JP3845055B2 - Gas permeability measuring device - Google Patents

Gas permeability measuring device Download PDF

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JP3845055B2
JP3845055B2 JP2002324939A JP2002324939A JP3845055B2 JP 3845055 B2 JP3845055 B2 JP 3845055B2 JP 2002324939 A JP2002324939 A JP 2002324939A JP 2002324939 A JP2002324939 A JP 2002324939A JP 3845055 B2 JP3845055 B2 JP 3845055B2
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temperature
pressure sensor
permeation pressure
measurement gas
permeation
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JP2004157068A (en
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良知 有賀
信行 柳澤
正博 高原
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株式会社東洋精機製作所
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Description

【０００１】
【発明の属する技術分野】
本発明は、試料膜を透過する測定ガスの透過率を測定するガス透過率測定装置に関する。
【０００２】
【従来の技術】
従来、試料膜を装着する一対のセルからなるチャンバーと、試料膜の一方のセル内に測定ガスを加える測定ガスタンクと、試料膜の他方のセル内を減圧する真空ポンプと、試料膜を透過した測定ガスの圧力を測定する透過圧力センサーとからなるガス透過率測定装置は知られている。このガス透過率測定装置を使用して一定温度条件下でガス透過率を測定する場合には、ガス透過率測定装置の全体を恒温槽内に入れて装置全体を温度制御することにより測定を行っていた。
【０００３】
【発明が解決しようとする課題】
しかし、ガス透過率測定装置の全体を恒温槽内に入れると、試料膜を透過した測定ガスの圧力を測定する透過圧力センサーも恒温槽内で温度制御されるため、透過圧力センサーの耐熱温度より高い温度でのガス透過率の測定ができないという課題があった。
また、装置全体を恒温槽内に入れるために恒温槽が大きくなり、温度制御する部分が増えることにより温度制御に時間を要すると共に、均一な温度分布に制御することが難しいという課題があった。
【０００４】
【課題を解決するための手段】
そこで、本発明は、上記課題を解決するために、試料膜を装着する一対のセルからなるチャンバーと、前記試料膜の一方の一次側セル内に測定ガスを加える測定ガスタンクと、前記試料膜の他方の二次側セル内を減圧する真空ポンプと、前記試料膜を透過した測定ガスの圧力を測定する透過圧力センサーとからなるガス透過率測定装置であって、前記チャンバーと前記測定ガスタンクの温度を制御する温度制御部を備え、前記透過圧力センサーによる測定圧力を前記温度制御部と前記透過圧力センサーの部分の温度により補正して測定ガスの透過率を求めるようにしたガス透過率測定装置を提供するものである。
本発明によれば、前記チャンバーと前記測定ガスタンクは温度制御部により温度制御し、一方、前記透過圧力センサーの部分は室温又は透過圧力センサーの耐熱温度以内に温度制御することによって、前記透過圧力センサーの耐熱温度に左右されることなく前記チャンバーと前記測定ガスタンクの温度を制御することができる。また、温度制御部は装置全体を温度制御しないことにより前記温度制御部が小さくなるから、温度制御の時間を短縮でき、ガス透過率の試験全体の時間を短縮することができる。
【０００５】
また、本発明は、前記温度制御部と前記透過圧力センサーの部分に温度センサーを設けた請求項１に記載のガス透過率測定装置を提供するものである。
本発明によれば、前記温度制御部と前記透過圧力センサーの部分の温度を測定して、前記透過圧力センサーによる測定圧力を補正して測定ガスの透過率を求めることができる。
【０００６】
また、本発明は、前記透過圧力センサーと前記チャンバーを接続する配管内の体積が二次側の体積の１％以上の場合に、前記透過圧力センサーの部分を配管と透過圧力センサーに分けて前記測定圧力を温度補正するようにした請求項１又は２に記載のガス透過率測定装置を提供するものである。
本発明によれば、前記配管内の体積が二次側の体積の１％以上の場合に、前記配管の温度勾配による測定圧力の補正誤差を小さくして測定ガスの透過率を求めることができる。
【０００７】
また、本発明は、前記透過圧力センサー側を透過圧力センサーの耐熱温度以内に温度制御する温度制御装置を備え、前記温度制御部と前記透過圧力センサー側に温度差がある場合に前記透過圧力センサーによる測定圧力を補正して測定ガスの透過率を求めるようにした請求項１乃至３のいずれかに記載のガス透過率測定装置を提供するものである。
本発明によれば、前記温度制御部と前記透過圧力センサー側を別々に温度制御するから透過圧力センサーの耐熱温度以上の試験温度で測定することができると共に、前記温度制御部と前記透過圧力センサー側の温度差が小さくなるように温度制御でき、補正レベルが小さくなり測定精度を向上させることができる。特に、試験温度が透過圧力センサーの耐熱温度以内の場合には、更に温度差を小さくして測定精度を向上させることができる。
【０００８】
また、本発明は前記測定ガスタンクと前記チャンバーの間に外部制御で開閉可能なバルブを設けた請求項１乃至３のいずれかに記載のガス透過率測定装置を提供するものである。
