JP2020000851A - 生体電極組成物、生体電極、及び生体電極の製造方法 - Google Patents
生体電極組成物、生体電極、及び生体電極の製造方法 Download PDFInfo
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- JP2020000851A JP2020000851A JP2019093509A JP2019093509A JP2020000851A JP 2020000851 A JP2020000851 A JP 2020000851A JP 2019093509 A JP2019093509 A JP 2019093509A JP 2019093509 A JP2019093509 A JP 2019093509A JP 2020000851 A JP2020000851 A JP 2020000851A
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- bioelectrode
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- silicone
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Abstract
Description
本発明の生体電極組成物は、スルホンアミド塩に結合するシリコーンを含有し、かつ、前記スルホンアミド塩が上記一般式(1)で示されるものであることを必須の条件とする。前記生体電極組成物は、前記スルホンアミド塩に結合するシリコーンと、粘着性樹脂とを含有するものであってもよい。前記生体電極組成物は、さらに導電性粉末(カーボン粉、金属粉)を含有することができ、またさらに有機溶剤等を含有することもできる。
本発明の生体電極組成物は、イオン性材料(塩)として(A)成分(スルホンアミド塩に結合するシリコーン)を含有する。前記生体電極組成物に導電性材料として配合されるイオン性材料(塩)は、下記一般式(1)で示されるスルホンアミドのリチウム塩、ナトリウム塩、カリウム塩、銀塩と結合したシリコーン化合物である。なお、以下において、スルホンアミド塩に結合するシリコーンを「スルホンアミド塩シリコーン」ともいう。
本発明の生体電極組成物の(A)成分は、上記の繰り返し単位aに加えて、導電性を向上させるために、グライム鎖を有するシロキサンからなる繰り返し単位bを有することができる。繰り返し単位bとしては、具体的には以下のものを例示することができる。
本発明の生体電極組成物の(A)成分は、上記の繰り返し単位a、bに加えて、(B)成分の粘着性樹脂との混合性を向上させるために、水素原子、アルキル基やアリール基を有するシロキサンからなる繰り返し単位cを有することができる。アルキル基やアリール基は、ヒドロキシ基、ハロゲン原子、エステル基、エーテル基、カルボキシル基、チオール基、(メタ)アクリル基、シアノ基、ニトロ基を有していても良い。繰り返し単位cとしては、具体的には以下のものを例示することができる。
本発明の生体電極組成物は(A)成分に加えて粘着性樹脂を(B)成分として含有することができる。生体電極組成物に配合される(B)成分は、上記の(A)スルホンアミド塩シリコーンと相溶して塩の溶出を防ぎ、カーボン粉や金属粉等の導電性向上剤を保持し、粘着性を発現させるための成分であり、粘着性樹脂からなる。なお、(B)成分は、上述の(A)成分以外の樹脂であればよく、熱硬化性樹脂及び光硬化性樹脂のいずれか、又はこれらの両方であることが好ましく、特には、シリコーン樹脂(シリコーン系樹脂)、(メタ)アクリレート樹脂(アクリル系樹脂)、及びウレタン樹脂(ウレタン系樹脂)から選ばれる1種以上の樹脂であることが好ましい。
