JP2021151436A - 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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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 9
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- 239000006229 carbon black Substances 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
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- RQIMPDXRFCFBGC-UHFFFAOYSA-N n-(oxomethylidene)sulfamoyl fluoride Chemical compound FS(=O)(=O)N=C=O RQIMPDXRFCFBGC-UHFFFAOYSA-N 0.000 claims description 7
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- CFJYNSNXFXLKNS-UHFFFAOYSA-N p-menthane Chemical compound CC(C)C1CCC(C)CC1 CFJYNSNXFXLKNS-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- BEZDDPMMPIDMGJ-UHFFFAOYSA-N pentamethylbenzene Chemical compound CC1=CC(C)=C(C)C(C)=C1C BEZDDPMMPIDMGJ-UHFFFAOYSA-N 0.000 description 1
- WQIQNKQYEUMPBM-UHFFFAOYSA-N pentamethylcyclopentadiene Chemical compound CC1C(C)=C(C)C(C)=C1C WQIQNKQYEUMPBM-UHFFFAOYSA-N 0.000 description 1
- HPQURZRDYMUHJI-UHFFFAOYSA-N pentylcyclopentane Chemical compound CCCCCC1CCCC1 HPQURZRDYMUHJI-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- NGATWIKLQRJVRN-UHFFFAOYSA-N phthalic acid;sodium Chemical compound [Na].[Na].OC(=O)C1=CC=CC=C1C(O)=O NGATWIKLQRJVRN-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 239000004224 potassium gluconate Substances 0.000 description 1
- 235000013926 potassium gluconate Nutrition 0.000 description 1
- 229960003189 potassium gluconate Drugs 0.000 description 1
- BWILYWWHXDGKQA-UHFFFAOYSA-M potassium propanoate Chemical compound [K+].CCC([O-])=O BWILYWWHXDGKQA-UHFFFAOYSA-M 0.000 description 1
- 239000004331 potassium propionate Substances 0.000 description 1
- 235000010332 potassium propionate Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- FIJPWGLOBMXXSF-UHFFFAOYSA-M potassium;2-hydroxyacetate Chemical compound [K+].OCC([O-])=O FIJPWGLOBMXXSF-UHFFFAOYSA-M 0.000 description 1
- LBOHISOWGKIIKX-UHFFFAOYSA-M potassium;2-methylpropanoate Chemical compound [K+].CC(C)C([O-])=O LBOHISOWGKIIKX-UHFFFAOYSA-M 0.000 description 1
- XWIJIXWOZCRYEL-UHFFFAOYSA-M potassium;methanesulfonate Chemical compound [K+].CS([O-])(=O)=O XWIJIXWOZCRYEL-UHFFFAOYSA-M 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- ZJMWRROPUADPEA-UHFFFAOYSA-N sec-butylbenzene Chemical compound CCC(C)C1=CC=CC=C1 ZJMWRROPUADPEA-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 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
- 235000017281 sodium acetate Nutrition 0.000 description 1
- KYKFCSHPTAVNJD-UHFFFAOYSA-L sodium adipate Chemical compound [Na+].[Na+].[O-]C(=O)CCCCC([O-])=O KYKFCSHPTAVNJD-UHFFFAOYSA-L 0.000 description 1
- 235000011049 sodium adipate Nutrition 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- MFBOGIVSZKQAPD-UHFFFAOYSA-M sodium butyrate Chemical compound [Na+].CCCC([O-])=O MFBOGIVSZKQAPD-UHFFFAOYSA-M 0.000 description 1
