced into the container (1a) by the gas introduction pipe (3). A film forming apparatus for forming a thin film 6 on the inner surface 1a of the three-dimensional hollow container by a plasma CVD method, wherein a surface average roughness (Ra) of a gas introduction pipe 3 for introducing a raw material gas is 5 μm or more and 50 μm or less. There is provided a thin film forming apparatus.
[Selection diagram] Fig. 1

Description

【００２５】
表１は、本発明において、実施例１、実施例２、実施例３、及び比較例１の方法において、ガス導入管３等の表面に成膜するごとに付着する薄膜６が堆積して，その後、該ガス導入管３表面等から薄膜６が部分的に剥離するまでの成膜回数を示す表である。
【００２６】
【発明の効果】
本発明により、３次元中空容器内面にプラズマＣＶＤ法により薄膜を成膜する場合に、連続して成膜を行った場合でも容器内部に設置されるガス導入管からの薄膜の剥離を長時間防止でき、剥離した薄膜が容器内に混入することを防止できる。
【図面の簡単な説明】
【図１】本発明の一実施例を示す概略図である。
【図２】本発明の一実施例のガス導入管にカバー管を設置した概略図である。
【符号の説明】
１・・・容器　　１ａ・・・容器内部　　　１ｂ・・・容器内面
２・・・真空チャンバー　２ａ・・・外部電極　２ｂ・・・天蓋
２ｃ・・・底蓋
３・・・ガス導入管（内部電極）
４・・・ガス導入管本体
５・・・カバー管
６・・・薄膜
７・・・容器口元部
８・・・治具
９・・・真空ポンプ接続口
１０・・・ガス導入口[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention forms a thin film on the surface of a three-dimensional hollow container, for example, a plastic bottle, a plastic cup, a plastic tray, a paper container, a paper cup, a paper tray, and other hollow plastic molded products by a plasma chemical vapor deposition method (plasma CVD method). Related to the device to be used.
[0002]
[Prior art]
In recent years, attempts have been made to form a thin film on the surface of a three-dimensional hollow container such as a plastic container to improve the gas barrier property, water vapor barrier property, surface wettability and the like of the container.
[0003]
One of the methods for forming these functional thin films on the inner surface of the container is as follows: an outer electrode having a cylindrical shape is an external electrode, and an internal electrode is provided in a vacuum chamber sealed by a canopy and a bottom lid. By applying a high frequency from the external electrode using a thin film forming apparatus provided with a raw material gas introduction pipe, the raw material gas filled in the plastic container is turned into plasma and a thin film is formed on the inner surface of the container. There is.
[0004]
Alternatively, a plastic container is filled by microwave irradiation using a thin film deposition apparatus having a raw material gas introduction tube in a vacuum chamber containing a cylindrical three-dimensional hollow container having no external electrodes or internal electrodes. There is also a plasma CVD method in which the raw material gas is turned into plasma and a thin film is formed on the inner surface of the container.
[0005]
For example, as shown in Japanese Patent Application Laid-Open No. 8-53117, a hollow external electrode having a shape substantially similar to the outer shape of the container and a container provided between the container and the internal electrode having a shape substantially similar to the outer shape of the container are formed. As disclosed in Japanese Patent Application Laid-Open No. 8-175528, a method is known in which both the external electrode and the internal electrode are arranged at a substantially constant distance from the surface of the container.
[0006]
In any case, when a thin film is formed on the inner surface of the container by using the plasma CVD method, it is necessary to introduce a gas introduction pipe for introducing a gas serving as a raw material into the plastic container.
[0007]
However, when a thin film is actually formed on the inner surface of the container by these methods, the thin film is formed on the inner surface of the container and simultaneously on the surface of the gas inlet tube. Then, when the film formation is repeated, there is a problem that the thickness of the thin film increases, and eventually the film deposited on the surface of the gas introduction pipe peels, and the peeled film mixes into the inside of the container.
[0008]
[Problems to be solved by the invention]
The present invention has been made to solve the above-mentioned problems of the prior art, that is, in an apparatus for forming a thin film on the inner surface of a container by a plasma CVD method, the surface of a gas introduction pipe installed inside the container is provided. We propose a thin film forming apparatus that does not cause a problem that a deposited film is separated and mixed into a container.
[0009]
[Means for Solving the Problems]
According to the first aspect of the present invention, a gas introduction pipe 3 for introducing a raw material gas is disposed in a vacuum chamber 2 containing a cylindrical three-dimensional hollow container 1, and the gas introduction pipe 3 is provided in the container 1a. Is a film forming apparatus for forming a thin film 6 on the inner surface 1a of the three-dimensional hollow container by a plasma CVD method, wherein a surface average roughness (Ra) of a gas introducing pipe 3 for introducing a raw material gas is provided. ) Is 5 μm or more and 50 μm or less.
[0010]
According to a second aspect of the present invention, in the thin film forming apparatus according to the first aspect, the gas introduction pipe 3 is composed of at least two parts, is installed inside, and the source gas actually flows through the inside thereof. A thin film deposition, characterized in that a main body 4 and a tubular cover tube 5 which is easily detachable are installed outside the main body 4, and the surface average roughness (Ra) of the cover tube 5 is 5 μm or more and 50 μm or less. Device.
[0011]
According to a third aspect of the present invention, in the thin film forming apparatus according to the first or second aspect, the surface average roughness (Ra) of the gas introduction pipe 3 is 5 μm or more and 50 μm or less, and the surface thereof is made of metal or ceramic. A thin film forming apparatus comprising a sprayed material.
[0012]
BEST MODE FOR CARRYING OUT THE INVENTION
An embodiment of the present invention will be described in detail with reference to FIGS.
[0013]
FIG. 1 shows the inside of a thin film forming apparatus of the present invention as an embodiment, in which an external electrode 2a having a cylindrical space capable of accommodating a container 1 and a canopy 2b above the external electrode 2a. The gas introduction pipe 3 is installed through the bottom cover 2c in the vacuum chamber 2 configured and arranged at the bottom with a bottom cover 2c.
[0014]
The container 1 is placed in the vacuum chamber 2, exhausted by a vacuum pump from the vacuum pump connection port 9, and the raw material gas is supplied from the tip of the gas introduction pipe 3 to the inside of the container while the inside 1 a of the container is maintained at a constant degree of vacuum. By supplying high frequency from the external electrode 2a to the container 1a, the source gas in the container 1a is turned into plasma, and the thin film 6 is formed on the container inner surface 1b.
[0015]
One of the important features of this device is that the surface roughness of the gas introduction pipe 3 installed in the container interior 1a is 5 μm or more and 50 μm or less. As described above, the adhesion between the thin film 6 adhered to the gas introduction pipe 3 and the gas introduction pipe 3 is increased by roughening the surface to an average roughness of 5 μm or more, and the thin film adhered to the gas introduction pipe 3 by repeated expansion and contraction due to heat. There is also an effect of reducing the stress that affects the gas 6, and it is possible to prevent the thin film 6 from peeling off from the surface of the gas introduction tube 3.
[0016]
However, if the surface roughness of the gas introduction pipe 3 installed in the container interior 1a is 5 μm or less, it is difficult to obtain a sufficient effect for preventing peeling. This causes a problem that the film cannot be stably formed.
[0017]
Even when the above method is used, it is necessary to periodically remove the thin film 6 formed on the surface of the gas introduction pipe 3 when performing a long-time film formation. In this case, as shown in FIG. 2, the gas introduction pipe 3 is made up of at least two parts, and is installed inside and a gas introduction pipe main body 4 through which the raw material gas actually flows, and a tube which can be easily attached and detached outside thereof. By setting the average surface roughness (Ra) of the cover tube 5 to 5 μm or more and 50 μm or less, in which the cover tube 5 is installed, the cover tube 5 can be simply replaced by a new one prepared in advance. This is preferable because film formation can be resumed in a short time.
[0018]
Next, the method of roughening the surface of the gas introduction pipe 3 is not particularly limited, but a method of roughening by sandblasting, a method of roughening by chemical etching, or the like can be used. Further, when the surface is roughened by spraying a metal or ceramic onto the surface of the gas inlet tube 3, the sprayed metal or ceramic adhered to the surface of the gas inlet tube 3 has a relatively rough surface, and The inside of the sprayed material is porous, so that stronger adhesion strength with the thin film 6 can be obtained, which is particularly preferable.
[0019]
【Example】
An embodiment of the above invention will be described below.
[0020]
<Example 1>
The container 1 was a polyethylene terephthalate container 1 having a capacity of 500 ml, and a thin film 6 of silicon oxide was continuously formed on the inner surface 1b of the container using a film forming apparatus as shown in FIG. The method for forming the film will be described. The source gas used for the film formation was a mixed gas of hexamethyldisiloxane and oxygen, and the respective flow rates were 10 sccm and 500 sccm. This mixed gas was introduced into the container interior 1a through a stainless steel gas introduction pipe 3 having a surface sandblasted and having an average surface roughness of 5 μm, and a high frequency was applied for 15 seconds at a film forming pressure of 0.5 torr and an applied power of 200 watt. Then, a film was repeatedly formed. At this time, Table 1 shows the result of examining the number of times of film formation until the thin film 6 attached to the gas introduction pipe 3 was peeled off.
[0021]
<Example 2>
A film was repeatedly formed under the same conditions as in Example 1 except that a copper gas introduction pipe 3 having a surface average roughness of 20 μm was used as the gas introduction pipe 3. At this time, Table 1 shows the result of examining the number of times of film formation until the thin film 6 attached to the gas introduction pipe 3 was peeled off.
[0022]
<Example 3>
A gas introduction pipe 3 composed of two parts as shown in FIG. 2 was prepared, and a sprayed material having an average roughness of 50 μm was attached to the surface of an aluminum cover pipe 5 by spraying aluminum. A film was repeatedly formed under the same conditions as in Example 1 except that the gas introduction pipe 3 was used. At this time, Table 1 shows the results of examining the number of film formations until the thin film 6 adhered to the cover tube 5 of the gas introduction tube 3 was peeled off.
[0023]
<Comparative Example 1>
A film was repeatedly formed under the same conditions as in Example 1 except that a gas introduction pipe 3 made of stainless steel having a surface average roughness of 3 μm was used as the gas introduction pipe 3. At this time, Table 1 shows the result of examining the number of times of film formation until the thin film 6 attached to the gas introduction pipe 3 was peeled off.
[0024]
[Table 1]

