JP3993971B2 - Plastic container having gas barrier coating layer and method for producing the same - Google Patents

Plastic container having gas barrier coating layer and method for producing the same Download PDF

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Publication number
JP3993971B2
JP3993971B2 JP2000240845A JP2000240845A JP3993971B2 JP 3993971 B2 JP3993971 B2 JP 3993971B2 JP 2000240845 A JP2000240845 A JP 2000240845A JP 2000240845 A JP2000240845 A JP 2000240845A JP 3993971 B2 JP3993971 B2 JP 3993971B2
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Japan
Prior art keywords
container
plastic container
gas barrier
barrier coating
mouth
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JP2000240845A
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JP2002053119A (en
Inventor
俊三 宮崎
浩二 松島
明久 鈴木
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HOKKAICAN CO.,LTD.
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HOKKAICAN CO.,LTD.
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Description

【0001】
【発明の属する技術分野】
本発明は、ガスバリア特性を有する被覆を備える被覆プラスチック容器に関し、特にプラズマCVD手段により内面にガスバリア被膜が形成された被覆プラスチック容器及びその製法に関する。
【0002】
【従来の技術】
ポリエステル樹脂やポリオレフィン樹脂等からなるボトル等の容器が飲料、食料、エアロゾール、化粧品等の容器として一般に用いられている。これら従来のプラスチック製容器はガスバリア性が劣り酸素や炭酸ガス等のガスを透過するため、例えば炭酸飲料等の容器としては使用できない等、容器により保存する内容物は限定されるという不利があった。
【0003】
これらプラスチック製容器のガスバリア性を改良するため、プラスチック製容器の内面にガスバリア性を有する被膜を施すことが提案されており、炭素含有ガス又はシリコン含有ガスを用いたプラズマCVDによるガスバリア被膜処理が注目されている。
【0004】
従来、プラスチック製容器のプラズマCVDによるガスバリア被膜処理法に付いては種々の提案がなされており、例えば、特開平2−70059号、特開平8−509166号、特開平8−53117号等があり、膜形成方法として、処理室を構成する中空の外部電極内にプラスチック製ボトルを配置し、該ボトル内部にアースされた内部電極を兼ねる原料ガス導入管を挿入して、ボトル内部を真空に排気した後、原料ガスを供給し外部電極に高周波電圧を印加することによってプラズマを発生させボトル内壁に硬質のDLC被膜を蒸着させる方法、或いは、プラズマ発生手段としてマイクロ波を使用し、原料ガスのプラズマを励起して容器内面に軟質のポリマー被覆を形成する方法等が知られている。
【0005】
これら従来のプラズマCVD法によりガスバリア被膜を形成した場合、一般にプラスチック製容器の口部の被膜が膜厚となる傾向がある。これは、容器口部から排気して真空度を制御し原料ガスを供給しつつプラズマを発生させる方法においては一般に口部近傍に原料ガスが流れやすく、口部近傍が厚膜になり易いためである。
【0006】
そのため、炭化水素化合物を原料ガスとするカーボン被膜の場合、厚膜部は褐色の着色が目立ち、外観が悪くなる。栓やフタの取り付け部となる容器口部は、変形を防止するために肉厚に成形するが、ホットパック用のポリエチレンテレフタレート樹脂製容器の場合は、口部を結晶化温度以上に加熱して白化結晶化させ、口部の耐熱性を高めた所謂口部白化ペットボトルとして使用する。かかる口部白化した容器においては、特に、口部が白色のため被膜が薄膜でも着色が目立ち、外観が悪くなり商品性が劣る。
【0007】
【発明が解決しようとする課題】
本発明は、ガスバリア性を有する被膜を内面に形成した被覆プラスチック容器のかかる不都合を解消して、商品性を向上させた被覆プラスチック容器及びその製法を提供することを目的とする。
【0008】
【課題を解決するための手段】
上記課題を解決するため本発明においては、プラスチック製容器の内面にガスバリア被膜が形成された被覆プラスチック容器において、前記ガスバリア被膜はポリマー性アモルファスカーボンからなり、前記容器の内面のうち口部を除いて被膜が形成されていることを特徴とするので、被覆プラスチック容器の外観が改善され商品性が向上する。容器の口部は蓋や栓を配設するため特に肉厚に成形されているので、口部の内面は被覆が施されなくとも被覆プラスチック容器のガスバリア性には影響がない。又、前記ガスバリア被膜はポリマー性アモルファスカーボンからなることを特徴とするので、被覆プラスチック容器の使用の際の変形に追従して剥離やクラックを生じない被膜となり、全付着量が少ない薄膜でも実用上充分なガスバリア性が得られる。
【0009】
更に、前記被覆プラスチック容器はポリエチレンテレフタレート樹脂製であって、前記口部が白化されていることを特徴とするので、ガスバリア被膜の付着が目立つ白色口部の内面は白色を維持した被覆プラスチック容器となり商品性が向上する
【0010】
前記課題を解決するため本発明の被覆プラスチック容器の製法は、プラスチック製容器の口部の内面にプラズマ状態のガスの接近を防止するマスキング手段を設け、プラズマCVDにより前記容器の内面にガスバリア被覆処理を行うことを特徴とするので、再使用可能なマスキング手段により簡便な装置で被覆プラスチック容器の口部内面の被膜付着を防止することができる。
【0011】
【発明の実施の形態】
次に、添付の図面を参照しながら本発明の実施の形態についてさらに詳しく説明する。図1は本発明に係るプラズマCVD装置の概略を示す断面図である。
【0012】
図1において、パイレックスガラスで形成された側壁1及び隔壁3により画成される処理室4に、500mlのポリエチレンテレフタレート樹脂製ボトルである容器14を配置した底板2を下方より上昇移動せしめて、容器14を処理室4に収納する。容器14はマスキング部材15を介して容器内部が隔壁3に設けられた排気孔5と連通するように配置される。マスキング部材15は上部突出部17が排気孔5に密に挿入され、マスキング部16が容器14の口部に挿入される。マスキング部16の外径と容器14の口部内径の間隔は1mm以下の間隙となるように構成される。
【0013】
マスキング部材15は予め容器4の口部に装着した状態で容器14を底板2上に配置し底板2の上昇により突出部17を排気孔5に挿入させてもよいし、隔壁3の排気孔5にマスキング部材15を装着しておき、底板2と共に上昇する容器14の口部にマスキング部16を挿入するようにしてもよい。
【0014】
隔壁3の上方に側壁9及び上壁12により形成される排気室7が設けられ、側壁9の開口10は図示しない真空装置19に連通する。排気室7と処理室4は隔壁3に設けられた通気口6に設けられたバルブ13を介して連通している。原料ガス導入管11は上壁8にシールを介して支持され、図示しない原料タンクに接続されて容器14内部に皮膜を形成する原料となるアセチレンを供給する。原料ガスは図示しないバルブ等により原料ガス流量が所定の流量となるように制御される。マイクロ波発生装置18はUHF領域の周波数例えば2.45GHzのマイクロ波を発生する。
【0015】
次に、本実施形態における被膜形成方法について詳述する。隔壁3の排気孔5にマスキング部材15を装着した後、容器14を配置した底板12を上昇させて図に示す位置に容器14を収納し容器14の口部内面にマスキング部16を配置する。真空装置19を作動して排気室7の空気を排出し、排気孔5及び通気口6を介して容器14の内部及び処理室4を減圧する。およそ60mbarに減圧した時点でバルブ13を閉じ、更に真空装置を作動させて容器内部を0.1mbar迄減圧した。
【0016】
次いでアセチレンを原料ガス導入管11から160sccmの流量で容器14内に供給しつつ、出力400Wで2.45GHzのマイクロ波を3秒間印加した。その後、マイクロ波の印加を停止して処理室4及び容器内部を大気圧に戻し底板2を降下させて容器14を取り出した。取り出した容器14は口部内面には被膜は形成されおらず、口部内面以外の容器14の内面には膜厚約1000Åのポリマー性アモルファスカーボン被膜が形成されていた。