本発明によれば、前記測定ガスタンクと前記チャンバーの間に設けたバルブの開閉を制御することにより、前記測定ガスタンク内に蓄えた試験圧力の測定ガスを試料膜に与えるタイミングを制御することができる。
【０００９】
【発明の実施の形態】
本発明の実施の形態を図示の実施例に基づいて説明する。
本発明に係るガス透過率測定装置は、試料膜１０を装着する一対のセル６，７からなるチャンバー１と、前記試料膜１０の一方の一次側セル６内に測定ガス１１を加える測定ガスタンク２と、前記試料膜１０の他方の二次側セル７内を減圧する真空ポンプ３と、前記試料膜１０を透過した測定ガス１１の圧力を測定する透過圧力センサー４とからなるガス透過率測定装置であって、前記チャンバー１と前記測定ガスタンク２の温度を制御する温度制御部５を備え、前記透過圧力センサー４による測定圧力を前記温度制御部５と前記透過圧力センサー４の部分の温度により補正して測定ガスの透過率を求めるように構成してある。
【００１０】
図１に示す実施例において、チャンバー１は、一次側セル６と二次側セル７の間に試料膜１０をセットして密閉することができるようにしてある。
一次側セル６は、配管２４を介して測定ガスタンク２と接続し、測定ガス１１を試料膜１０の一次側に加えることができるようにしてある。
二次側セル７の凹部２３には濾紙２０を設けてあると共に、配管１９を介して透過圧力センサー４と接続してある。また、一次側セル６には、温度センサー１２を設けてあり、温度制御部５内の測定ガスの温度を測定することができるように構成してある。
【００１１】
図１に示す実施例において、測定ガスタンク２は、バルブ１４を備えた配管２５を介して測定ガス源９に接続してあると共に、タンク圧力センサー８を設けてある。バルブ１４の開閉を制御することにより測定ガスタンク２内の測定ガス１１の圧力を試験圧力まで上昇させて、配管２４を介して試験圧力の測定ガス１１を一次側セル６に供給することができるように構成してある。
【００１２】
図１に示す実施例において、温度制御部５は、恒温槽からなり、チャンバー１と測定ガスタンク２を収納して試験温度に保つように温度制御している。ただし、図示の実施例のように測定ガスタンク２全体を恒温槽内に設ける場合に限らず、測定ガスタンク２は、タンクを恒温槽の外に引き出すと共に、該タンクとチャンバー１の間の恒温槽内に、チャンバー１内の測定ガス１１の容積の数倍のタンクを新たに設けて、測定ガス１１を試験温度に保つように構成することも可能である。
【００１３】
図１に示す実施例において、透過圧力センサー４は、配管１９を恒温槽の外に引き出して、温度制御部５である恒温槽の外の室温部３０に設けてある。これにより、温度制御部５内の温度を透過圧力センサー４の耐熱温度以上に設定することができると共に、透過圧力センサー４は耐熱性を要しないから耐熱性の低い圧力センサーを使用することが可能になる。
透過圧力センサー４は、アンプ２２を介してパソコン２９に接続してあり、試料膜１０を透過した測定ガス１１の圧力を測定してガス透過率を求めるようにしてある。また、透過圧力センサー４には、温度センサー１３を設けてあり、配管１９を含む透過圧力センサー４の部分の測定ガス１１の温度を測定することができるように構成してある。
【００１４】
室温部３０には撹拌ファン２１を設けてあり、透過圧力センサー４の周囲の空気を撹拌することにより、温度制御部５内から配管１９によって透過圧力センサー４に伝わる熱を減少させ、透過圧力センサー４の部分の温度を略一定に保つように構成してある。
【００１５】
また、室温部３０に透過圧力センサー４側（透過圧力センサー４と配管１９）を透過圧力センサー４の耐熱温度以内に温度制御する温度制御装置を備え、温度制御部５と透過圧力センサー４側に温度差がある場合に透過圧力センサー４による測定圧力を補正して測定ガスの透過率を求めるように構成することもできる。温度制御装置は、試験温度が透過圧力センサー４の耐熱温度以内の場合には、透過圧力センサー４側を試験温度に制御することができ、透過圧力センサー４による測定圧力から測定ガスの透過率を直接求めることもできる。一方、試験温度が透過圧力センサー４の耐熱温度以外の場合には、温度制御装置は透過圧力センサー４側を透過圧力センサー４の耐熱温度以内に温度制御することにより、温度制御部５と透過圧力センサー４側の温度差を小さくして、測定圧力の補正による誤差を小さくすることができる。
【００１６】
真空ポンプ３は、バルブ１６を備えた配管２６を介して配管２５に接続され、試料膜１０の一次側を減圧することができるようにしてあると共に、バルブ１５を備えた配管２７を介して配管１９に接続され、試料膜１０の二次側を減圧することができるようにしてある。さらに、配管２６，２７には、バルブ１８を備えた排気管２８を設けて、測定ガス１１を排気することができるように構成してある。
【００１７】
次に、図１に示す実施例において、ガス透過率の測定手順について説明する。
（１）試料膜１０をチャンバー１にセットして、チャンバー１を密閉する。
（２）全てのバルブ１４，１５，１６，１８を閉じて真空ポンプ３の電源を入れる。
（３）バルブ１５を開き、透過圧力センサー４の指示値が一定の真空値になるまで試料膜１０の二次側を減圧する。
（４）バルブ１６を開き、透過圧力センサー４及びタンク圧力センサー８の指示値が一定の真空値になるまで試料膜１０の一次側及び二次側を減圧する。
（５）バルブ１５，１６を閉じて減圧作業を終了する。
（６）バルブ１４を開き、測定ガス源９から測定ガスタンク２に測定ガス１１を供給し、タンク圧力センサー８の指示値が試験圧力まで上昇したところでバルブ１４を閉じ、ガス透過率測定の試験が開始される。
（７）二次側の圧力変化率が一定状態（定常状態）になると試験が終了する。
（８）試験終了後は、真空ポンプを停止して、バルブ１５，１６，１８を開き測定ガス１１を排気する。
【００１８】
そして、透過圧力センサー４によって測定された二次側の測定ガス（Ｖ１＋Ｖ２）の圧力Ｐ［ｋPa］から温度補正をして、試料膜１０のガス透過率ＧＴＲ（Gas Transmission Rate）を求める。
