JP7524148B2 - 生体電極組成物、生体電極、生体電極の製造方法、高分子化合物及び複合体 - Google Patents
生体電極組成物、生体電極、生体電極の製造方法、高分子化合物及び複合体 Download PDFInfo
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- JP7524148B2 JP7524148B2 JP2021151665A JP2021151665A JP7524148B2 JP 7524148 B2 JP7524148 B2 JP 7524148B2 JP 2021151665 A JP2021151665 A JP 2021151665A JP 2021151665 A JP2021151665 A JP 2021151665A JP 7524148 B2 JP7524148 B2 JP 7524148B2
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Images
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
- A61B5/251—Means for maintaining electrode contact with the body
- A61B5/257—Means for maintaining electrode contact with the body using adhesive means, e.g. adhesive pads or tapes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
- A61B5/263—Bioelectric electrodes therefor characterised by the electrode materials
-
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Description
生体電極組成物であって、(A)イオン性の高分子材料と粒子との複合体を含有し、
前記(A)成分が、フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマーと結合する粒子を含有するものである生体電極組成物を提供する。
生体電極組成物であって、(A)イオン性の高分子材料と粒子との複合体を含有し、
前記(A)成分が、フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマーと結合する粒子を含有するものである生体電極組成物である。
本発明の生体電極組成物は、(A)イオン性の高分子材料と粒子の複合体及び好ましくは(B)粘着性樹脂を含有するものである。以下、各成分について、更に詳細に説明する。なお、以下において、上記イオン性の高分子材料と粒子との複合体を「(A)成分」、粘着性樹脂を「(B)成分」、ブレンドイオン性ポリマーを「(C)成分」、導電性粉末を「(D)成分」、有機溶剤を「(E)成分」、その他の添加剤を「(F)成分」ともいう。
本発明の生体電極組成物において、(A)イオン性の高分子材料と粒子との複合体塩は、フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマー(イオン性ポリマー)と結合する粒子である。上記の塩はN-カルボニルフルオロスルホンアミドの塩であることが特開2018-70775号に示される様にイオン導電性が高く特に好ましい。好ましくは、上記ポリマーが更にアルコキシシリル基を有する繰り返し単位を有し、上記ポリマーが反応によって粒子と結合した材料である。
本発明におけるイオン性ポリマーとしては、前記繰り返し単位a1~a7に加えて、下記一般式(4)記載のアルコキシシリル基を有する繰り返し単位bを含むことが好ましい。
本発明の生体電極組成物の(A)成分中のイオン性ポリマーには、上記の繰り返し単位a1~a7、b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繰り返し単位cを共重合することも出来る。グライム鎖を有する繰り返し単位cを得るためのモノマーは、具体的には下記に例示することが出来る。グライム鎖を有する繰り返し単位を共重合することによって、本発明の生体電極がドライ電極の場合、肌から放出されるイオンのドライ電極膜内での移動を助長し、ドライ電極の感度を高めることが出来る。
本発明の生体電極組成物の(A)成分中のイオン性ポリマーには、上記の繰り返し単位a1~a7、b、cに加えて、導電性を向上させるために、ヒドロキシ基、カルボキシル基、アンモニウム塩、ベタイン、アミド基、ピロリドン、ラクトン環、ラクタム環、スルトン環、スルホン酸のナトリウム塩、スルホン酸のカリウム塩を有する親水性の繰り返し単位dを共重合することも出来る。親水性の繰り返し単位dを得るためのモノマーは、具体的には下記に例示することが出来る。これらの親水性基を含有する繰り返し単位を共重合することによって、肌から放出されるイオンの感受性を高め、ドライ電極の感度を高めることが出来る。
本発明の生体電極組成物に配合される(B)粘着性樹脂は、上記の(A)イオン性の高分子材料と粒子との複合体(塩)と相溶して塩の溶出を防ぎ、金属粉、炭素粉、珪素粉、チタン酸リチウム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る。(A)成分中のイオン性の高分子材料が粘着性を有している場合は、(B)粘着性樹脂は必ずしも必要ではない。なお、(B)成分の樹脂は、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、シリコーン系、アクリル系、及びウレタン系の樹脂から選ばれる1種以上であることが好ましい。