【0017】
かくして得られた被覆容器14のガスバリア効果はガスバリア被膜を設けない未処理のペットボトルの27〜30倍であり、ガスバリア被膜の付着量も1本の容器当たり8〜9mgで、再生容器の成形材料とするリサイクルの障害にならない値であった。
【0018】
本実施形態で得られるポリマー性アモルファスカーボンは硬質DLCアモルファスカーボンより水素含有量が多く軟質で密着性も良く容器の変形に追従して剥離しない特性を有する。炭化水素ガス等の水素含有化合物を原料ガスとするプラズマCVDにおいて、形成被膜の性質は被膜の水素含有量に依存することが知られており、被膜の水素含有量はプラズマCVDの条件特に被膜形成時の基材温度に依存すると考えられる。
【0019】
ポリマー性アモルファスカーボンは、基材温度に影響するバイアス電圧用の電極を使用せずに、UHF領域のマイクロ波によるプラズマCVD法を使用し被膜硬度とガス不透過性とが適切な値となるように条件を選択して得られるものである。上記実施形態で説明した原料ガス流量、マイクロ波出力及び処理時間は処理する容器の大きさによって適宜調整する必要がある。本発明におけるプラズマCVD法においては、容器の基材温度を50〜60℃に維持するように200〜600Wの高出力のUHF領域マイクロ波を使用し処理時間を10秒以下望ましくは5秒以下に印加してプラズマを励起して被覆を形成する。これにより、柔軟性がありガス不透過性も適度に維持するポリマー性アモルファスカーボン被膜が得られ、2000Å以下の膜厚で実用性のあるバリア効果が得られる。
【0020】
本実施形態においては、アセチレンを原料ガスとして使用しているが、メタン、エタン等のアルカン類、エチレン、プロピレン等のアルケン類、他のアルキン類又はベンゼン、トルエン等の芳香族類を単体又は混合して用いてもよく、又はアルゴンガスやヘリウムガス等で希釈して用いてもよい。又、含酸素炭化水素化合物や含窒素炭化水素化合物を使用することもできる。
【0021】
本実施の形態ではマイクロ波発生器18は処理室4を画成するパイレックスガラス製の側壁1に隣接させているが、側壁1の材質はマイクロ波を導入できる材料は全て使用可能であり、導波管を介して1又は複数のマイクロ波発生装置を処理室4に設ける構成としてもよい。
【0022】
更に、本発明の被覆プラスチック容器は、実施形態に記したプラズマCVD手段に限定されるものではなく、従来知られたプラスチック製容器の被覆形成手段においても実施可能である。
【図面の簡単な説明】
【図1】本発明に係る被覆プラスチック容器を製造するプラズマCVD被膜形成装置の一構成例を示す概略断面図。
【符号の説明】
1…側壁、2…底板、3…隔壁、4…処理室、5…排気孔、6…通気口、7…排気室、11…原料ガス導入管、13…バルブ、14…プラスチック製容器、15…マスキング部材、16…マスキング部 18…マイクロ波発生装置。
[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a coated plastic container having a coating having gas barrier properties, and more particularly to a coated plastic container having a gas barrier coating formed on the inner surface by plasma CVD means and a method for producing the same.
[0002]
[Prior art]
Containers such as bottles made of polyester resin or polyolefin resin are generally used as containers for beverages, foods, aerosols, cosmetics and the like. Since these conventional plastic containers have poor gas barrier properties and permeate gases such as oxygen and carbon dioxide, there is a disadvantage that the contents stored by the container are limited, for example, it cannot be used as a container for carbonated beverages or the like. .