このとき、二次側セル７の容積（濾紙２０の密度を含まない）をＶ１［cm３］、二次側の配管１９と透過圧力センサー４の容積をＶ２［cm３］、温度センサー１２の測定温度をＴ１［Ｋ］、温度センサー１３の測定温度をＴ２［Ｋ］とすると、理想温度Ｔ０［２７３Ｋ］に換算した二次側の測定ガス（Ｖ１＋Ｖ２）の理想圧力Ｐ’［ｋPa］は数１に示す式により求めることができる。
【００１９】
【数１】

Figure 0003845055
【００２０】
定常状態時の理想圧力Ｐ’［ｋPa］の変化と、試料膜１０に対して一次側の測定ガス１１と二次側の測定ガスの圧力差Ｐｄ［ｋPa］から、試料膜１０のガス透過率ＧＴＲは数２に示す式により求めることができる。
【００２１】
【数２】
Figure 0003845055
【００２２】
次に、図２に示す実施例について説明する。
１７は、バルブであり、測定ガスタンク２とチャンバー１の間を接続する配管２４に設けてある。バルブ１７は、パソコン２９により開閉を制御するようにしてあり、測定ガスタンク２内に蓄えた試験圧力の測定ガス１１を試料膜１０に加えるタイミングを制御することができるように構成してある。その他の構成は、図１に示す実施例と同様である。
【００２３】
図２に示す実施例において、ガス透過率と拡散係数の測定手順について説明する。
（１）試料膜１０をチャンバー１にセットして、チャンバー１を密閉する。
（２）全てのバルブ１４，１５，１６，１７，１８を閉じて真空ポンプ３の電源を入れる。
（３）バルブ１５を開き、透過圧力センサー４の指示値が一定の真空値になるまで試料膜１０の二次側を減圧する。
（４）バルブ１６，１７を開き、透過圧力センサー４及びタンク圧力センサー８の指示値が一定の真空値になるまで試料膜１０の一次側及び二次側を減圧する。
（５）バルブ１５，１６，１７を閉じて減圧作業を終了する。
（６）バルブ１４を開き、測定ガス源９から測定ガスタンク２に測定ガス１１を供給し、タンク圧力センサー８の指示値が試験圧力まで上昇したところでバルブ１４を閉じる。
（７）バルブ１７をパソコン２９の制御により開き、開いた瞬間より試験を開始し、経過時間に対する圧力を測定して、圧力変化率が一定状態になると試験が終了する。
（８）試験終了後は、真空ポンプを停止して、バルブ１５，１６，１８を開き測定ガス１１を排気する。
【００２４】
この手順（７）で試料膜１１の一次側に試験圧力の測定ガス１１を加えると、測定ガス１１は試料膜１０の中に拡散して徐々に透過が始まり、図３に示すように透過圧力センサー４の測定圧力は試験開始後徐々に増加し、その後、圧力変化率が一定状態になり、時間に対して直線的に変化するようになる。この直線的に変化する部分の透過圧力センサー４の測定圧力を用いて、図１の実施例の場合と同様に試料膜１０のガス透過率ＧＴＲを求めることができる。
【００２５】
また、図３に示す測定圧力の変化曲線の直線部分の外挿線と、時間軸の交点より遅れ時間θを求め、数３に示す式により拡散係数Ｄを求めることができる。
【００２６】
【数３】
Figure 0003845055
【００２７】
また、ガス透過率ＧＴＲは、拡散係数Ｄと溶解度係数Ｓの積（ＧＴＲ＝Ｓ×Ｄ）であることから、ガス透過率ＧＴＲと拡散係数Ｄが求まることにより溶解度係数Ｓを求めることもできる。
【００２８】
図１又は図２に示す実施例において、透過圧力センサー４とチャンバー１を接続する配管１９内の体積が二次側の体積（Ｖ１＋Ｖ２）の１％以上の場合に、透過圧力センサーの部分を配管１９と透過圧力センサー４に分けて測定圧力を温度補正するようにしてある。
配管１９の温度は、温度制御部５内の温度Ｔ１［Ｋ］から透過圧力センサー４の温度Ｔ２［Ｋ］まで変化するので、配管１９内の体積が二次側の体積の１％以上の場合には上述の数１に示す換算式では換算誤差が大きくなるため、透過圧力センサーの部分の容積Ｖ２を配管１９と透過圧力センサー４と分けて、数４に示す換算式により二次側の測定ガス１１の圧力を理想圧力Ｐ’［ｋPa］に換算するようにしてある。
透過圧力センサー４の容積をＶ２’［cm３］、配管１９の容積をＶ３［cm３］、配管１９の温度をＴ３（Ｔ３＝（Ｔ１＋Ｔ２）／２）［Ｋ］としている。
【００２９】
【数４】
Figure 0003845055
【００３０】
例えば、試料膜１０の二次側の各部の容積をＶ１＝１［cm３］、Ｖ２’＝３．５［cm３］としたとき、内径Φ＝２［mm］、長さＬ＝１０［cm］の配管１９を用いると、配管１９内の体積（Ｖ３）は二次側の体積（Ｖ１＋Ｖ２’＋Ｖ３）の６．２５％となるので、数４に示す換算式によって測定圧力を温度補正する。
ここで、配管１９の温度変化を直線勾配として温度Ｔ３を計算しているため、配管１９の実際の温度勾配との誤差が生じる。この温度Ｔ３の誤差が理想圧力Ｐ’に与える影響は、数４に示す換算式中のＴ３の係数（Ｖ３／（Ｖ１＋Ｖ２’＋Ｖ３））に依存するので、これによる誤差を小さくするにはＶ３を小さくすることが好ましい。
【００３１】
【発明の効果】
以上の通り、本発明に係るガス透過率測定装置によれば、試料膜を装着する一対のセルからなるチャンバーと、前記試料膜の一方の一次側セル内に測定ガスを加える測定ガスタンクと、前記試料膜の他方の二次側セル内を減圧する真空ポンプと、前記試料膜を透過した測定ガスの圧力を測定する透過圧力センサーとからなるガス透過率測定装置であって、前記チャンバーと前記測定ガスタンクの温度を制御する温度制御部を備え、前記透過圧力センサーによる測定圧力を前記温度制御部と前記透過圧力センサーの部分の温度により補正して測定ガスの透過率を求めるようにした構成を有することにより、前記チャンバーと前記測定ガスタンクは温度制御部により温度制御し、一方、前記透過圧力センサーの部分は室温又は透過圧力センサーの耐熱温度以内に温度制御することによって、前記透過圧力センサーの耐熱温度に左右されることなく前記チャンバーと前記測定ガスタンクの温度を制御することができる。また、温度制御部は装置全体を温度制御しないことにより前記温度制御部が小さくなるから、温度制御の時間を短縮でき、ガス透過率の試験全体の時間を短縮することができる効果がある。
【００３２】