- 229960005480 sodium caprylate Drugs 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 229940023144 sodium glycolate Drugs 0.000 description 1
- UDWXLZLRRVQONG-UHFFFAOYSA-M sodium hexanoate Chemical compound [Na+].CCCCCC([O-])=O UDWXLZLRRVQONG-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 229940045845 sodium myristate Drugs 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- BYKRNSHANADUFY-UHFFFAOYSA-M sodium octanoate Chemical compound [Na+].CCCCCCCC([O-])=O BYKRNSHANADUFY-UHFFFAOYSA-M 0.000 description 1
- 229940045870 sodium palmitate Drugs 0.000 description 1
- JXKPEJDQGNYQSM-UHFFFAOYSA-M sodium propionate Chemical compound [Na+].CCC([O-])=O JXKPEJDQGNYQSM-UHFFFAOYSA-M 0.000 description 1
- 239000004324 sodium propionate Substances 0.000 description 1
- 235000010334 sodium propionate Nutrition 0.000 description 1
- 229960003212 sodium propionate Drugs 0.000 description 1
- SJRDNQOIQZOVQD-UHFFFAOYSA-M sodium;2,2-dimethylpropanoate Chemical compound [Na+].CC(C)(C)C([O-])=O SJRDNQOIQZOVQD-UHFFFAOYSA-M 0.000 description 1
- SUAMAHKUSIHRMR-UHFFFAOYSA-M sodium;2-oxobutanoate Chemical compound [Na+].CCC(=O)C([O-])=O SUAMAHKUSIHRMR-UHFFFAOYSA-M 0.000 description 1
- AIMUHNZKNFEZSN-UHFFFAOYSA-M sodium;decane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCS([O-])(=O)=O AIMUHNZKNFEZSN-UHFFFAOYSA-M 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- NMTDPTPUELYEPL-UHFFFAOYSA-M sodium;heptanoate Chemical compound [Na+].CCCCCCC([O-])=O NMTDPTPUELYEPL-UHFFFAOYSA-M 0.000 description 1
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 description 1
- KKVTYAVXTDIPAP-UHFFFAOYSA-M sodium;methanesulfonate Chemical compound [Na+].CS([O-])(=O)=O KKVTYAVXTDIPAP-UHFFFAOYSA-M 0.000 description 1
- RUYRDULZOKULPK-UHFFFAOYSA-M sodium;nonane-1-sulfonate Chemical compound [Na+].CCCCCCCCCS([O-])(=O)=O RUYRDULZOKULPK-UHFFFAOYSA-M 0.000 description 1
- LTOCMXUTASYUOC-UHFFFAOYSA-M sodium;nonanoate Chemical compound [Na+].CCCCCCCCC([O-])=O LTOCMXUTASYUOC-UHFFFAOYSA-M 0.000 description 1
- DLJKLUIGOGBWRW-UHFFFAOYSA-M sodium;pentadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCC([O-])=O DLJKLUIGOGBWRW-UHFFFAOYSA-M 0.000 description 1
- LHYPLJGBYPAQAK-UHFFFAOYSA-M sodium;pentanoate Chemical compound [Na+].CCCCC([O-])=O LHYPLJGBYPAQAK-UHFFFAOYSA-M 0.000 description 1
- JUQGWKYSEXPRGL-UHFFFAOYSA-M sodium;tetradecanoate Chemical compound [Na+].CCCCCCCCCCCCCC([O-])=O JUQGWKYSEXPRGL-UHFFFAOYSA-M 0.000 description 1
- JZVZOOVZQIIUGY-UHFFFAOYSA-M sodium;tridecanoate Chemical compound [Na+].CCCCCCCCCCCCC([O-])=O JZVZOOVZQIIUGY-UHFFFAOYSA-M 0.000 description 1
- DBMQUCVJHLWQHT-UHFFFAOYSA-M sodium;undecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCS([O-])(=O)=O DBMQUCVJHLWQHT-UHFFFAOYSA-M 0.000 description 1
- ZOOPHYLANWVUDY-UHFFFAOYSA-M sodium;undecanoate Chemical compound [Na+].CCCCCCCCCCC([O-])=O ZOOPHYLANWVUDY-UHFFFAOYSA-M 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- WMOVHXAZOJBABW-UHFFFAOYSA-N tert-butyl acetate Chemical compound CC(=O)OC(C)(C)C WMOVHXAZOJBABW-UHFFFAOYSA-N 0.000 description 1