本発明の生体電極組成物は、(C)成分としての導電性粉末をさらに含有することができる。導電性粉末としては、導電性を有する粉末であれば特に制限されないが、カーボン粉(カーボン材料)、金属粉が好ましい。本発明の生体電極組成物は、イオン性材料(塩)として(A)成分(スルホンアミド塩に結合するシリコーン)を含有するが、このような導電性粉末(カーボン粉、金属粉)をさらに添加することによって一層導電性を向上させることができる。なお、以下において、導電性粉末を「導電性向上剤」ともいう。
導電性向上剤として、カーボン材料(カーボン粉)を添加することができる。カーボン材料としては、カーボンブラック、カーボンナノチューブ、炭素繊維等を挙げることができる。カーボンナノチューブは単層、多層のいずれであってもよく、表面が有機基で修飾されていても構わない。カーボン材料の添加量は、樹脂100質量部に対して1〜50質量部の範囲とすることが好ましい。
本発明の生体電極組成物には、電子導電性を高めるために、(C)成分として、金、銀、白金、銅、錫、チタン、ニッケル、アルミニウム、タングステン、モリブデン、ルテニウム、クロム、インジウムから選ばれる金属粉を添加することが好ましい。金属粉の添加量は、樹脂100質量部に対して1〜50質量部の範囲とすることが好ましい。
本発明の生体電極組成物は、必要に応じて(D)成分としての添加剤をさらに含有することができる。添加剤としては、上記(A)から(C)成分以外のものであれば特に限定されないが、粘着性付与剤などの前記生体電極組成物の硬化物の伸縮性や粘着性を向上させることができる成分や、ラジカル発生剤、白金触媒などの硬化反応を促進する成分、有機溶剤などの生体電極組成物の取扱いを容易にする成分などを挙げることができる。以下、(D)成分について詳細に説明する。
本発明の生体電極組成物には、生体に対する粘着性を付与するために、粘着性付与剤を添加してもよい。このような粘着性付与剤としては、例えば、シリコーンレジンや非架橋性のシロキサン、非架橋性のポリ(メタ)アクリレート、非架橋性のポリエーテル等を挙げることができる。本発明の生体電極組成物は、必要に応じて(B)成分として粘着性樹脂を含有することができるが、このような粘着性付与剤を添加することによっても、生体に対する粘着性が更に好ましいものとなる。
また、本発明の生体電極組成物には、有機溶剤を添加することができる。有機溶剤としては、具体的には、トルエン、キシレン、クメン、1,2,3−トリメチルベンゼン、1,2,4−トリメチルベンゼン、1,3,5−トリメチルベンゼン、スチレン、αメチルスチレン、ブチルベンゼン、sec−ブチルベンゼン、イソブチルベンゼン、シメン、ジエチルベンゼン、2−エチル−p−キシレン、2−プロピルトルエン、3−プロピルトルエン、4−プロピルトルエン、1,2,3,5−テトラメチルトルエン、1,2,4,5−テトラメチルトルエン、テトラヒドロナフタレン、4−フェニル−1−ブテン、tert−アミルベンゼン、アミルベンゼン、2−tert−ブチルトルエン、3−tert−ブチルトルエン、4−tert−ブチルトルエン、5−イソプロピル−m−キシレン、3−メチルエチルベンゼン、tert−ブチル−3−エチルベンゼン、4−tert−ブチル−o−キシレン、5−tert−ブチル−m−キシレン、tert−ブチル−p−キシレン、1,2−ジイソプロピルベンゼン、1,3−ジイソプロピルベンゼン、1,4−ジイソプロピルベンゼン、ジプロピルベンゼン、ペンタメチルベンゼン、ヘキサメチルベンゼン、ヘキシルベンゼン、1,3,5−トリエチルベンゼン等の芳香族系炭化水素系溶剤、n−ヘプタン、イソヘプタン、3−メチルヘキサン、2,3−ジメチルペンタン、3−エチルペンタン、1,6−ヘプタジエン、5−メチル−1−ヘキシン、ノルボルナン、ノルボルネン、ジシクロペンタジエン、1−メチル−1,4−シクロヘキサジエン、1−ヘプチン、2−ヘプチン、シクロヘプタン、シクロヘプテン、1,3−ジメチルシクロペンタン、エチルシクロペンタン、メチルシクロヘキサン、1−メチル−1−シクロヘキセン、3−メチル−1−シクロヘキセン、メチレンシクロヘキサン、4−メチル−1−シクロヘキセン、2−メチル−1−ヘキセン、2−メチル−2−ヘキセン、1−ヘプテン、2−ヘプテン、3−ヘプテン、n−オクタン、2,2−ジメチルヘキサン、2,3−ジメチルヘキサン、2,4−ジメチルヘキサン、2,5−ジメチルヘキサン、3,3−ジメチルヘキサン、3,4−ジメチルヘキサン、3−エチル−2−メチルペンタン、3−エチル−3−メチルペンタン、2−メチルヘプタン、3−メチルヘプタン、4−メチルヘプタン、2,2,3−トリメチルペンタン、2,2,4−トリメチルペンタン、シクロオクタン、シクロオクテン、1,2−ジメチルシクロヘキサン、1,3−ジメチルシクロヘキサン、1,4−ジメチルシクロヘキサン、エチルシクロヘキサン、ビニルシクロヘキサン、イソプロピルシクロペンタン、2,2−ジメチル−3−ヘキセン、2,4−ジメチル−1−ヘキセン、2,5−ジメチル−1−ヘキセン、2,5−ジメチル−2−ヘキセン、3,3−ジメチル−1−ヘキセン、3,4−ジメチル−1−ヘキセン、4,4−ジメチル−1−ヘキセン、2−エチル−1−ヘキセン、2−メチル−1−ヘプテン、1−オクテン、2−オクテン、3−オクテン、4−オクテン、1,7−オクタジエン、1−オクチン、2−オクチン、3−オクチン、4−オクチン、n−ノナン、2,3−ジメチルヘプタン、2,4−ジメチルヘプタン、2,5−ジメチルヘプタン、3,3−ジメチルヘプタン、3,4−ジメチルヘプタン、3,5−ジメチルヘプタン、4−エチルヘプタン、2−メチルオクタン、3−メチルオクタン、4−メチルオクタン、2,2,4,4−テトラメチルペンタン、2,2,4−トリメチルヘキサン、2,2,5−トリメチルヘキサン、2,2−ジメチル−3−ヘプテン、2,3−ジメチル−3−ヘプテン、2,4−ジメチル−1−ヘプテン、2,6−ジメチル−1−ヘプテン、2,6−ジメチル−3−ヘプテン、3,5−ジメチル−3−ヘプテン、2,4,4−トリメチル−1−ヘキセン、3,5,5−トリメチル−1−ヘキセン、1−エチル−2−メチルシクロヘキサン、1−エチル−3−メチルシクロヘキサン、1−エチル−4−メチルシクロヘキサン、プロピルシクロヘキサン、イソプロピルシクロヘキサン、1,1,3−トリメチルシクロヘキサン、1,1,4−トリメチルシクロヘキサン、1,2,3−トリメチルシクロヘキサン、1,2,4−トリメチルシクロヘキサン、1,3,5−トリメチルシクロヘキサン、アリルシクロヘキサン、ヒドリンダン、1,8−ノナジエン、1−ノニン、2−ノニン、3−ノニン、4−ノニン、1−ノネン、2−ノネン、3−ノネン、4―ノネン、n−デカン、3,3−ジメチルオクタン、3,5−ジメチルオクタン、4,4−ジメチルオクタン、3−エチル−3−メチルヘプタン、2−メチルノナン、3−メチルノナン、4−メチルノナン、tert−ブチルシクロヘキサン、ブチルシクロヘキサン、イソブチルシクロヘキサン、4−イソプロピル−1−メチルシクロヘキサン、ペンチルシクロペンタン、1,1,3,5−テトラメチルシクロヘキサン、シクロドデカン、1−デセン、2−デセン、3−デセン、4−デセン、5−デセン、1,9−デカジエン、デカヒドロナフタレン、1−デシン、2−デシン、3−デシン、4−デシン、5−デシン、1,5,9−デカトリエン、2,6−ジメチル−2,4,6−オクタトリエン、リモネン、ミルセン、1,2,3,4,5−ペンタメチルシクロペンタジエン、α−フェランドレン、ピネン、テルピネン、テトラヒドロジシクロペンタジエン、5,6−ジヒドロジシクロペンタジエン、1,4−デカジイン、1,5−デカジイン、1,9−デカジイン、2,8−デカジイン、4,6−デカジイン、n−ウンデカン、アミルシクロヘキサン、1−ウンデセン、1,10−ウンデカジエン、1−ウンデシン、3−ウンデシン、5−ウンデシン、トリシクロ[6.2.1.02,7]ウンデカ−4−エン、n−ドデカン、2−メチルウンデカン、3−メチルウンデカン、4−メチルウンデカン、5−メチルウンデカン、2,2,4,6,6−ペンタメチルヘプタン、1,3−ジメチルアダマンタン、1−エチルアダマンタン、1,5,9−シクロドデカトリエン、1,2,4−トリビニルシクロヘキサン、イソパラフィン等の脂肪族炭化水素系溶剤、シクロヘキサノン、シクロペンタノン、2−オクタノン、2−ノナノン、2−ヘプタノン、3−ヘプタノン、4−ヘプタノン、2−ヘキサノン、3−ヘキサノン、ジイソブチルケトン、メチルシクロヘキサノン、メチルn−ペンチルケトン等のケトン系溶剤、3−メトキシブタノール、3−メチル−3−メトキシブタノール、1−メトキシ−2−プロパノール、1−エトキシ−2−プロパノール等のアルコール系溶剤、プロピレングリコールモノメチルエーテル、エチレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、エチレングリコールモノエチルエーテル、プロピレングリコールジメチルエーテル、ジエチレングリコールジメチルエーテル、ジイソプロピルエーテル、ジイソブチルエーテル、ジイソペンチルエーテル、ジ−n−ペンチルエーテル、メチルシクロペンチルエーテル、メチルシクロヘキシルエーテル、ジ−n−ブチルエーテル、ジ−secブチルエーテル、ジ−sec−ペンチルエーテル、ジ−tert−アミルエーテル、ジ−n−ヘキシルエーテル、アニソール等のエーテル系溶剤、プロピレングリコールモノメチルエーテルアセテート、プロピレングリコールモノエチルエーテルアセテート、乳酸エチル、ピルビン酸エチル、酢酸ブチル、3−メトキシプロピオン酸メチル、3−エトキシプロピオン酸エチル、酢酸tert−ブチル、プロピオン酸tert−ブチル、プロピレングリコールモノtert−ブチルエーテルアセテート等のエステル系溶剤、γ−ブチロラクトン等のラクトン系溶剤などを挙げることができる。
また、本発明では、導電性基材と該導電性基材上に形成された生体接触層とを有する生体電極であって、前記生体接触層が、上述の本発明の生体電極組成物の硬化物である生体電極を提供する。
本発明の生体電極は、導電性基材を有するものである。この導電性基材は、通常、センサーデバイス等と電気的に接続されており、生体から生体接触層を介して取り出した電気信号をセンサーデバイス等まで伝導させる。
本発明の生体電極は、導電性基材上に形成された生体接触層を有するものである。この生体接触層は、生体電極を使用する際に、実際に生体と接触する部分であり、導電性及び粘着性を有する。生体接触層は、上述の本発明の生体電極組成物の硬化物であり、即ち、上述の(A)成分と、必要に応じて(B)成分、(C)成分、(D)成分を含有する組成物の硬化物からなる粘着性の樹脂層である。
また、本発明では、導電性基材と該導電性基材上に形成された生体接触層とを有する生体電極の製造方法であって、前記導電性基材上に、上述の本発明の生体電極組成物を塗布し、硬化させることで前記生体接触層を形成する生体電極の製造方法を提供する。
Mw=12,800
Mw/Mn=3.34
Mw=11,100
Mw/Mn=2.87
Mw=13,100
Mw/Mn=2.79
Mw=13,500
Mw/Mn=3.87
Mw=13,600
Mw/Mn=3.30
Mw=13,100
Mw/Mn=3.59
30%トルエン溶液での粘度が27,000mPa・sであり、アルケニル基含有量が0.007モル/100gであり、分子鎖末端がSiMe2Vi基で封鎖されたビニル基含有ポリジメチルシロキサンをシロキサン化合物1とした。
Me3SiO0.5単位及びSiO2単位からなるMQレジンのポリシロキサン(Me3SiO0.5単位/SiO2単位=0.8)の60%トルエン溶液をシロキサン化合物2とした。