また、本発明は、前記温度制御部と前記透過圧力センサーの部分に温度センサーを設けた請求項１に記載の構成を有することにより、前記温度制御部と前記透過圧力センサーの部分の温度を測定して、前記透過圧力センサーによる測定圧力を補正して測定ガスの透過率を求めることができる効果がある。
【００３３】
また、本発明は、前記透過圧力センサーと前記チャンバーを接続する配管内の体積が二次側の体積の１％以上の場合に、前記透過圧力センサーの部分を配管と透過圧力センサーに分けて前記測定圧力を温度補正するようにした請求項１又は２に記載の構成を有することにより、前記配管内の体積が二次側の体積の１％以上の場合に、前記配管の温度勾配による測定圧力の補正誤差を小さくして測定ガスの測定率を求めることができる効果がある。
【００３４】
また、本発明は、前記透過圧力センサー側を透過圧力センサーの耐熱温度以内に温度制御する温度制御装置を備え、前記温度制御部と前記透過圧力センサー側に温度差がある場合に前記透過圧力センサーによる測定圧力を補正して測定ガスの透過率を求めるようにした請求項１乃至３のいずれかに記載の構成を有することにより、前記温度制御部と前記透過圧力センサー側を別々に温度制御するから透過圧力センサーの耐熱温度以上の試験温度で測定することができると共に、前記温度制御部と前記透過圧力センサー側の温度差が小さくなるように温度制御でき、補正レベルが小さくなり測定精度を向上させることができる。特に、試験温度が透過圧力センサーの耐熱温度以内の場合には、更に温度差を小さくして測定精度を向上させることができる効果がある。
【００３５】
また、本発明は前記測定ガスタンクと前記チャンバーの間にバルブを設けた請求項１乃至３のいずれかに記載の構成を有することにより、前記測定ガスタンクと前記チャンバーの間に設けたバルブの開閉を制御することによって、前記測定ガスタンク内に蓄えた試験圧力の測定ガスを試料膜に与えるタイミングを制御することができる効果がある。
【図面の簡単な説明】
【図１】 本発明ガス透過率測定装置の一実施例を示す構成図
【図２】 他の実施例を示す構成図
【図３】 試料膜の二次側の圧力変化を示す図
【符号の説明】
１ チャンバー
２ 測定ガスタンク
３ 真空ポンプ
４ 透過圧力センサー
５ 温度制御部
６ 一次側セル
７ 二次側セル
８ タンク圧力センサー
９ 測定ガス源
１０ 試料膜
１１ 測定ガス
１２，１３ 温度センサー
１４，１５，１６，１７，１８ バルブ
１９ 配管
２０ 濾紙
２１ 撹拌ファン
２２ アンプ
２３ 凹部
２４，２５，２６，２７ 配管
２８ 排気管
２９ パソコン
３０ 室温部[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a gas permeability measuring apparatus that measures the permeability of a measurement gas that passes through a sample membrane.
[0002]
[Prior art]
Conventionally, a chamber composed of a pair of cells on which a sample film is mounted, a measurement gas tank for adding a measurement gas into one cell of the sample film, a vacuum pump for depressurizing the other cell of the sample film, and the sample film permeated A gas permeability measuring device comprising a permeation pressure sensor that measures the pressure of a measurement gas is known. When measuring gas permeability under a constant temperature condition using this gas permeability measuring device, the entire gas permeability measuring device is placed in a thermostatic chamber and the temperature is controlled by controlling the entire device. It was.
[0003]
[Problems to be solved by the invention]
However, when the entire gas permeability measuring device is placed in a thermostatic chamber, the temperature of the permeation pressure sensor that measures the pressure of the measurement gas that has permeated the sample membrane is also controlled in the thermostatic chamber. There was a problem that the gas permeability could not be measured at a high temperature.
Moreover, since the thermostat bath becomes large in order to put the entire apparatus in the thermostat bath, and there are more portions for temperature control, it takes time to control the temperature, and it is difficult to control the temperature distribution uniformly.
