JP7149448B1 - 生体電極、生体電極の製造方法、及び生体信号の測定方法 - Google Patents
生体電極、生体電極の製造方法、及び生体信号の測定方法 Download PDFInfo
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- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- 229920002379 silicone rubber Polymers 0.000 description 1
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- NBPUSGBJDWCHKC-UHFFFAOYSA-M sodium 3-hydroxybutyrate Chemical compound [Na+].CC(O)CC([O-])=O NBPUSGBJDWCHKC-UHFFFAOYSA-M 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
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- KYKFCSHPTAVNJD-UHFFFAOYSA-L sodium adipate Chemical compound [Na+].[Na+].[O-]C(=O)CCCCC([O-])=O KYKFCSHPTAVNJD-UHFFFAOYSA-L 0.000 description 1
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
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- UDWXLZLRRVQONG-UHFFFAOYSA-M sodium hexanoate Chemical compound [Na+].CCCCCC([O-])=O UDWXLZLRRVQONG-UHFFFAOYSA-M 0.000 description 1
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- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 1
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- SJRDNQOIQZOVQD-UHFFFAOYSA-M sodium;2,2-dimethylpropanoate Chemical compound [Na+].CC(C)(C)C([O-])=O SJRDNQOIQZOVQD-UHFFFAOYSA-M 0.000 description 1
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- NWMVPLQDJXJDEW-UHFFFAOYSA-N trimethyl(3-methylpent-1-yn-3-yloxy)silane Chemical compound CCC(C)(C#C)O[Si](C)(C)C NWMVPLQDJXJDEW-UHFFFAOYSA-N 0.000 description 1
- JEJAMASKDTUEBZ-UHFFFAOYSA-N tris(1,1,3-tribromo-2,2-dimethylpropyl) phosphate Chemical compound BrCC(C)(C)C(Br)(Br)OP(=O)(OC(Br)(Br)C(C)(C)CBr)OC(Br)(Br)C(C)(C)CBr JEJAMASKDTUEBZ-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/14—Monomers containing only one unsaturated aliphatic radical containing one ring substituted by heteroatoms or groups containing heteroatoms
- C08F212/30—Sulfur
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- A61B5/257—Means for maintaining electrode contact with the body using adhesive means, e.g. adhesive pads or tapes
- A61B5/259—Means for maintaining electrode contact with the body using adhesive means, e.g. adhesive pads or tapes using conductive adhesive means, e.g. gels
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- A61B5/266—Bioelectric electrodes therefor characterised by the electrode materials containing electrolytes, conductive gels or pastes
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- A61B5/268—Bioelectric electrodes therefor characterised by the electrode materials containing conductive polymers, e.g. PEDOT:PSS polymers
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Abstract
Description
本発明の生体電極は、多孔質の伸縮性基材と、珪素を含有する粘着性の導電膜と、導電路とを有し、前記導電膜が前記多孔質の伸縮性基材の片面に形成されており、前記導電路が前記導電膜に接続し、かつ前記伸縮性基材を貫通し反対側の面に露出しているか、前記伸縮性基材の側面に露出しているものである生体電極である。また、本発明の生体電極は、多孔質膜を貫通する導電路上、又は多孔質膜上の導電路に形成された生体接触層となるシリコーン含有粘着性の導電膜を有するものである。
