JP2016204685A - ガスバリア性プラスチック成形体及びその製造方法 - Google Patents
ガスバリア性プラスチック成形体及びその製造方法 Download PDFInfo
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- JP2016204685A JP2016204685A JP2015085018A JP2015085018A JP2016204685A JP 2016204685 A JP2016204685 A JP 2016204685A JP 2015085018 A JP2015085018 A JP 2015085018A JP 2015085018 A JP2015085018 A JP 2015085018A JP 2016204685 A JP2016204685 A JP 2016204685A
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- C—CHEMISTRY; METALLURGY
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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Abstract
【解決手段】本発明に係るガスバリア性プラスチック成形体90は、プラスチック成形体91と、プラスチック成形体91の表面に設けたガスバリア薄膜92とを備えるガスバリア性プラスチック成形体において、ガスバリア薄膜92は、構成元素として珪素(Si)、炭素(C)及び酸素(O)を含有し、かつ、条件(1)でX線電子分光分析すると、Si−Cの結合エネルギーのピーク出現位置に、メインピークが観察される領域を有する。
条件(1)測定範囲を95〜105eVとする。
【選択図】図1
Description
条件(1)測定範囲を95〜105eVとする。
(数1)C含有率[%]={(C含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数1において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数2)Si含有率[%]={(Si含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数2において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数3)O含有率[%]={(O含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数3において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数1)C含有率[%]={(C含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数1において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数3)O含有率[%]={(O含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数3において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
条件(1)測定範囲を95〜105eVとする。
条件(1)測定範囲を95〜105eVとする。
(数1)C含有率[%]={(C含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数1において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数2)Si含有率[%]={(Si含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数2において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数3)O含有率[%]={(O含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数3において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数5)BIF=[薄膜未形成のプラスチック成形体の酸素透過度]/[ガスバリア性プラスチック成形体の酸素透過度]
図2に示す成膜装置を用いてガスバリア性プラスチック成形体を製造した。プラスチック成形体としてPET製のプラスチックボトル(内容量500ml)、珪素含有炭化水素ガスとしてビニルシラン、発熱体として炭化タンタル線(φ0.5mm)を用いた。まず、排気工程を次のとおり行った。排気工程では、真空チャンバの内部を排気して真空チャンバ内を初期圧力P0=1.5Pa以下に調整した。次いで、準備工程を次のとおり行った。準備工程では、ゲートバルブを開けた後、真空チャンバ内に珪素含有炭化水素ガスを導入して真空チャンバ内の圧力をP0Paに調整した後、P0Paより高いPAPaに到達させた。また、プラスチックボトルを出入用チャンバから降下させて発熱体及び原料ガス供給管をプラスチックボトルの内部に挿入した。次に、成膜工程を次のとおり行った。成膜工程では、珪素含有炭化水素ガスの導入を継続しながら発熱体の加熱を開始し、2100〜2200℃まで加熱して、プラスチックボトルの内表面に堆積した薄膜が20nmに到達したところで、発熱体の加熱を停止した。その後、プラスチックボトルを出入チャンバに戻してゲートバルブを閉じるとともに、ガスの供給を停止した。また、成膜工程では、真空チャンバ内の圧力をPAPaより高いPBPaに到達させた。各工程での圧力PA,PBは、(PB−PA)/P0が0.16となるように調整した。成膜工程が完了した後、出入チャンバ内を大気解放して、得られたガスバリア性プラスチック成形体を取り出し、新たな未処理のプラスチックボトルを投入して開閉ゲートを閉じた。これら一連の成膜作業を繰り返し行った。
各工程での圧力PA,PBを(PB−PA)/P0が0.15となるように調整した以外は、実施例1と同様にしてガスバリア性プラスチック成形体を製造した。
各工程での圧力PA,PBを(PB−PA)/P0が0.11となるように調整した以外は、実施例1と同様にしてガスバリア性プラスチック成形体を製造した。
発熱体として炭化処理していないタンタル線(φ0.5mm)を用い、準備工程を行わなわず、薄膜の膜厚を36nmに変更した以外は、実施例1と同様にしてガスバリア性プラスチック成形体を製造した。
実施例1及び比較例1について一連の成膜作業1回目で得られたプラスチックボトルの薄膜の表面をXPS装置(型式:QUANTERASXM、PHI社製)を用いて分析した。薄膜表面の構成元素の比率を表2に示す。XPS分析の条件は、次の通りである。
測定条件
励起X線:Al mono
検出領域:100μmφ
取出角:90deg
検出深さ:約8nm
実施例1及び比較例1について一連の成膜作業1回目で得られたプラスチックボトルの薄膜の表面を前記したXPS装置を用いて条件(1)で分析した。試験片及び分析条件は、組成分析と同様とした。