[0004]
[Means for Solving the Problems]
Therefore, in order to solve the above problems, the present invention provides a chamber composed of a pair of cells on which a sample film is mounted, a measurement gas tank for adding a measurement gas into one of the primary cells of the sample film, and the sample film A gas permeability measuring device comprising a vacuum pump for reducing the pressure in the other secondary cell and a permeation pressure sensor for measuring the pressure of the measurement gas that has permeated through the sample membrane, wherein the temperature of the chamber and the measurement gas tank A gas permeability measuring device comprising a temperature control unit for controlling the pressure, and correcting the measurement pressure by the permeation pressure sensor with the temperature of the temperature control unit and the permeation pressure sensor part to obtain the permeability of the measurement gas It is to provide.
According to the present invention, the temperature of the chamber and the measurement gas tank is controlled by a temperature control unit, while the portion of the permeation pressure sensor is controlled at a room temperature or within a heat resistant temperature of the permeation pressure sensor, thereby the permeation pressure sensor. The temperature of the chamber and the measurement gas tank can be controlled without being affected by the heat resistant temperature of the gas. In addition, since the temperature control unit becomes smaller by not controlling the temperature of the entire apparatus, the temperature control unit can be shortened, and the time for the entire gas permeability test can be shortened.
[0005]
The present invention also provides the gas permeability measuring apparatus according to claim 1, wherein temperature sensors are provided in the temperature control section and the permeation pressure sensor.
According to the present invention, the temperature of the temperature control unit and the permeation pressure sensor can be measured, and the measurement gas permeability can be determined by correcting the measurement pressure by the permeation pressure sensor.
[0006]
In the present invention, when the volume in the pipe connecting the permeation pressure sensor and the chamber is 1% or more of the volume on the secondary side, the permeation pressure sensor portion is divided into the pipe and the permeation pressure sensor. The gas permeability measuring apparatus according to claim 1 or 2, wherein the measurement pressure is temperature-corrected.
According to the present invention, when the volume in the pipe is 1% or more of the volume on the secondary side, the measurement gas permeability can be obtained by reducing the correction error of the measurement pressure due to the temperature gradient of the pipe. .
[0007]
In addition, the present invention includes a temperature control device that controls the temperature of the permeation pressure sensor within a heat resistant temperature of the permeation pressure sensor, and the permeation pressure sensor when there is a temperature difference between the temperature control unit and the permeation pressure sensor. The gas permeability measuring device according to any one of claims 1 to 3, wherein the measuring gas permeability is corrected to obtain the measuring gas permeability.
According to the present invention, since the temperature control unit and the permeation pressure sensor side are separately temperature controlled, the temperature control unit and the permeation pressure sensor can be measured at a test temperature equal to or higher than the heat resistance temperature of the permeation pressure sensor. The temperature can be controlled so that the temperature difference on the side becomes small, the correction level becomes small, and the measurement accuracy can be improved. In particular, when the test temperature is within the heat resistance temperature of the transmission pressure sensor, the temperature difference can be further reduced to improve the measurement accuracy.
[0008]
The present invention also provides a gas permeability measuring device according to any one of claims 1 to 3, wherein a valve that can be opened and closed by external control is provided between the measurement gas tank and the chamber.
According to the present invention, by controlling the opening and closing of a valve provided between the measurement gas tank and the chamber, it is possible to control the timing at which the measurement gas having the test pressure stored in the measurement gas tank is applied to the sample film. .
[0009]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described based on the illustrated examples.
The gas permeability measuring apparatus according to the present invention includes a chamber 1 including a pair of cells 6 and 7 in which a sample film 10 is mounted, and a measurement gas tank 2 that adds a measurement gas 11 into one primary cell 6 of the sample film 10. A gas permeability measuring device comprising: a vacuum pump 3 that depressurizes the other secondary cell 7 of the sample film 10; and a permeation pressure sensor 4 that measures the pressure of the measurement gas 11 that has permeated the sample film 10. A temperature control unit 5 for controlling the temperature of the chamber 1 and the measurement gas tank 2, and the pressure measured by the permeation pressure sensor 4 is corrected by the temperature of the temperature control unit 5 and the permeation pressure sensor 4. Thus, the transmittance of the measurement gas is obtained.
[0010]
In the embodiment shown in FIG. 1, the chamber 1 is configured so that a sample film 10 can be set and sealed between a primary side cell 6 and a secondary side cell 7.
The primary cell 6 is connected to the measurement gas tank 2 via a pipe 24 so that the measurement gas 11 can be added to the primary side of the sample film 10.
A filter paper 20 is provided in the concave portion 23 of the secondary cell 7 and is connected to the permeation pressure sensor 4 through a pipe 19. Moreover, the temperature sensor 12 is provided in the primary side cell 6, and it is comprised so that the temperature of the measurement gas in the temperature control part 5 can be measured.
[0011]
In the embodiment shown in FIG. 1, the measurement gas tank 2 is connected to the measurement gas source 9 via a pipe 25 provided with a valve 14 and is provided with a tank pressure sensor 8. By controlling the opening / closing of the valve 14, the pressure of the measurement gas 11 in the measurement gas tank 2 is increased to the test pressure, and the measurement gas 11 of the test pressure can be supplied to the primary cell 6 via the pipe 24. It is configured.
[0012]
In the embodiment shown in FIG. 1, the temperature control unit 5 includes a thermostatic bath, and controls the temperature so that the chamber 1 and the measurement gas tank 2 are housed and kept at the test temperature. However, the measurement gas tank 2 is not limited to the case where the entire measurement gas tank 2 is provided in the thermostat as in the illustrated embodiment, and the measurement gas tank 2 draws the tank out of the thermostat and is in the thermostat between the tank and the chamber 1. It is also possible to provide a tank several times the volume of the measurement gas 11 in the chamber 1 so as to keep the measurement gas 11 at the test temperature.