以下、本発明の生体電極の導電膜を形成する各成分について、更に詳細に説明する。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)イオン性材料(導電性材料)として配合される塩は、(A)のイオン性材料として、フルオロスルホン酸、フルオロスルホンイミド、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、銀塩から選ばれるイオン性の繰り返し単位を有するポリマーを含有することができる。
上記一般式(2)で示される繰り返し単位A1~A7のうち、繰り返し単位A1~A5を得るためのフルオロスルホン酸塩モノマーとしては、具体的には下記のものを例示することができる。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)成分には、上記の繰り返し単位A1~A7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B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B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、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。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)成分には、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、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Cを共重合することも出来る。親水性の繰り返し単位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。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。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)成分には、上記の繰り返し単位A1~A7、B、Cに加えて、粘着能を付与させる繰り返し単位Dを有することが出来る。繰り返し単位Dを得るためのモノマーは、具体的には下記のものを例示することができる。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)成分には、上記の繰り返し単位A1~A7、B、C、Dに加えて、架橋性の繰り返し単位Eを共重合することも出来る。架橋性の繰り返し単位Eはオキシラン環又はオキセタン環を有する繰り返し単位を挙げることが出来る。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)成分には、上記の繰り返し単位A1~A7、B、C、D、Eに加えて、珪素を有する繰り返し単位Fを有することが出来る。繰り返し単位Fを得るためのモノマーは、具体的には、以下のものを例示することができる。
本発明の生体電極に用いられる導電膜を形成するための材料の(A)成分には、上記の繰り返し単位A1~A7、B、C、D、E、Fに加えて、フッ素を有する繰り返し単位Gを有することが出来る。
本発明の生体電極に用いられる導電膜を形成するための材料に配合される(B)樹脂は、上記の(A)イオン性材料(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、撥水性付与のためのシリコーンを含有し、粘着性を発現させるための成分である。(A)のイオン性材料にシリコーンを含有し粘着性を有している場合は、(B)樹脂は必ずしも必要ではないし、(B)樹脂にシリコーンを含んでいなくても良い。なお、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、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さらに好ましく、特には、シリコーン系、シリコーン含有のアクリル系、及びシリコーン含有の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。これらの中でも、シリコーン系粘着剤が、撥水性、皮膚呼吸性、貼り付けたときの肌の痒み等の不快感が少ない点で最も好ましい。
本発明の生体電極の導電膜の組成物には(C)成分として、カーボン粉、金属粉、珪素粉、及びチタン酸リチウム粉から選択される1つ以上をさらに含有することができる。(C)成分のうち、カーボン粉及び金属粉は電子導電性を高めるために添加され、珪素粉、及びチタン酸リチウム粉はイオン受容の感度を高めるために添加される。
本発明の生体電極の導電膜の組成物には、電子導電性を高めるために、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、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。特に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が好ましい。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。
本発明の生体電極の導電膜の組成物には、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、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。
本発明の生体電極の導電膜の組成物には、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、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。
本発明の生体電極の導電膜の組成物には、粘着性付与剤、架橋剤、架橋触媒、イオン性添加剤、有機溶剤などの任意成分を含むことができる。
また、本発明の生体電極の導電膜の組成物には、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。
本発明の生体電極の導電膜の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、樹脂100質量部に対して1~30質量部である。
本発明の生体電極の導電膜の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号公報中、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、樹脂100質量部に対して0.01~10質量部である。