30%トルエン溶液での粘度が42,000mPa・sであり、アルケニル基含有量が0.007モル/100gであり、分子鎖末端がOHで封鎖されたビニル基含有ポリジメチルシロキサン40質量部、Me3SiO0.5単位及びSiO2単位からなるMQレジンのポリシロキサン(Me3SiO0.5単位/SiO2単位=0.8)の60%トルエン溶液100質量部、及びトルエン26.7質量部からなる溶液を還流させながら4時間加熱後、冷却して、MQレジンにポリジメチルシロキサンを結合させたものをシロキサン化合物3とした。
メチルハイドロジェンシリコーンオイルとして、信越化学工業製 KF−99を用いた。
アクリルポリマー1
Mw=108,000
Mw/Mn=2.32
PGMEA:プロピレングリコール−1−モノメチルエーテル−2−アセテート
PGME:プロピレングリコール−1−モノメチルエーテル
PGEE:プロピレングリコール−1−モノエチルエーテル
金属粉 銀粉:Sigma−Aldrich社製 銀フレーク 直径10μm
金粉:Sigma−Aldrich社製 金粉 直径10μm以下
錫粉:Sigma−Aldrich社製 錫粉 直径45μm以下
チタン粉:Sigma−Aldrich社製 チタン粉 直径45μm以下
銅粉:Sigma−Aldrich社製 銅粉 直径45μm以下
ラジカル発生剤:富士フイルム和光純薬社製 V−601
白金触媒:信越化学工業製 CAT−PL−50T
カーボンブラック:デンカ社製 デンカブラックHS−100
多層カーボンナノチューブ:Sigma−Aldrich社製 直径110〜170nm、長さ5〜9μm
表1及び表2に記載の組成で、イオン性材料(スルホンアミド塩シリコーン、比較塩)、樹脂(粘着性樹脂)、有機溶剤、及びその他の添加剤(ラジカル発生剤、白金触媒、導電性向上剤)をブレンドし、生体電極組成物溶液(生体電極組成物溶液1〜19、比較生体電極組成物溶液1〜5)を調製した。
直径3cm、厚さ0.2mmのアルミニウム製の円板の上にアプリケーターを用いて生体電極組成物溶液を塗布し、室温で6時間風乾した後、オーブンを用いて窒素雰囲気下120℃で30分間ベークして硬化させて、1つの生体電極組成物溶液につき生体電極を4枚作製した。このようにして得られた生体電極は、図3(a)、(b)に示されるように、一方の面には生体接触層3を有し、他方の面には導電性基材としてアルミニウム製の円板8を有するものであった。次に、図3(b)に示されるように、生体接触層で覆われていない側のアルミニウム製の円板8の表面に銅配線9を粘着テープで貼り付けて引き出し電極とし、これをインピーダンス測定装置に接続した。図4に示されるように、人の腕の肌と生体接触層側が接触するように生体電極1’を2枚貼り付けて、その間隔を15cmとした。ソーラトロン社製の交流インピーダンス測定装置SI1260を用い、周波数を変えながら初期インピーダンスを測定した。次に、残りの2枚の生体電極を純水中に1時間浸漬し、水を乾燥させた後、上記と同様の方法で肌上のインピーダンスを測定した。周波数1,000Hzにおけるインピーダンスを表3に示す。
生体電極組成物溶液を、アプリケーターを用いて厚さ100μmのPEN(ポリエチレンナフタレート)基板上に塗布し、室温で6時間風乾後、オーブンを用いて窒素雰囲気下120℃で30分間ベークして硬化させて、粘着フィルムを作製した。この粘着フィルムから25mm幅のテープを切り取り、これをステンレス板(SUS304)に圧着させ、室温で20時間放置した後、引っ張り試験機を用い角度180度、300mm/分の速度で粘着フィルムから作製したテープをステンレス板から引きはがすのに要する力(N/25mm)を測定した。結果を表3に示す。
上記の導電性評価試験で作製した生体電極において、生体接触層の厚さをマイクロメーターを用いて測定した。結果を表3に示す。