[0013]
In the embodiment shown in FIG. 1, the permeation pressure sensor 4 is provided in the room temperature portion 30 outside the thermostatic chamber which is the temperature control unit 5 by pulling the pipe 19 out of the thermostatic bath. As a result, the temperature in the temperature control unit 5 can be set higher than the heat resistance temperature of the permeation pressure sensor 4, and since the permeation pressure sensor 4 does not require heat resistance, a pressure sensor with low heat resistance can be used. become.
The permeation pressure sensor 4 is connected to a personal computer 29 through an amplifier 22 and measures the pressure of the measurement gas 11 that has permeated through the sample film 10 to obtain the gas permeability. Further, the permeation pressure sensor 4 is provided with a temperature sensor 13 so that the temperature of the measurement gas 11 in the permeation pressure sensor 4 including the pipe 19 can be measured.
[0014]
A stirring fan 21 is provided in the room temperature portion 30, and the heat transmitted from the temperature control unit 5 to the permeation pressure sensor 4 through the pipe 19 is reduced by agitating the air around the permeation pressure sensor 4. The temperature of the portion 4 is configured to be kept substantially constant.
[0015]
Further, the room temperature portion 30 is provided with a temperature control device for controlling the temperature of the permeation pressure sensor 4 side (the permeation pressure sensor 4 and the pipe 19) within the heat resistance temperature of the permeation pressure sensor 4, and the temperature control unit 5 and the permeation pressure sensor 4 side. When there is a temperature difference, the measurement pressure by the permeation pressure sensor 4 can be corrected to obtain the measurement gas permeability. When the test temperature is within the heat resistance temperature of the permeation pressure sensor 4, the temperature control device can control the permeation pressure sensor 4 side to the test temperature, and change the permeability of the measurement gas from the pressure measured by the permeation pressure sensor 4. You can also ask directly. On the other hand, when the test temperature is other than the heat resistance temperature of the permeation pressure sensor 4, the temperature control device controls the temperature of the permeation pressure sensor 4 within the heat resistance temperature of the permeation pressure sensor 4. The temperature difference on the sensor 4 side can be reduced, and the error due to the correction of the measured pressure can be reduced.
[0016]
The vacuum pump 3 is connected to a pipe 25 via a pipe 26 provided with a valve 16 so that the primary side of the sample film 10 can be depressurized and is connected via a pipe 27 provided with a valve 15. 19, the secondary side of the sample film 10 can be depressurized. Further, the pipes 26 and 27 are provided with an exhaust pipe 28 provided with a valve 18 so that the measurement gas 11 can be exhausted.
[0017]
Next, in the embodiment shown in FIG. 1, a measurement procedure for gas permeability will be described.
(1) The sample film 10 is set in the chamber 1 and the chamber 1 is sealed.
(2) Close all the valves 14, 15, 16, 18 and turn on the vacuum pump 3.
(3) Open the valve 15 and depressurize the secondary side of the sample film 10 until the indicated value of the permeation pressure sensor 4 reaches a certain vacuum value.
(4) The valve 16 is opened, and the primary side and the secondary side of the sample film 10 are depressurized until the indicated values of the permeation pressure sensor 4 and the tank pressure sensor 8 become constant vacuum values.
(5) The valves 15 and 16 are closed to finish the pressure reducing operation.
(6) The valve 14 is opened, the measurement gas 11 is supplied from the measurement gas source 9 to the measurement gas tank 2, the valve 14 is closed when the indicated value of the tank pressure sensor 8 rises to the test pressure, and the gas permeability measurement test is performed. Be started.
(7) The test ends when the secondary side pressure change rate reaches a constant state (steady state).
(8) After completion of the test, the vacuum pump is stopped, the valves 15, 16, 18 are opened, and the measurement gas 11 is exhausted.
[0018]
Then, temperature correction is performed from the pressure P [kPa] of the secondary measurement gas (V 1 + V 2 ) measured by the permeation pressure sensor 4 to obtain a gas transmission rate (GTR) of the sample film 10. .
At this time, the volume of the secondary side cell 7 (not including the density of the filter paper 20) is V 1 [cm 3 ], the volume of the secondary side pipe 19 and the permeation pressure sensor 4 is V 2 [cm 3 ], and the temperature sensor If the measured temperature of 12 is T 1 [K] and the measured temperature of the temperature sensor 13 is T 2 [K], the ideal of the secondary measurement gas (V 1 + V 2 ) converted to the ideal temperature T 0 [273K]. The pressure P ′ [kPa] can be obtained by the equation shown in Equation 1.
[0019]
[Expression 1]
Figure 0003845055
[0020]
From the change in the ideal pressure P ′ [kPa] in the steady state and the pressure difference P d [kPa] between the measurement gas 11 on the primary side and the measurement gas on the secondary side with respect to the sample film 10, the gas permeation of the sample film 10. The rate GTR can be obtained by the equation shown in Equation 2.
[0021]
[Expression 2]
Figure 0003845055
[0022]
Next, the embodiment shown in FIG. 2 will be described.
Reference numeral 17 denotes a valve, which is provided in a pipe 24 connecting the measurement gas tank 2 and the chamber 1. The valve 17 is controlled to be opened and closed by a personal computer 29, and is configured so that the timing at which the measurement gas 11 having the test pressure stored in the measurement gas tank 2 is applied to the sample film 10 can be controlled. Other configurations are the same as those of the embodiment shown in FIG.
[0023]
In the embodiment shown in FIG. 2, a procedure for measuring gas permeability and diffusion coefficient will be described.
(1) The sample film 10 is set in the chamber 1 and the chamber 1 is sealed.
(2) Close all the valves 14, 15, 16, 17, 18 and turn on the vacuum pump 3.