本発明の生体電極の導電膜の組成物には、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、サッカリン、アセスルファムカリウム、特開2018-044147号公報、同2018-059050号公報、同2018-059052号公報、同2018-130534公報の塩を挙げることが出来る。
また、本発明の生体電極の導電膜の組成物には、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、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、n-トリデカン、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、ジイソペンチルエーテル、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。
本発明の生体電極の導電膜の組成物には、シリカ粒子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、親水性のイオンポリマーやポリグリセリンシリコーンとのなじみが良く、疎水性のシリコーン粘着剤でのイオンポリマーやポリグリセリンシリコーン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。フルオロスルホンアミド塩やフルオロスルホンイミド塩で修飾されたシリカ粒子を添加することも出来る。
以下、本発明の生体電極について、図面を参照しながら詳細に説明するが、本発明はこれらに限定されるものではない。
図4では本発明の生体電極の製造方法の一例が示されている。ここで、粘着層付き不織布シートに穴を開け、スナップで上下を挟む。補強フィルムを使う場合は、粘着層付き不織布シートと下部スナップの間に挟むと良い。シリコーン含有粘着性の導電膜は、リリースライナー上に印刷する。印刷方法は、スクリーン印刷、ステンシル印刷、フレキソ印刷、グラビア印刷、インクジェット印刷を挙げることが出来る。印刷した後に溶剤の乾燥と硬化のためにベークを行う。最後にリリースライナーが着いた状態で導電膜をスナップに圧着させて生体電極が出来上がる。
図5では、導電膜の片面をリリースライナーで覆った場合、図6では両面を覆った場合である。
本発明の生体電極は、多孔質膜を貫通する導電路上に形成された生体接触層となるシリコーン含有粘着性の導電膜を有するものである。この導電膜は、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。導電膜は、上述の本発明の生体電極の導電膜の組成物の硬化物であり、即ち、上述の(A)イオン性材料(塩)、(B)樹脂等の添加剤を含有するシリコーン含有の粘着性の樹脂層である。
また、本発明では、多孔質の伸縮性基材を貫通する導電路を作製するか、伸縮性基材の側面に露出するように前記伸縮性基材上に導電路を作製し、肌に貼り付ける側の導電路に接続されるように珪素を含有する粘着性の導電膜を形成する生体電極の製造方法を提供する。
また、本発明では、本発明の生体電極を肌に貼り付け、入浴もしくはシャワー後、又は入浴もしくはシャワー中に生体信号を測定する生体信号の測定方法を提供する。
イオン性ポリマー1を以下に示す。
(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。
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
DGDE:ジエチレングリコールジエチルエーテル
チタン酸リチウム粉:Sigma-Aldrich社製 サイズ200nm以下
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
銀フレーク:Sigma-Aldrich社製 平均サイズ10μm
付加反応制御剤:1-エチニルシクロヘキサノール
表1、2に記載の組成で、イオン性ポリマー、粘着性樹脂、有機溶剤、及び添加剤(チタン酸リチウム粉、白金触媒、導電性向上剤)、金属粉、付加反応制御剤をブレンドし、300メッシュのステンレスフィルターでろ過し、導電膜溶液(導電膜溶液1~13、比較導電膜溶液1)を調製した。
伸縮性基材として、多孔質膜1としてアクリル粘着剤が塗布された伸縮性が20%のポリエチレン不織布(400μm厚み)、多孔質膜2としてアクリル粘着剤が塗布された伸縮性が50%のポリウレタン不織布(400μm厚み)、多孔質膜3としてウレタン粘着剤が塗布された伸縮性が20%のポリエチレン不織布(380μm厚み)、多孔質膜4としてシリコーン粘着剤が塗布された伸縮性が20%のポリエチレン不織布(330μm厚み)、多孔質膜5としてアクリル粘着剤が塗布された伸縮性が20%のウレタンメンブレン膜(150μm厚み)を用いた。比較例用の非多孔質膜として、伸縮性が10%の膜厚50μmのTPUシートを用いた。
(1)図4に示されるリリースライナー上のシリコーン粘着導電膜パターンの作製
リリースライナー上に、上記導電膜溶液を用い、スクリーン印刷機を用いてステンシル穴開きマスクでシリコーン粘着導電膜パターンを印刷し、室温にて風乾10分後125℃で10分間オーブン中で硬化させ、膜厚50μmのシリコーン粘着導電膜パターンを形成した。
リリースライナー上に、オールグッド(株)製自動フィルムアプリケーター(スリットコーター)を用い、上記導電膜溶液を塗布し、室温にて風乾10分後125℃で10分間オーブン中で硬化させた。スリットコーターのスリット幅をそれぞれ350μm、550μm、740μmとし、それぞれ硬化後の膜厚が50μm、100μm、150μm厚みのシリコーン粘着導電膜を形成した。50μm厚品は、表3中の実施例16、19、20、21に適用、膜厚100μm品は実施例17、膜厚150μm品は実施例18の生体電極の作製に適用した。
1:ニッパ(株)製PETセパレーターSS1A(100μm厚み)
2:ニッパ(株)製PETセパレーターSS1A(50μm厚み)
3:ニッパ(株)製PETセパレーターFSD5(100μm厚み)
4:ニッパ(株)製PETセパレーターFSD5(38μm厚み)
5:テフロン繊維シート(280μm厚み)
PETセパレーターSS1Aの剥離力よりも、PETセパレーターFSD5の剥離力が低く、より剥離しやすい。又、PETセパレーターSS1A(100μm厚み)よりもPETセパレーターSS1A(50μm厚み)の方が剥離力が低い。PETセパレーターFSD5(38μm厚み)よりもテフロン繊維シートの方が剥離力が低い。