4…イオン性シリコーン材料、 5a…金属粉、 5b…カーボン粉、
6…樹脂、 7…生体、 8…アルミニウム製の円板、 9…銅配線。
Claims (16)
- スルホンアミド塩に結合するシリコーンを含有する生体電極組成物であって、前記スルホンアミド塩が下記一般式(1)で示されるものであることを特徴とする生体電極組成物。
- 前記スルホンアミド塩に結合するシリコーンが下記一般式(2)で示される繰り返し単位aを有するものであることを特徴とする請求項1に記載の生体電極組成物。
(式中、R1、Rf、Mは前述の通りであり、R2は炭素数1〜10の直鎖状、分岐状、環状のアルキル基であり、ハロゲン原子で置換されていても良く、又は炭素数6〜10のアリール基である。) - (A)成分としての前記スルホンアミド塩に結合するシリコーンと、(B)成分としての粘着性樹脂を含有するものであることを特徴とする請求項1又は請求項2に記載の生体電極組成物。
- 前記(B)成分が、シリコーン樹脂、(メタ)アクリレート樹脂、ウレタン樹脂から選ばれる1種以上であることを特徴とする請求項3に記載の生体電極組成物。
- 前記(B)成分として、RxSiO(4−x)/2単位(Rは炭素数1〜10の置換又は非置換の一価炭化水素基、xは2.5〜3.5の範囲である。)及びSiO2単位を有するシリコーン樹脂と、アルケニル基を有するジオルガノシロキサンと、SiH基を有するオルガノハイドロジェンポリシロキサンとを含有するものであることを特徴とする請求項3又は請求項4に記載の生体電極組成物。
- 更に(C)成分として、カーボン粉及び/又は金属粉を含有するものであることを特徴とする請求項1から請求項5のいずれか1項に記載の生体電極組成物。
- 前記カーボン粉が、カーボンブラック及びカーボンナノチューブのいずれか又は両方であることを特徴とする請求項6に記載の生体電極組成物。
- 前記金属粉が、金、銀、白金、銅、錫、チタン、ニッケル、アルミニウム、タングステン、モリブデン、ルテニウム、クロム、インジウムから選ばれる金属粉であることを特徴とする請求項6又は請求項7に記載の生体電極組成物。
- 前記金属粉が、銀粉、銅粉、錫粉、チタン粉であることを特徴とする請求項8に記載の生体電極組成物。
- 前記生体電極組成物が、更に(D)成分として有機溶剤を含有するものであることを特徴とする請求項1から請求項9のいずれか1項に記載の生体電極組成物。
- 導電性基材と該導電性基材上に形成された生体接触層とを有する生体電極であって、前記生体接触層が、請求項1から請求項10のいずれか1項に記載の生体電極組成物の硬化物であることを特徴とする生体電極。
- 前記導電性基材が、金、銀、塩化銀、白金、アルミニウム、マグネシウム、スズ、タングステン、鉄、銅、ニッケル、ステンレス、クロム、チタン、炭素、及び導電性ポリマーから選ばれる1種以上を含むものであることを特徴とする請求項11に記載の生体電極。
- 導電性基材と該導電性基材上に形成された生体接触層とを有する生体電極の製造方法であって、
前記導電性基材上に、請求項1から請求項10のいずれか1項に記載の生体電極組成物を塗布し、硬化させることで前記生体接触層を形成することを特徴とする生体電極の製造方法。 - 前記導電性基材として、金、銀、塩化銀、白金、アルミニウム、マグネシウム、スズ、タングステン、鉄、銅、ニッケル、ステンレス、クロム、チタン、炭素、及び導電性ポリマーから選ばれる1種以上を含むものを用いることを特徴とする請求項13に記載の生体電極の製造方法。
- 下記一般式(2)で示される部分構造を有することを特徴とするシリコーン化合物。
- 下記一般式(2)で示される繰り返し単位を有することを特徴とする重量平均分子量1000〜1000000の範囲のシリコーンポリマー。
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