本発明の生体電極組成物には、(A)成分以外に別途イオン性のポリマー(ブレンドイオン性ポリマー)を添加することが出来る。ブレンドイオン性ポリマーの繰り返し単位は上記(A)成分中のイオン性ポリマーのところで説明したもの、特に上記一般式(2)で示されるものを使うことが出来る。ブレンドイオン性ポリマーの添加量は、(B)成分の樹脂100質量部に対して0.1~100質量部の範囲とすることが好ましい。
[金属粉]
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、(D)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もできる。金属粉の添加量は、(B)成分の樹脂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。
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、黒鉛、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、(B)成分の樹脂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、イオン受容の感度を高めるために、珪素粉を添加することが出来る。珪素粉としては、珪素、一酸化珪素、炭化珪素からなる粉体を挙げることが出来る。粉体の粒子径は100μmよりも小さい方が好ましく、より好ましくは1μm以下である。より細かい粒子の方が表面積が大きいために、たくさんのイオンを受け取ることが出来、高感度な生体電極となる。珪素粉の添加量は、(B)成分の樹脂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、イオン受容の感度を高めるために、チタン酸リチウム粉を添加することが出来る。チタン酸リチウム粉としては、Li2TiO3、LiTiO2、スピネル構造のLi4Ti5O12の分子式を挙げることが出来、スピネル構造品が好ましい。又、カーボンと複合化したチタン酸リチウム粒子を用いることも出来る。粉体の粒子径は100μmよりも小さい方が好ましく、より好ましくは1μm以下である。より細かい粒子の方が表面積が大きいために、たくさんのイオンを受け取ることが出来、高感度な生体電極となる。これらは炭素との複合粉であっても良い。チタン酸リチウム粉の添加量は、(B)成分の樹脂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。
また、本発明の生体電極組成物には、(E)成分として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モノメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノプロピルエーテル、ジエチレングリコールモノブチルエーテル、ジエチレングリコールモノペンチルエーテル、ジエチレングリコールモノヘプチルエーテル、ジエチレングリコールジエチルエーテル、ジエチレングリコールジプロピルエーテル、ジエチレングリコールジブチルエーテル、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、水などを挙げることができる。
本発明の生体電極組成物には、(B)成分のところで述べた白金触媒や付加反応制御剤、ラジカル発生剤の他、架橋剤、架橋触媒、イオン性添加剤、それに加えてシリカ粒子やポリエーテルシリコーン、ポリグリセリンシリコーンを混合することも出来る。シリカ粒子は表面が親水性であり、親水性のイオン性ポリマーやポリエーテルシリコーンやポリグリセリンシリコーンとのなじみが良く、イオン性ポリマーやポリエーテルシリコーンやポリグリセリンシリコーンの疎水性のシリコーン粘着剤での分散性を向上させることが出来る。シリカ粒子は乾式、湿式どちらでも好ましく用いることが出来る。
本発明の生体電極組成物にはエポキシ系の架橋剤を添加することも出来る。この場合の架橋剤は、エポキシ基やオキセタン基を1分子内に複数有する化合物である。添加量としては、(B)成分の樹脂100質量部に対して1~30質量部である。
本発明の生体電極組成物にはエポキシ基やオキセタン基を架橋するための触媒を添加することも出来る。この場合の触媒は、特表2019-503406号中、段落0027~0029に記載されているものを用いることが出来る。添加量としては、(B)成分の樹脂100質量部に対して0.01~10質量部である。
本発明の生体電極組成物には、イオン導電性を上げるためのイオン性添加剤を添加することが出来る。生体適合性を考慮すると、塩化ナトリウム、塩化カリウム、塩化カルシウム、塩化マグネシウム、サッカリンナトリウム塩、アセスルファムカリウム、カルボン酸ナトリウム、カルボン酸カリウム、カルボン酸カルシウム、スルホン酸ナトリウム、スルホン酸カリウム、スルホン酸カルシウム、リン酸ナトリウム、リン酸カリウム、リン酸カルシウム、リン酸マグネシウム、ベタイン、特開2018-44147号公開、特開2018-59050号公開、特開2018-59052号公開、特開2018-130534号公開の塩を挙げることが出来る。
本発明の生体電極組成物において、膜の保湿性を向上させて肌から放出されるイオンの感受性とイオン導電性を向上させるために、ポリグリセリン構造を有するシリコーン化合物を添加することも出来る。ポリグリセリン構造を有するシリコーン化合物の配合量は、(A)成分と(B)成分の合計100質量部に対して0.01~100質量部とすることが好ましく、0.5~60質量部とすることがより好ましい。また、ポリグリセリン構造を有するシリコーン化合物は、1種を単独で使用してもよいし、2種以上を混合で使用してもよい。