[0003]
In order to improve the gas barrier properties of these plastic containers, it has been proposed to apply a film having gas barrier properties to the inner surface of the plastic container, and attention is paid to the gas barrier coating treatment by plasma CVD using a carbon-containing gas or a silicon-containing gas. Has been.
[0004]
Conventionally, various proposals have been made for a gas barrier coating treatment method by plasma CVD of a plastic container, such as JP-A-2-70059, JP-A-8-509166, JP-A-8-53117, and the like. As a film forming method, a plastic bottle is arranged in a hollow external electrode constituting a processing chamber, and a raw material gas introduction pipe that also serves as an internal electrode grounded is inserted into the bottle, and the inside of the bottle is evacuated to a vacuum. After that, a source gas is supplied and a high frequency voltage is applied to the external electrode to generate plasma and a hard DLC film is deposited on the inner wall of the bottle, or a microwave is used as a plasma generating means, and plasma of the source gas is used. A method of forming a soft polymer coating on the inner surface of the container by exciting the oxidant is known.
[0005]
When a gas barrier coating is formed by these conventional plasma CVD methods, the coating on the mouth of a plastic container generally tends to have a film thickness. This is because, in the method of generating plasma while exhausting from the container mouth and controlling the degree of vacuum and supplying the source gas, the source gas generally tends to flow in the vicinity of the mouth, and the vicinity of the mouth tends to be a thick film. is there.
[0006]
Therefore, in the case of a carbon film using a hydrocarbon compound as a raw material gas, the thick film portion is conspicuously brown and the appearance is deteriorated. The container mouth, which is the stopper and lid attachment part, is formed thick to prevent deformation, but in the case of a polyethylene terephthalate resin container for hot packs, the mouth is heated above the crystallization temperature. It is used as a so-called whitened PET bottle that is whitened and crystallized to enhance the heat resistance of the mouth. In such a mouth-whitened container, in particular, since the mouth is white, coloring is conspicuous even if the film is a thin film, the appearance is deteriorated, and the merchantability is poor.
[0007]
[Problems to be solved by the invention]
An object of the present invention is to provide a coated plastic container having improved merchantability and a method for producing the same, by eliminating the disadvantages of the coated plastic container in which a coating having gas barrier properties is formed on the inner surface.
[0008]
[Means for Solving the Problems]
In order to solve the above problems, in the present invention, in the coated plastic container in which the gas barrier coating is formed on the inner surface of the plastic container, the gas barrier coating is made of polymeric amorphous carbon, and the mouth of the inner surface of the container is excluded. Since the coating is formed, the appearance of the coated plastic container is improved, and the merchantability is improved. Since the mouth portion of the container is formed with a particularly thick wall in order to provide a lid and a stopper, the gas barrier property of the coated plastic container is not affected even if the inner surface of the mouth portion is not coated. Further, since the gas barrier coating is made of polymeric amorphous carbon, it is a coating that does not cause peeling or cracking following deformation during use of a coated plastic container, and even a thin film with a small total adhesion amount is practical. Sufficient gas barrier properties can be obtained.
[0009]
Further, the coated plastic container is made of polyethylene terephthalate resin, and the mouth portion is whitened, so that the inner surface of the white mouth portion where the gas barrier coating is conspicuous is maintained as a white coated plastic container. Productivity is improved .
[0010]
In order to solve the above problems, the method for producing a coated plastic container according to the present invention is provided with a masking means for preventing the gas in the plasma from approaching the inner surface of the mouth of the plastic container, and the inner surface of the container is subjected to gas barrier coating treatment by plasma CVD. Therefore, the reusable masking means can prevent the film from adhering to the inner surface of the mouth of the coated plastic container with a simple apparatus.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
Next, embodiments of the present invention will be described in more detail with reference to the accompanying drawings. FIG. 1 is a sectional view schematically showing a plasma CVD apparatus according to the present invention.
