CN114533073A - 生物体电极组成物、生物体电极、生物体电极的制造方法、以及反应复合体 - Google Patents
生物体电极组成物、生物体电极、生物体电极的制造方法、以及反应复合体 Download PDFInfo
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- CN114533073A CN114533073A CN202111412135.5A CN202111412135A CN114533073A CN 114533073 A CN114533073 A CN 114533073A CN 202111412135 A CN202111412135 A CN 202111412135A CN 114533073 A CN114533073 A CN 114533073A
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Images
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Abstract
本发明涉及生物体电极组成物、生物体电极、生物体电极的制造方法、以及反应复合体。本发明提供能形成导电性及生物体适合性优异、轻量且能够以低成本制造,即使被水沾湿即使干燥,导电性仍不大幅下降的生物体电极用的生物体接触层的生物体电极组成物、以该生物体电极组成物形成了生物体接触层的生物体电极、及其制造方法。一种生物体电极组成物,含有(A)具有离子性官能团的单体与碳粒子的反应复合体,前述(A)成分含有:和具有选自氟磺酸、氟磺酰亚胺、及N‑羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体键结的碳粒子。
Description
技术领域
本发明关于与生物体的皮肤接触并利用来自皮肤的电信号而能检测到心搏数等身体状态的生物体电极、及其制造方法、以及适用于生物体电极的生物体电极组成物。
现有技术
近年,随着IoT(物联网(Internet of Things))的普及,穿戴式器件的开发也在进展。能连接到因特网的钟表、眼镜为其代表例。又,在医疗领域、运动领域方面也需要能随时监测身体状态的穿戴式器件,为今后具成长性的领域。
在医疗领域方面,例如有人研究如利用电信号来感测心脏搏动的心电图测定般通过感测微弱电流来监测身体脏器的状态的穿戴式器件。心电图的测定将涂有导电糊剂的电极装设于身体并进行测定,但此为仅1次的短时间的测定。反观如上述的医疗用的穿戴式器件的开发,以连续数周随时监测健康状态的器件的开发为目标。是以,对于使用于医疗用穿戴式器件的生物体电极,会要求长时间使用时也不会有导电性的变化、不会皮肤过敏。此外,也要求轻量、能以低成本制造。
医疗用穿戴式器件有贴附于身体的类型、与纳入于衣服的类型,作为贴附于身体的类型,有人提案使用为上述导电糊剂的材料的含有水与电解质的水溶性凝胶的生物体电极(专利文献1)。关于水溶性凝胶,在用以保持水的水溶性聚合物中含有钠、钾、钙作为电解质,会将来自皮肤的离子浓度的变化转换成电。另一方面,作为纳入于衣服的类型,有人提案将纤维中纳入有如PEDOT-PSS(Poly-3,4-ethylenedioxythiophene-Polystyrenesulfonate;聚-3,4-乙烯二氧噻吩-聚苯乙烯磺酸盐)的导电性聚合物、银糊剂的布使用于电极的方法(专利文献2)。
但使用上述含有水与电解质的水溶性凝胶时,有因干燥导致水消失时导电性也会消失的问题。另一方面,使用铜等游离倾向高的金属时,有对于有些人而言存在引起皮肤过敏的风险的问题,使用如PEDOT-PSS的导电性聚合物时,也有因导电性聚合物的酸性强而存在引起皮肤过敏的风险的问题、洗涤时导电聚合物从纤维剥落的问题。