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、(E)成分、その他(F)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。
生体電極組成物溶液にイオン性材料(導電性材料)として配合したイオン性ポリマー1~14は、以下のようにして合成した。各モノマーの30質量%シクロペンタノン溶液を反応容器に入れて混合し、反応容器を窒素雰囲気下-70℃まで冷却し、減圧脱気、窒素ブローを3回繰り返した。室温まで昇温後、重合開始剤としてアゾビスイソブチロニトリル(AIBN)をモノマー全体1モルに対して0.02モル加え、60℃まで昇温後、15時間反応させた。得られたポリマーの組成は、溶剤を乾燥後、1H-NMRにより確認した。また、得られたポリマーの分子量(Mw)及び分散度(Mw/Mn)は、溶剤としてテトラヒドロフラン(THF)を用いたゲルパーミエーションクロマトグラフィー(GPC)により確認した。このようにして合成したアルコキシシリル基を有するイオン性ポリマー1~14を以下に示す。
モレキュラーシーブで乾燥したメチルイソブチルケトン(MIBK)100g中に、乾式シリカ(SIGMA-Aldrich社、サイズ5~20nm)5gを添加して1日攪拌し、その中に30重量%濃度のイオン性ポリマー1のシクロペンタノン溶液の15gを滴下し、室温で20時間攪拌の後に溶剤を乾燥して、イオン性ポリマー1がペンダントされたイオン性ポリマー1複合シリカを合成した。
(シロキサン化合物1)
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。
(シロキサン化合物2)
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。
(シロキサン化合物3)
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。
(シロキサン化合物4)
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。
EDE:ジエチレングリコールジエチルエーテル
アイソパーG:イソパラフィン系溶剤 スタンダード石油製
アイソパーM:イソパラフィン系溶剤 スタンダード石油製
金属粉 銀粉:Sigma-Aldrich社製 銀フレーク 直径10μm
チタン酸リチウム粉、スピネル:Sigma-Aldrich社製 サイズ200nm以下
ラジカル発生剤:BASF社製 イルガキュアTPO
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Li-400
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~表3に記載の組成で、イオン性ポリマー複合粒子、樹脂、イオン性ポリマー、有機溶剤、及び添加剤(ラジカル発生剤、白金触媒、導電性向上剤等)をブレンドし、生体電極組成物溶液(生体電極組成物溶液1~29、比較生体電極組成物溶液1~4)を調製した。
図3に示すように、ビーマス(Bemis)社の熱可塑性ウレタン(TPU)フィルム20のST-604上に、スクリーン印刷によって藤倉化成製の導電ペースト、ドータイトFA-333をコートし、120℃で10分間オーブン中でベークして円の直径が2cmの鍵穴状の導電パターン2を印刷した。その上の円形部分に重ねて、表1~3記載の生体電極組成物溶液をスクリーン印刷で塗布し、室温で10分風乾した後、オーブンを用いて125℃で10分間ベークして溶剤を蒸発させ硬化させ生体接触層3を形成し、生体電極1とした。更には、実施例14~18では、窒素雰囲気下でキセノンランプを200mJ/cm2照射して硬化させた。次に図4に示すように、生体電極1が印刷された熱可塑性ウレタンフィルム20を切り取って、両面テープ21を貼り付けて、1つの組成物溶液につき生体電極サンプル10を3個作製した。
上記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4に示す。
生体電極の導電ペーストによる導電配線パターンとオムロンヘルスケア((株))製携帯心電計HCG-901とを導電線で結び、心電計のプラス電極を図5中の人体のLAの場所、マイナス電極をLLの場所、アースをRAの場所に貼り付けた。貼り付け直後に心電図の測定を開始し、図6に示されるP、Q、R、S、T波からなる心電図波形(ECGシグナル)が現れるまでの時間を計測した。結果を表4に示す。
4…イオン性複合体、 5…ブレンドイオン性ポリマー、 6…粘着性樹脂、
7…生体、 10…生体電極サンプル、 20…熱可塑性ウレタンフィルム、
21…両面テープ。
Claims (27)
- 生体電極組成物であって、(A)イオン性の高分子材料と粒子との複合体を含有し、
前記(A)成分が、フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマーと結合する粒子を含有し、前記繰り返し単位が、下記一般式(1)-1から(1)-4のいずれかで示される構造を有するものであることを特徴とする生体電極組成物。
- 前記粒子が直径2nm~50μmの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。
- 前記粒子が珪素材料粒子、アルミナ粒子、チタニア粒子、ジルコニア粒子、チタン酸リチウム粒子、酸化ハフニウム粒子、酸化亜鉛粒子、ゲルマニウム粒子、酸化ゲルマニウム粒子、スズ粒子、酸化スズ粒子、酸化アンチモン粒子、酸化ストロンチウム粒子、酸化タングステン粒子、酸化ビスマス粒子、酸化イットリウム粒子、酸化イッテルビウム粒子、酸化ガドリウム粒子、酸化インジウム粒子、酸化モリブデン粒子、酸化スカンジウム粒子のうちのいずれか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。