(3) Open the valve 15 and depressurize the secondary side of the sample film 10 until the indicated value of the permeation pressure sensor 4 reaches a certain vacuum value.
(4) The valves 16 and 17 are opened, and the primary side and the secondary side of the sample film 10 are depressurized until the indicated values of the permeation pressure sensor 4 and the tank pressure sensor 8 become constant vacuum values.
(5) The valves 15, 16, and 17 are closed to finish the pressure reducing operation.
(6) The valve 14 is opened, the measurement gas 11 is supplied from the measurement gas source 9 to the measurement gas tank 2, and the valve 14 is closed when the indicated value of the tank pressure sensor 8 rises to the test pressure.
(7) The valve 17 is opened under the control of the personal computer 29, the test is started from the moment it is opened, the pressure with respect to the elapsed time is measured, and the test is terminated when the pressure change rate becomes a constant state.
(8) After completion of the test, the vacuum pump is stopped, the valves 15, 16, 18 are opened, and the measurement gas 11 is exhausted.
[0024]
When the measurement gas 11 of the test pressure is added to the primary side of the sample film 11 in this procedure (7), the measurement gas 11 diffuses into the sample film 10 and gradually begins to permeate, and the permeation pressure is shown in FIG. The measured pressure of the sensor 4 gradually increases after the start of the test, and then the pressure change rate becomes constant and changes linearly with time. Using the measurement pressure of the permeation pressure sensor 4 in the linearly changing portion, the gas permeability GTR of the sample film 10 can be obtained in the same manner as in the embodiment of FIG.
[0025]
Further, the lag time θ is obtained from the intersection of the linear portion of the change curve of the measured pressure shown in FIG. 3 and the time axis, and the diffusion coefficient D can be obtained from the equation shown in Equation 3.
[0026]
[Equation 3]
Figure 0003845055
[0027]
Further, since the gas permeability GTR is a product of the diffusion coefficient D and the solubility coefficient S (GTR = S × D), the solubility coefficient S can be obtained by obtaining the gas permeability GTR and the diffusion coefficient D.
[0028]
In the embodiment shown in FIG. 1 or FIG. 2, when the volume in the pipe 19 connecting the permeation pressure sensor 4 and the chamber 1 is 1% or more of the secondary side volume (V 1 + V 2 ), the permeation pressure sensor The portion is divided into the pipe 19 and the permeation pressure sensor 4 so that the measured pressure is temperature-corrected.
Temperature of the pipe 19, since changes from the temperature T 1 [K] of the temperature control unit 5 to the temperature T 2 [K] of the transmitted pressure sensor 4, the volume of the pipe 19 is 1% or more of the volume of the secondary side In this case, since the conversion error is large in the conversion formula shown in the above formula 1, the volume V 2 of the permeation pressure sensor portion is divided into the pipe 19 and the permeation pressure sensor 4, and the second order is calculated by the conversion formula shown in the formula 4. The pressure of the measurement gas 11 on the side is converted into an ideal pressure P ′ [kPa].
The volume of the permeation pressure sensor 4 is V 2 ′ [cm 3 ], the volume of the pipe 19 is V 3 [cm 3 ], and the temperature of the pipe 19 is T 3 (T 3 = (T 1 + T 2 ) / 2) [K]. It is said.
[0029]
[Expression 4]
Figure 0003845055
[0030]
For example, when the volume of each part on the secondary side of the sample film 10 is V 1 = 1 [cm 3 ] and V 2 ′ = 3.5 [cm 3 ], the inner diameter Φ = 2 [mm] and the length L = When the pipe 19 of 10 [cm] is used, the volume (V 3 ) in the pipe 19 is 6.25% of the secondary volume (V 1 + V 2 ′ + V 3 ). The temperature of the measured pressure is corrected by
Here, since the calculated temperature T 3 as a linear gradient of temperature change of the pipe 19, the error between the actual temperature gradient of the pipe 19 occurs. The influence of the error of the temperature T 3 on the ideal pressure P ′ depends on the coefficient (V 3 / (V 1 + V 2 ′ + V 3 )) of T 3 in the conversion formula shown in Equation 4, so that the error caused thereby it is preferable to a smaller to reduce the V 3.
[0031]
【The invention's effect】
As described above, according to the gas permeability measuring device of the present invention, a chamber composed of a pair of cells on which a sample film is mounted, a measurement gas tank for adding a measurement gas into one primary cell of the sample film, A gas permeability measuring device comprising a vacuum pump for reducing the pressure in the other secondary cell of the sample film, and a permeation pressure sensor for measuring the pressure of the measurement gas that has permeated the sample film, wherein the chamber and the measurement A temperature control unit for controlling the temperature of the gas tank is provided, and a measurement gas permeability is obtained by correcting the measurement pressure by the permeation pressure sensor with the temperature of the temperature control unit and the permeation pressure sensor. Thus, the temperature of the chamber and the measurement gas tank is controlled by a temperature controller, while the portion of the permeation pressure sensor is the room temperature or the permeation pressure sensor. By controlling the temperature within the thermal temperature, it is possible to control the temperature of the measuring gas tank and the chamber without being influenced by the heat resistance temperature of the transmission pressure sensor. In addition, since the temperature control unit becomes smaller by not controlling the temperature of the entire apparatus, the temperature control time can be shortened, and the time required for the entire gas permeability test can be shortened.
[0032]
In addition, the present invention has a configuration according to claim 1 in which a temperature sensor is provided in the temperature control unit and the permeation pressure sensor, thereby measuring the temperature of the temperature control unit and the permeation pressure sensor. Thus, there is an effect that the measurement gas permeability can be obtained by correcting the measurement pressure by the permeation pressure sensor.