又,金属纳米线、炭黑、及纳米碳管等具有优异的导电性,故也有人探讨将它们作为电极材料使用(专利文献3、4、5)。金属纳米线由于线彼此的接触机率变高,故少量的添加量即可通电。但,金属纳米线为前端尖的纤细材料,故会成为皮肤过敏发生的原因。如上所述,即便该物本身不会引起过敏反应,有时仍会因材料的形状、刺激性导致生物相容性恶化,同时兼有导电性与生物相容性是困难的。
据认为金属膜的导电性非常高,故会作为优异的生物体电极而发挥功能,但未必如此。因心脏的搏动而从皮肤释出的并不只是微弱电流,也会放出钠离子、钾离子、钙离子。因此须将离子的浓度变化转换成电流,但不易游离的贵金属而言将来自皮肤的离子转换成电流的效率不佳。故使用了贵金属的生物体电极的阻抗高,与皮肤的通电是高电阻的。
另一方面,也有人研究添加了离子性液体的电池(专利文献6)。离子性液体的热稳定性、化学稳定性高而有导电性优异的特征,在电池用途的应用正在加广。但是专利文献6所示般分子量小的离子性液体会溶于水,故若使用了添加其的生物体电极,离子性液体会被来自皮肤的汗液萃取,不只导电性降低,还会渗透到皮肤而成为皮肤粗糙的原因。
又,有人探讨使用了聚合物型磺酰亚胺的锂盐的电池(非专利文献1)。但是锂的离子移动性高,故可应用在电池,但并非是具有生物体适合性的材料。而且,也有人探讨悬吊于聚硅氧的氟磺酸的锂盐(非专利文献2)。
生物体电极若离开皮肤,便无法获得来自身体的资讯。且即使仅是接触面积变化,通电的电量也会出现变动,心电图(电信号)的基线会变动。因此为了从身体获得稳定的电信号,生物体电极需要一直接触皮肤,且其接触面积不变化。因此生物体电极需有粘着性。又,也需要能追随皮肤伸缩、弯曲变化的伸缩性、可挠性。
有人探讨接触皮肤的部分为氯化银并叠层了银作为与器件导通的部分而得的生物体电极。固体的氯化银对皮肤无粘着力也无伸缩性,故特别是人体在动作时,生物体信号的收集能力会降低。所以,以在氯化银与银的叠层膜、与皮肤之间叠层了水溶性凝胶而成的生物体电极的形式使用。于此情形,会因前述凝胶干燥导致出现劣化。
据报告若将炭黑与环氧树脂混合,会比起仅有环氧树脂时在更低温进行硬化反应。其原因在于通过在炭黑表面存在的羧基与环氧基的反应,能在更低温进行交联反应(非专利文献3)。
有人报告使用氧化石墨烯作为导电辅助剂的锂离子电池(专利文献7)。于此情形,氧化石墨烯作为使钴酸锂等正极材的分散性及导电性更好的粘结剂使用。离子电池和生物体电极在需要高离子导电性方面是共通的。
现有技术文献
专利文献
[专利文献1]国际公开第WO2013-039151号小册
[专利文献2]日本特开2015-100673号公报
[专利文献3]日本特开平5-095924号公报
[专利文献4]日本特开2003-225217号公报
[专利文献5]日本特开2015-019806号公报
[专利文献6]日本特表2004-527902号公报
[专利文献7]日本特开2020-140973号公报
非专利文献
[非专利文献1]J.Mater.Chem.A,2016,4,p10038-10069
[非专利文献2]J.of the Electrochemical Society,150(8)A1090-A1094(2003)
[非专利文献3]高分子论文集Vol.41,No.10,p597-603(1984)
发明内容
[发明欲解决的课题]
本发明是为了解决上述问题,目的在于提供能形成导电性及生物体适合性优异、轻量且能以低成本制造,即使被水沾湿即使干燥,导电性仍不大幅降低的生物体电极用的生物体接触层的生物体电极组成物、以该生物体电极组成物形成了生物体接触层的生物体电极、及其制造方法。