上記の生体電極の作製で作製した生体電極において、多孔質膜と導電膜を合わせた厚さをマイクロメーターを用いて測定した。基材がTPUシートの場合はTPUシートと導電膜を合わせた厚みを測定した。これらの厚みを生体接触層の厚さとした。結果を表3に示す。
生体電極のリリースライナーを剥がし、貼り付け直前に貼り付けの場所の肌を水で湿らせたガーゼで拭いて、心電計のプラス電極を図34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。
貼り付け直後と、毎日同時刻に、椅子に座った安静状態で、オムロンヘルスケア(株)製携帯心電計HCG-901とを生体電極のスナップと導電線の先に取り付けたクリップで挟んで接続し、心電図の測定を行った。測定していない時は、生体電極は体に貼り付けたままの状態とし、前記携帯心電計と電線のみを外した。1日1回、15分から30分の間、約40℃の風呂に入浴した。結果を表3に示す。図35に示されるPQRSTU波に代表されるECGシグナルが現れるかどうかを確認し、この波形が出てこなくなるまで計測を行った。
Claims (21)
- 生体電極であって、多孔質の伸縮性基材と、珪素を含有する粘着性の導電膜と、導電路とを有し、前記導電膜が前記多孔質の伸縮性基材の片面に形成されており、前記導電路が前記導電膜に接続し、かつ前記伸縮性基材を貫通し反対側に露出しているか、前記伸縮性基材の側面に露出しており、
前記珪素を含有する粘着性の導電膜が、フルオロスルホン酸、フルオロスルホンイミド、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、カリウム塩から選ばれるイオン性材料(A)を含有している ものであることを特徴とする生体電極。 - 前記多孔質の伸縮性基材が不織布又はメンブレン膜であることを特徴とする請求項1に記載の生体電極。
- 前記イオン性材料(A)が下記一般式(1)-1から(1)-4で示される部分構造を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。
- 前記イオン性材料(A)が、下記一般式(2)で表される繰り返し単位A1~A7から選ばれる1種以上を有するイオン性ポリマー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。
- 前記イオン性材料(A)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4のいずれか一項に記載の生体電極。
- 前記(A)成分に加えて、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種以上の(A)成分以外の粘着性の樹脂(B)成分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のいずれか一項に記載の生体電極。
- 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6に記載の生体電極。
- 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6又は請求項7に記載の生体電極。
- (C)成分として、カーボン粉、金属粉、珪素粉、及びチタン酸リチウム粉から選択される1つ以上をさらに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8のいずれか一項に記載の生体電極。
- 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9に記載の生体電極。
- 前記導電路が、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1から請求項10のいずれか一項に記載の生体電極。
- 前記導電路が、スナップ形状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。
- 前記伸縮性基材と前記導電膜を合わせた膜厚が、1mm以下であることを特徴とする請求項1から請求項12のいずれか一項に記載の生体電極。
- 前記伸縮性基材と前記導電膜を合わせた膜厚が、500μm以下であることを特徴とする請求項13に記載の生体電極。
- 前記伸縮性基材が粘着層を有してい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。
- 前記導電膜の上をリリースライナーで覆ったものであることを特徴とする請求項1から請求項15のいずれか一項に記載の生体電極。
- 前記リリースライナーが、フッ素樹脂、ポリエチレン、ポリプロピレン、環状ポリオレフィン、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンナフタレート、ポリブチレンナフタレート、ポリ塩化ビニル、ポリメチルメタクリレート、ポリ酢酸ビニル、ポリスチレン、ポリメチルペンテン、ポリイミド、ポリフェニレンスルファイド、ポリスルフォン、ポリエーテルサルフォン、ポリエーテルケトン、ポリアミドイミド、ポリエーテルイミド、ポリアセタール、ポリカーボネート、ポリフェニレンエーテル、ポリアクリロニトリル、セロファン、及び紙から選ばれ、前記フッ素樹脂以外はフッ素系の剥離剤又はシリコーン/フッ素系の剥離剤が塗布されているものであることを特徴とする請求項16に記載の生体電極。
- 多孔質の伸縮性基材を貫通する導電路を作製するか、伸縮性基材の側面に露出するように前記伸縮性基材上に導電路を作製し、肌に貼り付ける側の導電路に接続されるように珪素を含有する粘着性の導電膜を形成することを特徴とする請求項1から請求項17のいずれか一項に記載の生体電極の製造方法。
- 前記多孔質の伸縮性基材を貫通する導電路または前記伸縮性基材の側面に露出する前記伸縮性基材上の導電路の肌に貼り付ける側に前記珪素を含有する粘着性の導電膜を、リリースライナー上に形成した前記珪素を含有する粘着性の導電膜を転写することにより形成するか、導電路上に直接印刷することによって形成することを特徴とする請求項18に記載の生体電極の製造方法。
- リリースライナー上に珪素を含有する粘着性の導電膜材料を塗布し、硬化することを特徴とする請求項18又は請求項19に記載の生体電極の製造方法。
- 請求項1から請求項17のいずれか一項に記載の生体電極を肌に貼り付け、入浴もしくはシャワー後、又は入浴もしくはシャワー中に生体信号を測定することを特徴とする生体信号の測定方法。
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