[0025]
Table 1 shows that in the present invention, in the methods of Example 1, Example 2, Example 3, and Comparative Example 1, a thin film 6 is deposited each time a film is formed on the surface of the gas introduction pipe 3 or the like. 4 is a table showing the number of film formations until the thin film 6 is partially peeled off from the surface of the gas introduction tube 3 or the like.
[0026]
【The invention's effect】
According to the present invention, when a thin film is formed on the inner surface of a three-dimensional hollow container by a plasma CVD method, peeling of the thin film from a gas introduction pipe installed inside the container is prevented for a long time even when the film is continuously formed. It is possible to prevent the peeled thin film from being mixed into the container.
[Brief description of the drawings]
FIG. 1 is a schematic diagram showing one embodiment of the present invention.
FIG. 2 is a schematic diagram illustrating a gas inlet pipe according to an embodiment of the present invention, in which a cover pipe is installed.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Container 1a ... Container inside 1b ... Container inner surface 2 ... Vacuum chamber 2a ... External electrode 2b ... Canopy 2c ... Bottom cover 3 ... Gas introduction pipe (Internal electrode )
4 gas inlet tube body 5 cover tube 6 thin film 7 container mouth 8 jig 9 vacuum pump connection port 10 gas inlet

Claims (3)

A gas introduction pipe for introducing a raw material gas is disposed in a vacuum chamber for accommodating a cylindrical three-dimensional hollow container, the raw material gas is introduced into the container by the gas introduction pipe, and plasma is introduced into the inner surface of the three-dimensional hollow container. A thin film forming apparatus for forming a thin film by a CVD method, wherein a surface average roughness (Ra) of a gas introduction pipe for introducing a source gas is 5 μm or more and 50 μm or less. 2. The thin film forming apparatus according to claim 1, wherein the gas introduction pipe is composed of at least two parts, and is provided inside and a gas introduction pipe main body through which a raw material gas actually flows, and a tubular shape which can be easily attached to and detached from the outside. Wherein the cover tube has a surface average roughness (Ra) of 5 μm or more and 50 μm or less. 3. The thin film deposition apparatus according to claim 1, wherein the gas introduction pipe has a surface average roughness (Ra) of 5 μm or more and 50 μm or less, and the surface thereof is formed of a metal or ceramic sprayed material. apparatus.

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