- 前記フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位が、下記一般式(2)記載の繰り返し単位a1~a7から選ばれる1種以上であることを特徴とする請求項1から請求項3のいずれか一項に記載の生体電極組成物。
- 前記(A)成分において前記粒子が珪素材料粒子であり、前記(A)成分が珪素材料粒子100質量部に対して前記アルコキシシリル基を有するポリマー5質量部以上を反応させたものであることを特徴とする請求項5に記載の生体電極組成物。
- 前記(A)成分が、前記アンモニウム塩を構成するアンモニウムイオンとして、下記一般式(3)で示されるアンモニウムイオン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6のいずれか一項に記載の生体電極組成物。
- 更に、(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から請求項7のいずれか一項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8に記載の生体電極組成物。
- 前記(B)成分として、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8又は請求項9に記載の生体電極組成物。
- 前記(B)成分として、更に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を含有するものであることを特徴とする請求項10に記載の生体電極組成物。
- 更に(C)成分として、イオン性の繰り返し単位を有する高分子化合物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11のいずれか一項に記載の生体電極組成物。
- 生体電極組成物であって、(A)イオン性の高分子材料と粒子との複合体を含有し、
前記(A)成分が、フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマーと結合する粒子を含有し、更に(C)成分として、イオン性の繰り返し単位を有する高分子化合物を含有するものであることを特徴とする生体電極組成物。 - 前記(C)成分の前記イオン性の繰り返し単位が、下記一般式(2)に記載のフルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、及び銀塩から選ばれる構造を有する繰り返し単位を含有することを特徴とする請求項12又は請求項13に記載の生体電極組成物。
- 更に(D)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14のいずれか一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15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15又は請求項16に記載の生体電極組成物。
- 前記金属粉が、銀粉であることを特徴とする請求項17に記載の生体電極組成物。
- 更に(E)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18のいずれか一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19のいずれか一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20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19のいずれか一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22に記載の生体電極の製造方法。
- イオン性の高分子材料と粒子が結合した複合体であって、前記複合体が、フルオロスルホン酸、フルオロスルホンイミド、及びN-カルボニルフルオロスルホンアミドのうちのいずれかのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマーと結合する粒子であり、
前記繰り返し単位が、下記一般式(1)-1から(1)-4のいずれかで示される構造を有するものであることを特徴とする複合体。
- イオン性の高分子材料と粒子が結合した複合体であって、前記複合体が、N-カルボニルフルオロスルホンアミドのアンモニウム塩、リチウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる構造を有する繰り返し単位を有するポリマーと結合する粒子であることを特徴とする請求項24に記載の複合体。
- 前記粒子が直径2nm~50μmのものであることを特徴とする請求項24又は請求項25に記載の複合体。
- 前記粒子が珪素材料粒子、アルミナ粒子、チタニア粒子、ジルコニア粒子、チタン酸リチウム粒子、酸化ハフニウム粒子、酸化亜鉛粒子、ゲルマニウム粒子、酸化ゲルマニウム粒子、スズ粒子、酸化スズ粒子、酸化アンチモン粒子、酸化ストロンチウム粒子、酸化タングステン粒子、酸化ビスマス粒子、酸化イットリウム粒子、酸化イッテルビウム粒子、酸化ガドリウム粒子、酸化インジウム粒子、酸化モリブデン粒子、酸化スカンジウム粒子のうちのいずれかであることを特徴とする請求項24から請求項26のいずれか一項に記載の複合体。
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