- JAELLLITIZHOGQ-UHFFFAOYSA-N tert-butyl propanoate Chemical compound CCC(=O)OC(C)(C)C JAELLLITIZHOGQ-UHFFFAOYSA-N 0.000 description 1
- XTVMZZBLCLWBPM-UHFFFAOYSA-N tert-butylcyclohexane Chemical compound CC(C)(C)C1CCCCC1 XTVMZZBLCLWBPM-UHFFFAOYSA-N 0.000 description 1
- LPSXSORODABQKT-UHFFFAOYSA-N tetrahydrodicyclopentadiene Chemical compound C1C2CCC1C1C2CCC1 LPSXSORODABQKT-UHFFFAOYSA-N 0.000 description 1
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- JNRUXZIXAXHXTN-UHFFFAOYSA-N trimethyl(2-methylbut-3-yn-2-yloxy)silane Chemical compound C#CC(C)(C)O[Si](C)(C)C JNRUXZIXAXHXTN-UHFFFAOYSA-N 0.000 description 1
- 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
- JABYJIQOLGWMQW-UHFFFAOYSA-N undec-4-ene Chemical compound CCCCCCC=CCCC JABYJIQOLGWMQW-UHFFFAOYSA-N 0.000 description 1
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Abstract
Description
本発明の生体電極は、導電性基材と生体接触層を含み、前記生体接触層は水を含まない樹脂層を含み、該樹脂層の生体に接触する表面側に、ナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩、ベタインから選ばれる水溶性塩と水とが浸透した浸透層を有するものであることを特徴とする。
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、導電性基材と生体接触層を含み、前記生体接触層は水を含まない樹脂層を含み、該樹脂層の生体に接触する表面側に、ナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩、ベタインから選ばれる水溶性塩と水とが浸透した浸透層を有するものである。この生体接触層は、導電性基材上に形成されており、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って、導電性及び粘着性を有する。生体接触層は、前記水を含まない樹脂層を含み、該樹脂層の生体に接触する表面側に、前記浸透層を有するものであれば特に限定されないが、例えば、後述の生体電極組成物の硬化物からなる樹脂層であり、即ち、後述の高分子化合物(A)のイオン性材料(塩)、(B)樹脂等の添加剤を含有する組成物を硬化させた粘着性の樹脂層上に、特定のイオンを含有する水溶液を浸透させて浸透層を形成したものとすることができる。
本発明の生体電極の生体接触層は水を含まない樹脂層を含む。以下水を含まない樹脂層について説明する。
本発明の生体電極の水を含まない樹脂層を作製するための生体電極組成物は、特に限定されないが、例えば、高分子化合物(A)のイオン性材料として、イオンの繰り返し単位を有するポリマーを含有するものであることができる。以下、一例として、このような生体電極組成物の各成分について、更に詳細に説明する。
生体電極組成物に高分子化合物(A)((A)成分)のイオン性材料(導電性材料)として配合される塩は、高分子化合物(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、ナトリウム塩、カリウム塩、銀塩から選ばれる塩構造の繰り返し単位を有するポリマーであることができる。
生体電極組成物の高分子化合物(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。
生体電極組成物の高分子化合物(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、リ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。
生体電極組成物の高分子化合物(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ために繰り返し単位Dを共重合することも出来る。繰り返し単位Dを得るためのモノマーは、具体的には下記に例示することができる。
生体電極組成物の高分子化合物(A)成分には、上記の繰り返し単位A1〜A7、B〜Dに加えて、更には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。オキシラン環又はオキセタン環を有する繰り返し単位E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できる。
生体電極組成物の高分子化合物(A)成分には、上記の繰り返し単位A1〜A7、B〜Eに加えて、珪素を有する繰り返し単位Fを共重合することも出来る。珪素を有する繰り返し単位F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できる。
生体電極組成物の高分子化合物(A)成分には、上記の繰り返し単位A1〜A7、B〜Fに加えて、フッ素を有する繰り返し単位Gを共重合することも出来る。フッ素を有する繰り返し単位G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できる。
上記生体電極組成物に配合される(B)樹脂((B)成分)は、上記の高分子化合物(A)のイオン性材料(塩)と相溶して塩の溶出を防ぎ、金属粉、カーボン材料、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。高分子化合物(A)のイオン性材料が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。なお、樹脂は、上述の高分子化合物(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。