[0012]
In FIG. 1, a bottom plate 2 in which a container 14, which is a 500 ml polyethylene terephthalate resin bottle, is lifted and moved from below into a processing chamber 4 defined by a side wall 1 and a partition wall 3 made of Pyrex glass. 14 is stored in the processing chamber 4. The container 14 is arranged so that the inside of the container communicates with the exhaust hole 5 provided in the partition wall 3 via the masking member 15. In the masking member 15, the upper protruding portion 17 is closely inserted into the exhaust hole 5, and the masking portion 16 is inserted into the mouth of the container 14. The interval between the outer diameter of the masking portion 16 and the inner diameter of the mouth portion of the container 14 is configured to be a gap of 1 mm or less.
[0013]
The masking member 15 may be placed on the bottom plate 2 in a state where the masking member 15 is previously mounted on the container 4, and the protruding portion 17 may be inserted into the exhaust hole 5 by raising the bottom plate 2, or the exhaust hole 5 of the partition wall 3. The masking member 15 may be attached to the mask 14 and the masking portion 16 may be inserted into the mouth of the container 14 that rises together with the bottom plate 2.
[0014]
An exhaust chamber 7 formed by the side wall 9 and the upper wall 12 is provided above the partition wall 3, and the opening 10 of the side wall 9 communicates with a vacuum device 19 (not shown). The exhaust chamber 7 and the processing chamber 4 communicate with each other via a valve 13 provided in a vent 6 provided in the partition wall 3. The raw material gas introduction pipe 11 is supported on the upper wall 8 through a seal and is connected to a raw material tank (not shown) to supply acetylene as a raw material for forming a film inside the container 14. The source gas is controlled by a valve (not shown) so that the source gas flow rate becomes a predetermined flow rate. The microwave generator 18 generates a microwave having a frequency in the UHF region, for example, 2.45 GHz.
[0015]
Next, the film forming method in the present embodiment will be described in detail. After the masking member 15 is attached to the exhaust hole 5 of the partition wall 3, the bottom plate 12 on which the container 14 is disposed is raised to store the container 14 at the position shown in the figure, and the masking portion 16 is disposed on the inner surface of the mouth of the container 14. The vacuum device 19 is operated to discharge the air in the exhaust chamber 7, and the inside of the container 14 and the processing chamber 4 are decompressed through the exhaust hole 5 and the vent 6. When the pressure was reduced to approximately 60 mbar, the valve 13 was closed, and the vacuum device was further operated to reduce the pressure inside the container to 0.1 mbar.
[0016]
Next, 2.45 GHz microwave was applied at an output of 400 W for 3 seconds while acetylene was supplied into the container 14 at a flow rate of 160 sccm from the source gas introduction tube 11. Thereafter, the application of microwaves was stopped, the inside of the processing chamber 4 and the container was returned to atmospheric pressure, the bottom plate 2 was lowered, and the container 14 was taken out. The taken-out container 14 had no film formed on the inner surface of the mouth part, and a polymer amorphous carbon film having a film thickness of about 1000 mm was formed on the inner surface of the container 14 other than the inner surface of the mouth part.
[0017]
The coating container 14 thus obtained has a gas barrier effect of 27 to 30 times that of an untreated PET bottle not provided with a gas barrier coating, and the amount of adhesion of the gas barrier coating is 8 to 9 mg per container. It was a value that would not hinder recycling.
[0018]
The polymeric amorphous carbon obtained in the present embodiment has a characteristic that it has a higher hydrogen content than soft DLC amorphous carbon, is soft, has good adhesion, and does not peel off following the deformation of the container. In plasma CVD using a hydrogen-containing compound such as a hydrocarbon gas as a source gas, it is known that the properties of the formed film depend on the hydrogen content of the film. It is thought that it depends on the substrate temperature at the time.