[解决课题的方式]
为了解决上述课题,本发明提供一种生物体电极组成物,
含有(A)具有离子性官能团的单体与碳粒子的反应复合体,
前述(A)成分含有:和具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体键结的碳粒子。
若为如此的生物体电极组成物,会成为能形成导电性及生物体适合性优异、轻量、且能以低成本制造、即使被水沾湿即使干燥,导电性仍不大幅降低的生物体电极用的生物体接触层的生物体电极组成物。
又,前述碳粒子宜选自炭黑、纳米碳管、石墨(graphite)、石墨烯较佳。
若为如此的碳粒子,可理想地使用于本发明。
又,前述具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体,宜具有下列通式(1)-1至(1)-4中的任一者表示的结构较佳。
[化1]
式中,Rf1及Rf2为氢原子、氟原子、氧原子、甲基、或三氟甲基,Rf1及Rf2为氧原子时,Rf1及Rf2是键结于1个碳原子而形成羰基的1个氧原子,Rf3及Rf4为氢原子、氟原子、或三氟甲基,Rf1~Rf4中的一者以上为氟原子或三氟甲基。Rf5、Rf6、Rf7为氟原子、碳数1~4的直链状、分支状的烷基,且有至少1个以上的氟原子。m为1~4的整数。M+是选自铵离子、锂离子、钠离子、钾离子、银离子的离子。
此时前述具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体,宜为下列通式(2)-1至(2)-4表示者中的任意者较佳。
[化2]
式中,R1为碳数1~8的亚烷基,也可和R3键结并形成环,也可以具有醚基。R2为氢原子、碳数1~4的烷基,R3为单键或碳数1~20的直链状、分支状、环状的亚烷基,也可以具有芳香族基、醚键、酯键、羟基、氮原子。R4为单键或亚甲基。R5为单键、或也可以具有醚基、酯基的碳数1~10的(n+1)价烃基。n为1或2。Rf1~Rf7、M+、及m同前所述。
又,前述(A)成分,宜是相对于前述碳粒子100质量份使前述具有离子性官能团的单体5质量份以上反应而得者较佳。
又,前述(A)成分宜含有下列通式(3)表示的铵离子作为构成前述铵盐的铵离子较佳。
[化3]
式中,R101d、R101e、R101f、R101g各为氢原子、碳数1~13的直链状、分支状、或环状的烷基、碳数2~12的直链状、分支状、或环状的烯基或炔基、或碳数4~20的芳香族基,也可以具有选自醚基、羰基、酯基、羟基、氨基、硝基、磺酰基、亚磺酰基、卤素原子、及硫原子中的1种以上。R101d与R101e、R101d与R101e与R101f也可以和它们所键结的氮原子一起形成环,当形成环时,R101d与R101e及R101d与R101e与R101f形成碳数3~10的亚烷基、或形成环中具有式中的氮原子的杂芳香族环。
若为如此的生物体电极组成物,具有离子性官能团的单体悬吊于碳粒子,借此,离子导电性与电子导电性皆提升,不仅生物体电极的感度更好,尚能防止具有离子性官能团的单体萃取到生物体电极膜外,可防止由于萃取导致生物体信号的感度下降,对于皮肤的渗透性降低,对于皮肤的刺激性下降,故更能防止通过皮肤而引起过敏。
又,宜更含有作为(B)成分的粘着性树脂较佳。
此时前述(B)成分宜为选自聚硅氧树脂、(甲基)丙烯酸酯树脂、氨基甲酸酯树脂中的1种以上较佳。
若为如此,可一直密合于皮肤,并长时间获得稳定的电信号。
又,针对前述(B)成分,宜含有具有烯基的二有机硅氧烷与具有SiH基的有机氢聚硅氧烷较佳。