生体電極組成物には、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。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。
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、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。
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、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、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。
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、樹脂100質量部に対して1〜30質量部である。
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、樹脂100質量部に対して0.01〜10質量部である。
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、特開2018−44147号公報、同2018−59050号公報、同2018−59052号公報、同2018−130534公報の塩を挙げることが出来る。
また、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が挙げられる。
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。
生体電極組成物には、シリカ粒子、アルミナ粒子、チタニア粒子、ジルコニア粒子を混合することも出来る。シリカ粒子、アルミナ粒子、チタニア粒子、ジルコニア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、アルミナ粒子、チタニア粒子、ジルコニア粒子は乾式、湿式どちらでも好ましく用いることが出来る。シリカ粒子、アルミナ粒子、チタニア粒子、ジルコニア粒子の形状は、球状、楕円状、不定形状、中空状、多孔質のいずれであっても構わない。
本発明の生体電極の製造方法は、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、生体接触層が水を含まない樹脂層を含み、該樹脂層の生体に接触する表面側に、水溶性塩と水とが浸透した浸透層を有するように構成できれば特に限定されないが、例えば、前記導電性基材上に、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した後、浸透層を形成する方法とすることができる。浸透層は、水を含まない樹脂層の生体に接触する表面側に、水溶性塩と水とを含む液(浸透液)が浸透することで形成できる。浸透液は後述のものを使用できる。
本発明の生体電極の生体接触層に含まれる浸透層は、前記水を含まない樹脂層の生体に接触する表面側に、ナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩、ベタインから選ばれる水溶性塩と水とを含む液(浸透液)を浸透させる処理を行うことで形成される。
前記浸透液に含まれる前記水溶性塩は特に限定されないが、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、ベタインから選ばれる塩であることができる。なお、上述の高分子化合物(A)は、前記水溶性塩に含まれない。
前記浸透液は、さらに炭素数1〜4の1価アルコール又は多価アルコールを含有することができ、前記アルコールがエタノール、イソプロピルアルコール、エチレングリコール、ジエチレングリコール、トリエチレングリコール、グリセリン、ペンタエリスリトール、ソルビタン、ソルビトール、ポリエチレングリコール、ポリプロピレングリコール、ジグリセリン、ポリグリセリン、ポリグリセリン構造を有するシリコーン化合物、単糖類、多糖類又はこれらのヒドロキシ基が置換されている材料から選ばれるものであることが好ましく、前記ポリグリセリン構造を有するシリコーン化合物が上記一般式(3)で示されるものであることがより好ましい。
本発明の生体信号の測定方法は、肌の上を水を含有する溶液で処理し、処理した部分に本発明の生体電極を貼り付けて生体信号を測定する方法である。生体電極が貼り付けられる側の肌を、貼り付ける直前に水や水を含有するエタノールやグリセリン、ジグリセリン、ポリグリセリンなどのアルコールを含有する布で拭いたり、スプレー塗布したりすることは、肌の表面を湿らせてより短時間で高感度かつ高精度な生体信号を取る上で有効である。前記水含有布で拭くことは、肌を湿らすだけでなく、肌表面の油脂を取り除く効果もあり、これによっても生体信号の感度が向上する。
(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
BE:ジエチレングリコールブチルエーテル
アイソパーG(エクソンモービル社製):イソパラフィン
チタン酸リチウム粉、スピネル:Sigma−Aldrich社製 サイズ200nm以下
銀フレーク:Sigma−Aldrich社製 平均サイズ10μm
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2に記載の組成で、イオン性材料(塩)、樹脂、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)、架橋剤をブレンドし、生体電極溶液(生体電極溶液1〜17、比較生体電極溶液1、2)を調製した。
ビーマス(Bemis)社の熱可塑性ウレタン(TPU)フィルムの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を印刷した。その上の円形部分に重ねて、表1、2記載の生体電極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、硬化させて生体電極を作製した(生体電極1〜9、比較生体電極1、2)。更には生体電極10〜17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。図4はウレタンフィルム7上に導電パターン8が印刷され、硬化して作製された生体電極9を示す図である。図5は導電パターン8が印刷されて硬化したウレタンフィルム7を切り取って、両面テープ10を貼り付けた生体電極9を示す図である。