[0019]
Polymeric amorphous carbon uses a plasma CVD method using microwaves in the UHF region without using an electrode for bias voltage that affects the substrate temperature, so that the film hardness and gas impermeability become appropriate values. It can be obtained by selecting conditions. The raw material gas flow rate, microwave output, and processing time described in the above embodiment need to be adjusted as appropriate depending on the size of the container to be processed. In the plasma CVD method of the present invention, a high-power UHF region microwave of 200 to 600 W is used so that the substrate temperature of the container is maintained at 50 to 60 ° C., and the processing time is 10 seconds or less, preferably 5 seconds or less. Applied to excite the plasma to form a coating. As a result, a polymeric amorphous carbon film that is flexible and maintains gas impermeability in an appropriate manner can be obtained, and a practical barrier effect can be obtained with a film thickness of 2000 mm or less.
[0020]
In this embodiment, acetylene is used as a raw material gas, but alkanes such as methane and ethane, alkenes such as ethylene and propylene, other alkynes, or aromatics such as benzene and toluene are used alone or mixed. Or may be used diluted with argon gas or helium gas. Moreover, an oxygen-containing hydrocarbon compound and a nitrogen-containing hydrocarbon compound can also be used.
[0021]
In the present embodiment, the microwave generator 18 is adjacent to the Pyrex glass side wall 1 that defines the processing chamber 4. However, any material that can introduce microwaves can be used for the side wall 1. One or a plurality of microwave generators may be provided in the processing chamber 4 via a wave tube.
[0022]
Furthermore, the coated plastic container of the present invention is not limited to the plasma CVD means described in the embodiment, and can be implemented in a conventionally known plastic container coating forming means.
[Brief description of the drawings]
FIG. 1 is a schematic cross-sectional view showing a configuration example of a plasma CVD film forming apparatus for producing a coated plastic container according to the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Side wall, 2 ... Bottom plate, 3 ... Partition, 4 ... Processing chamber, 5 ... Exhaust hole, 6 ... Vent, 7 ... Exhaust chamber, 11 ... Source gas introduction pipe, 13 ... Valve, 14 ... Plastic container, 15 ... masking member, 16 ... masking section, 18 ... microwave generator.

Claims (4)

プラスチック製容器の内面にガスバリア被膜が形成された被覆プラスチック容器において、前記ガスバリア被膜はポリマー性アモルファスカーボンからなり、前記容器の内面のうち口部を除いて被膜が形成されていることを特徴とする被覆プラスチック容器。In a coated plastic container in which a gas barrier coating is formed on the inner surface of a plastic container, the gas barrier coating is made of polymeric amorphous carbon, and the coating is formed except for the mouth portion of the inner surface of the container. Coated plastic container. 前記被覆プラスチック容器はポリエチレンテレフタレート樹脂製であって、前記口部が白化されていることを特徴とする請求項1記載の被覆プラスチック容器。  2. The coated plastic container according to claim 1, wherein the coated plastic container is made of polyethylene terephthalate resin, and the mouth is whitened. 前記ガスバリア被覆はプラズマCVD処理により形成されたことを特徴とする請求項1または請求項2記載の被覆プラスチック容器。 3. The coated plastic container according to claim 1, wherein the gas barrier coating is formed by a plasma CVD process. プラスチック製容器の口部の内面にプラズマ状態のガスの接近を防止するマスキング手段を設け、プラズマCVDにより前記容器の内面にガスバリア被覆処理を行うことことを特徴とする被覆プラスチック容器の製造方法。  A method for producing a coated plastic container, comprising: providing an inner surface of a mouth of a plastic container with a masking means for preventing a gas in a plasma state from approaching, and performing a gas barrier coating treatment on the inner surface of the container by plasma CVD.
JP2000240845A 2000-08-09 2000-08-09 Plastic container having gas barrier coating layer and method for producing the same Expired - Fee Related JP3993971B2 (en)

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