[0033]
In the present invention, when the volume in the pipe connecting the permeation pressure sensor and the chamber is 1% or more of the volume on the secondary side, the permeation pressure sensor portion is divided into the pipe and the permeation pressure sensor. The measurement pressure due to the temperature gradient of the pipe when the volume in the pipe is 1% or more of the volume on the secondary side by having the configuration according to claim 1 or 2 wherein the measurement pressure is temperature-corrected. It is possible to obtain the measurement rate of the measurement gas by reducing the correction error.
[0034]
In addition, the present invention includes a temperature control device that controls the temperature of the permeation pressure sensor within a heat resistant temperature of the permeation pressure sensor, and the permeation pressure sensor when there is a temperature difference between the temperature control unit and the permeation pressure sensor. The temperature control unit and the permeation pressure sensor side are separately temperature controlled by having the configuration according to any one of claims 1 to 3, wherein the measurement gas permeability is corrected to obtain the measurement gas permeability. Can be measured at a test temperature equal to or higher than the heat resistance temperature of the permeation pressure sensor, and temperature control can be performed so that the temperature difference between the temperature control unit and the permeation pressure sensor is small, so that the correction level is reduced and measurement accuracy is improved. Can be made. In particular, when the test temperature is within the heat resistance temperature of the permeation pressure sensor, there is an effect that the measurement accuracy can be improved by further reducing the temperature difference.
[0035]
In addition, the present invention has a configuration according to any one of claims 1 to 3 in which a valve is provided between the measurement gas tank and the chamber, thereby opening and closing the valve provided between the measurement gas tank and the chamber. By controlling, there is an effect that it is possible to control the timing at which the measurement gas having the test pressure stored in the measurement gas tank is applied to the sample film.
[Brief description of the drawings]
FIG. 1 is a block diagram showing an embodiment of the gas permeability measuring apparatus of the present invention. FIG. 2 is a block diagram showing another embodiment. FIG. 3 is a diagram showing a change in pressure on the secondary side of a sample membrane. Explanation】
DESCRIPTION OF SYMBOLS 1 Chamber 2 Measurement gas tank 3 Vacuum pump 4 Transmission pressure sensor 5 Temperature control part 6 Primary side cell 7 Secondary side cell 8 Tank pressure sensor 9 Measurement gas source 10 Sample film 11 Measurement gas 12, 13 Temperature sensors 14, 15, 16, 17, 18 Valve 19 Piping 20 Filter paper 21 Stirring fan 22 Amplifier 23 Recesses 24, 25, 26, 27 Piping 28 Exhaust pipe 29 PC 30 Room temperature section

Claims (5)

試料膜を装着する一対のセルからなるチャンバーと、前記試料膜の一方の一次側セル内に測定ガスを加える測定ガスタンクと、前記試料膜の他方の二次側セル内を減圧する真空ポンプと、前記試料膜を透過した測定ガスの圧力を測定する透過圧力センサーとからなるガス透過率測定装置であって、前記チャンバーと前記測定ガスタンクの温度を制御する温度制御部を備え、前記透過圧力センサーによる測定圧力を前記温度制御部と前記透過圧力センサーの部分の温度により補正して測定ガスの透過率を求めるようにしたガス透過率測定装置。A chamber composed of a pair of cells on which the sample film is mounted, a measurement gas tank for adding a measurement gas into one primary side cell of the sample film, a vacuum pump for depressurizing the other secondary side cell of the sample film, A gas permeability measuring device comprising a permeation pressure sensor for measuring the pressure of a measurement gas that has permeated the sample membrane, comprising a temperature control unit that controls the temperature of the chamber and the measurement gas tank, and the permeation pressure sensor A gas permeability measuring device that obtains the measured gas permeability by correcting the measured pressure with the temperature of the temperature controller and the permeation pressure sensor. 前記温度制御部と前記透過圧力センサーの部分に温度センサーを設けた請求項１に記載のガス透過率測定装置。The gas permeability measuring apparatus according to claim 1, wherein a temperature sensor is provided in a portion of the temperature control unit and the permeation pressure sensor. 前記透過圧力センサーと前記チャンバーを接続する配管内の体積が二次側の体積の１％以上の場合に、前記透過圧力センサーの部分を配管と透過圧力センサーに分けて前記測定圧力を温度補正するようにした請求項１又は２に記載のガス透過率測定装置。When the volume in the pipe connecting the permeation pressure sensor and the chamber is 1% or more of the volume on the secondary side, the permeation pressure sensor portion is divided into the pipe and the permeation pressure sensor, and the measured pressure is temperature corrected. The gas permeability measuring apparatus according to claim 1 or 2, wherein the gas permeability measuring apparatus according to claim 1 or 2 is used. 前記透過圧力センサー側を透過圧力センサーの耐熱温度以内に温度制御する温度制御装置を備え、前記温度制御部と前記透過圧力センサー側に温度差がある場合に前記透過圧力センサーによる測定圧力を補正して測定ガスの透過率を求めるようにした請求項１乃至３のいずれかに記載のガス透過率測定装置。A temperature control device is provided for controlling the temperature of the permeation pressure sensor within the permissible temperature of the permeation pressure sensor, and corrects the measurement pressure by the permeation pressure sensor when there is a temperature difference between the temperature control unit and the permeation pressure sensor side. The gas permeability measuring device according to claim 1, wherein the permeability of the measurement gas is obtained. 前記測定ガスタンクと前記チャンバーの間に外部制御で開閉可能なバルブを設けた請求項１乃至４のいずれかに記載のガス透過率測定装置。The gas permeability measuring device according to any one of claims 1 to 4, wherein a valve that can be opened and closed by external control is provided between the measurement gas tank and the chamber.
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