上記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。
前記の様に作製した生体電極1〜17の上に、前処理水溶液1〜25を、噴霧法では噴霧ノズルから発せられた水滴を20秒間当て、その後20分間乾燥させ、テフロンフィルムを貼った。ディスペンス法では、生体電極上に前処理溶液を約100μL垂らし、テフロンフィルムを貼った。
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6中の人体のLAの場所、マイナス電極をLLの場所に、アースをRAの場所にそれぞれ貼り付けた。実施例30では、貼り付ける直前に、水を含有する脱脂綿で肌の表面を拭いた。テフロンフィルムを剥がし、速やかに胸の上に貼り付け、その直後に心電図の測定を開始し、図7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…カーボン材料、 5−1…浸透層、 5−2…水を含まない樹脂層、
6…生体、 7…ウレタンフィルム、 8…導電パターン、 9…生体電極、
10…両面テープ。
Claims (20)
- 生体電極であって、前記生体電極は導電性基材と生体接触層を含み、前記生体接触層は水を含まない樹脂層を含み、該樹脂層の生体に接触する表面側に、ナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩、ベタインから選ばれる水溶性塩と水とが浸透した浸透層を有するものであることを特徴とする生体電極。
- 前記水溶性塩が、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、ベタインから選ばれる塩であることを特徴とする請求項1に記載の生体電極。
- 前記樹脂層が、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、ナトリウム塩、カリウム塩、銀塩から選ばれる塩構造を有する繰り返し単位を含有する高分子化合物(A)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。
- 前記一般式(1)−1、(1)−2で示されるフルオロスルホン酸、(1)−3で示されるスルホンイミド、又は(1)−4で示されるスルホンアミドのアンモニウム塩、ナトリウム塩、カリウム塩、銀塩から選ばれる1種以上の繰り返し単位が、下記一般式(1’)で示される繰り返し単位A1〜A7から選ばれる1種以上を有する繰り返し単位であることを特徴とする請求項4に記載の生体電極。
- 前記一般式(1)−1〜(1)−4で示される塩構造が、M+として、下記一般式(2)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4又は請求項5に記載の生体電極。
- 前記浸透層が、さらに炭素数1〜4の1価アルコール又は多価アルコールを含有することを特徴とする請求項1から請求項6のいずれか1項に記載の生体電極。
- 前記多価アルコールがグリセリン、ペンタエリスリトール、ソルビタン、ソルビトール、ポリエチレングリコール、ポリプロピレングリコール、ジグリセリン、ポリグリセリン、ポリグリセリン構造を有するシリコーン化合物、単糖類、多糖類又はこれらのヒドロキシ基が置換されている材料から選ばれるものであることを特徴とする請求項7に記載の生体電極。
- 前記ポリグリセリン構造を有するシリコーン化合物が下記一般式(3)、(4)で示されるものであることを特徴とする請求項8に記載の生体電極。
- 前記樹脂層が、更に(B)成分として、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9のいずれか1項に記載の生体電極。
- 前記(B)成分のシリコーン系樹脂が、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、アルケニル基を有するジオルガノシロキサン、並びにSiH基を有するオルガノハイドロジェンポリシロキサン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。
- 前記樹脂層が、カーボン材料、銀粉、珪素粉、チタン酸リチウム粉を含有することを特徴とする請求項1から請求項11のいずれか1項に記載の生体電極。
- 前記カーボン材料が、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12に記載の生体電極。
- 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、及び炭素から選ばれる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13のいずれか1項に記載の生体電極。
- 前記浸透層上に、さらに保護フィルムを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1項に記載の生体電極。
- 生体電極の製造方法であって、導電性基材の上に、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、ナトリウム塩、カリウム塩、銀塩から選ばれる塩構造を有する繰り返し単位を含有する高分子化合物(A)を含有する生体電極組成物を塗布し、硬化させて生体接触層を形成し、前記生体接触層の生体に接触する表面側に、ナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩、ベタインから選ばれる水溶性塩を含む水溶液を接触させて、前記生体接触層の生体に接触する表面側に、前記水溶性塩を含む水溶液が浸透した浸透層を形成することを特徴とする生体電極の製造方法。
- 前記生体接触層の生体に接触する表面側に、前記水溶性塩と、炭素数1〜4の1価アルコール又は多価アルコールと、水とを含有する溶液を噴霧法により接触させることを特徴とする請求項16に記載の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、及び炭素から選ばれる1種以上を含むものを用いることを特徴とする請求項16又は請求項17に記載の生体電極の製造方法。
- 前記浸透層の上に、さらに保護フィルムを積層することを特徴とする請求項16から請求項18のいずれか1項に記載の生体電極の製造方法。
- 肌の上を水を含有する溶液で処理し、処理した部分に請求項1から請求項15のいずれか1項に記載の生体電極を貼り付けて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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