前記したXPS装置を用いて、アルゴンイオンエッチングを行いながら、実施例1及び比較例1について一連の成膜作業1回目で得られたプラスチックボトルの薄膜の深さプロファイルを分析した。試験片及び分析条件は、組成分析と同様とした。ここで、ガスバリア薄膜を深さ方向に二等分して考えたとき、実施例1ではプラスチック成形体とは反対側の10nmを上層とし、プラスチック成形体側の10nmを下層とし、比較例1ではプラスチック成形体とは反対側の18nmを上層とし、プラスチック成形体側の18nmを下層とした。
実施例及び比較例について一連の成膜作業1回目で得られたプラスチックボトルと用いて透明性を評価した。透明性はb*値で評価した。b*値は、自記分光光度計(U‐3900形、日立社製)に同社製60Φ積分球付属装置(赤外可視近赤外用)を取り付けたものを用いて測定した。検知器としては、超高感度光電子増倍管(R928:紫外可視用)と冷却型PbS(近赤外域用)を用いた。測定波長は、380nmから780nmの範囲で透過率を測定した。ペットボトルの透過率を測定することによって、ガスバリア薄膜のみの透過率測定を算出することができるが、本実施例のb*値は、ペットボトルの吸収率も含めた形で算出したものをそのまま示している。測定には、光沢度の測定で用いた試験片を使用した。3枚の平均値をb*値として表3に示した。
実施例及び比較例について一連の成膜作業の繰返し回数が1回目、100回目、200回目で得られた各プラスチックボトルを用いてガスバリア性を評価した。ガスバリア性はBIFで評価した。まず、実施例又は比較例の各プラスチックボトルについて酸素透過度を測定した。酸素透過度は、酸素透過度測定装置(型式:Oxtran 2/20、Modern Control社製)を用いて、23℃、90%RHの条件にて測定し、測定開始から24時間コンディションし、測定開始から72時間経過後の値とした。BIFは、数5において、未成膜ボトルの酸素透過度の値を薄膜未形成のプラスチック成形体の酸素透過度とし、実施例又は比較例の各プラスチックボトルの酸素透過度の値をガスバリア性プラスチック成形体の酸素透過度として算出した。評価基準は、次のとおりである。評価結果を表3に示す。
◎:各プラスチックボトルのBIFが10以上である(実用レベル)。
○:各プラスチックボトルのBIFが5以上10未満である(実用下限レベル)。
×:各プラスチックボトルのBIFが5未満である(実用不適レベル)。
一連の成膜作業を1万回繰り返した後、発熱体を成膜装置から外して、返し部から40〜80mm部分を指で把持し、強度を確認した。評価基準は次のとおりである。評価結果を表3に示す。
○:発熱体直線部が±1.5mmの範囲を維持し、指で把持しても破損しない(実用レベル)。
△:発熱体直線部が±3.0mmの範囲を維持し、指で把持しても破損しない(実用下限レベル)。
×:発熱体直線部が±3.0mmの範囲を超え、指把持により破損する(実用不適レベル)。
31 成膜専用チャンバ(真空チャンバ)
32 出入用チャンバ
33 ゲートバルブ
42 発熱体
56 開閉ゲート
80 圧力検出部
VP1 真空ポンプ
VP2 真空ポンプ
90 ガスバリア性プラスチック成形体
91 プラスチック成形体
92 ガスバリア薄膜
92a 上層
92b 下層
92s ガスバリア薄膜の表面
Claims (7)
- プラスチック成形体と、該プラスチック成形体の表面に設けたガスバリア薄膜とを備えるガスバリア性プラスチック成形体において、
前記ガスバリア薄膜は、構成元素として珪素(Si)、炭素(C)及び酸素(O)を含有し、かつ、条件(1)でX線電子分光分析すると、Si−Cの結合エネルギーのピーク出現位置に、メインピークが観察される領域を有することを特徴とするガスバリア性プラスチック成形体。
条件(1)測定範囲を95〜105eVとする。 - 前記ガスバリア薄膜は、深さ方向に傾斜組成を有し、
前記ガスバリア薄膜を深さ方向に二等分し、前記プラスチック成形体とは反対側を上層とし、前記プラスチック成形体側を下層としたとき、
前記上層における(数1)で表されるC含有率が、前記上層における(数2)で表されるSi含有率よりも高いことを特徴とする請求項1に記載のガスバリア性プラスチック成形体。
(数1)C含有率[%]={(C含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数1において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数2)Si含有率[%]={(Si含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数2において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。 - 前記上層における(数3)で表されるO含有率が、前記上層におけるSi含有率よりも低いことを特徴とする請求項2に記載のガスバリア性プラスチック成形体。
(数3)O含有率[%]={(O含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数3において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。 - 前記ガスバリア薄膜は、深さ方向に傾斜組成を有し、
前記ガスバリア薄膜を深さ方向に二等分し、前記プラスチック成形体とは反対側を上層とし、前記プラスチック成形体側を下層としたとき、
前記下層における(数1)で表されるC含有率が、前記下層における(数3)で表されるO含有率よりも高いことを特徴とする請求項1〜3のいずれか1つに記載のガスバリア性プラスチック成形体。
(数1)C含有率[%]={(C含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数1において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。
(数3)O含有率[%]={(O含有量[atomic%])/(Si,O及びCの合計含有量[atomic%])}×100
数3において、Si,O又はCの含有量は、Si,O及びCの3元素の内訳における含有量である。 - 真空チャンバの内部を排気して前記真空チャンバ内を初期圧力P0以下に調整する排気工程と、
前記真空チャンバ内の圧力がP0以下に調整され、かつ、真空チャンバ内に配置された炭化タンタル相を有する発熱体が加熱されていないときに、珪素含有炭化水素ガスを前記真空チャンバ内に導入して該真空チャンバ内の圧力を前記P0に調整する準備工程と、
前記珪素含有炭化水素ガスを継続して前記真空チャンバに導入しながら前記発熱体を加熱して、前記真空チャンバ内に収容されているプラスチック成形体の表面にガスバリア薄膜を形成する成膜工程と、
を有することを特徴とするガスバリア性プラスチック成形体の製造方法。 - 前記準備工程において、前記真空チャンバ内の圧力を前記P0に調整後、前記真空チャンバ内の圧力を前記P0より高い圧力PAに到達させ、
前記成膜工程において、前記真空チャンバ内の圧力を前記PAより高い圧力PBに到達させることを特徴とする請求項5に記載のガスバリア性プラスチック成形体の製造方法。 - (PB−PA)/P0が0.11以上であることを特徴とする請求項6に記載のガスバリア性プラスチック成形体の製造方法。
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