此时针对前述(B)成分,宜更含有具有RxSiO(4-x)/2单元(R为碳数1~10的经取代或未经取代的一价烃基,x为2.5~3.5的范围。)及SiO2单元的聚硅氧树脂较佳。
若为如此,适合作为生物体电极组成物使用。
又,宜更含有具有离子性重复单元的高分子化合物作为(C)成分较佳。
此时前述(C)成分的前述离子性重复单元,宜含有具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、及银盐的结构的重复单元较佳。
若为含有具有如此的重复单元的高分子化合物的生物体电极组成物,则本发明的效果会更好。
又,针对(D)成分宜含有碳粉及/或金属粉较佳。
此时前述碳粉为炭黑及纳米碳管中的任一者或两者较佳。
又,前述金属粉宜为选自金、银、铂、铜、锡、钛、镍、铝、钨、钼、钌、铬、铟的金属粉较佳。
此时前述金属粉为银粉较佳。
若为如此,则导电性会更良好。
又,宜更含有有机溶剂作为(E)成分较佳。
若为如此,生物体电极组成物的涂布性会更良好。
又,本发明提供一种生物体电极,具有导电性基材及形成在该导电性基材上的生物体接触层,前述生物体接触层是上述生物体电极组成物的硬化物。
若为本发明的生物体电极,会成为导电性及生物体适合性优异、轻量且能够以低成本制造,即使被水沾湿即使干燥,导电性仍不大幅下降的生物体电极。
又,前述导电性基材宜含有选自金、银、氯化银、铂、铝、镁、锡、钨、铁、铜、镍、不锈钢、铬、钛、碳、及导电性聚合物中的1种以上较佳。
本发明的生物体电极特别适合使用如此的导电性基材。
又,本发明提供一种生物体电极的制造方法,是具有导电性基材及形成在该导电性基材上的生物体接触层的生物体电极的制造方法,通过在前述导电性基材上涂布上述生物体电极组成物并使其硬化,以形成前述生物体接触层。
若为本发明的生物体电极的制造方法,则能轻易地制造导电性及生物体适合性优异、轻量且能够以低成本制造,即使被水沾湿即使干燥,导电性仍不大幅下降的生物体电极。
又,针对前述导电性基材,使用含有选自金、银、氯化银、铂、铝、镁、锡、钨、铁、铜、镍、不锈钢、铬、钛、碳、及导电性聚合物中的1种以上者较佳。
本发明的生物体电极的制造方法特别适合使用如此的导电性基材。
又,本发明提供一种反应复合体,是具有离子性官能团的单体与碳粒子的反应复合体,前述反应复合体是和单体键结的碳粒子,该单体具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构。
又,前述碳粒子宜选自炭黑、纳米碳管、石墨(graphite)、石墨烯较佳。
碳粒子通过以具有离子性官能团的单体修饰,作为能形成能将从皮肤放出的离子、电信号以高感度、良好效率地传递到器件(也即导电性优异)、即使长期间装设于皮肤亦无引起过敏之虞(也即生物体适合性优异)、即使被水沾湿即使干燥,导电性仍不大幅下降的生物体电极用的生物体接触层的生物体电极组成物的成分特别有用。
[发明的效果]
如上,若为本发明的含有:和具有离子性官能团的单体键结的碳粒子(具有离子性官能团的单体与碳粒子的反应复合体)的生物体电极组成物,则会成为能形成可将来自皮肤的电信号以良好效率传递到器件(也即导电性优异)、即使长期间装设于皮肤也无引起过敏之虞(也即生物体适合性优异)、轻量、能以低成本制造、即使被水沾湿即使干燥,导电性仍不大幅下降的生物体电极用的生物体接触层的生物体电极组成物。又,通过添加离子性的高分子化合物、导电性粉末(碳粉、金属粉),导电性会更好,通过和有粘着性及伸缩性的树脂组合,能够制造特别高粘着力且伸缩性高的生物体电极。又,可通过添加剂等使得对于皮肤的伸缩性、粘着性更好,也可通过适当调整树脂的组成、生物体接触层的厚度来调整伸缩性、粘着性。
又,若为本发明的生物体电极,可通过上述和具离子性官能团的单体键结的碳粒子而兼顾导电性及生物体适合性,也有粘着性,故和皮肤的接触面积一定,能够稳定地以高感度获得来自皮肤的电信号。
又,若为本发明的生物体电极的制造方法,则能以低成本轻易地制造导电性及生物体适合性优异、轻量、即使被水沾湿即使干燥,导电性仍不大幅下降的本发明的生物体电极。
附图说明
图1显示本发明的生物体电极的一例的概略剖面图。
图2显示本发明的生物体电极装设于生物体时的一例的概略剖面图。
图3显示以本发明的实施例制作的生物体电极印刷后的概略图。
图4显示切取本发明的实施例制作的生物体电极的一者并安装了粘着层及电线的概略图。
图5显示本发明的实施例中实施生物体信号的测定时,电极及接地对人体贴附部位的图。
图6显示使用本发明的实施例的生物体电极获得的一幅心电图波形。
具体实施方式
如上述,寻求开发出能形成用以展现高感度且低杂讯的生物体信号的高导电性及生物体适合性优异、轻量且能够以低成本制造,即使被水沾湿、即使干燥,导电性也不大幅下降,从皮肤剥离后于皮肤上不生残渣的生物体电极用的生物体接触层的生物体电极组成物、以该生物体电极组成物形成了生物体接触层的生物体电极、及其制造方法。
和心脏的搏动连动,会从皮肤表面放出钠、钾、钙离子。生物体电极需将从皮肤放出的离子的增减变换为电信号。所以,需要用以传达离子的增减的离子导电性优异的材料。和心脏的搏动连动,皮肤表面的电位也会变动。此电位变动微小,也需要用以将微弱电流传递到器件的电子传导性。
含有氯化钠、氯化钾的水溶性凝胶具有高离子导电性及电子导电性,但水干掉则丧失导电性。又,由于入浴、淋浴导致氯化钠、氯化钾溶出到生物体电极外,也会造成导电性降低。
使用金、银等金属的生物体电极仅可检知到微弱电流,离子导电性低,故作为生物体电极的感度低。碳和金属同样具有电子导电性,但电子导电性比金属更低,作为生物体电极的感度比金属更低。
PEDOT-PSS为代表的导电聚合物具有电子导电性及离子导电性两者,但极化低,故离子导电性低。
氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺的盐,极化性高,具有高离子导电性。本发明的目的为通过使其和碳粒子键结,以展现高离子导电性及电子导电性两者。
为了贴附于皮肤而稳定地获得生物体信号,生物体电极膜需有粘着性。另一方面,长时间贴附而剥离后若皮肤上有残渣,很可能成为起疹、皮肤粗糙的原因。为了不产生残渣,考量需为和碳粒子键结的离子性单体的形态,乃完成本发明。
本申请发明人等提出:含有键结于碳粒子的离子性单体的生物体电极组成物作为生物体电极组成物、及将其硬化成的生物体电极。
形成中和盐的酸,若酸性度高则离子会强极化,离子导电性提高。就锂离子电池而言,双(三氟甲烷磺酰基)酰亚胺酸、三(三氟甲烷磺酰基)甲基化酸的锂盐显示高离子导电性即是因此缘故。另一方面,有在成为中和盐前的酸的状态下酸强度越高,则其盐的生物体刺激性越强的问题。即,离子导电性与生物体刺激性处于取舍关系。但是使用在生物体电极的盐,必需兼顾高离子导电特性及低生物体刺激性。
离子化合物的分子量越大,则有对于皮肤的渗透性越降低且对于皮肤的刺激性越降低的特性。因而离子化合物宜为高分子量的聚合物型、键结于碳、二氧化硅等粒子的形态较佳。本申请发明人等想到添加离子性单体和碳粉键结成的复合体,借此,即使于皮肤长时间贴附后剥离也不产生残渣。
进而,通过使用将此盐混合在例如聚硅氧系、丙烯酸系、氨基甲酸乙酯系的粘着剂(树脂)而得者,能一直和皮肤密合且长时间获得稳定的电信号。
为了构成高感度的生物体电极,不仅需高离子导电性,高电子导电性亦为重要。为了提高电子导电性,添加金属粉、碳粉是有效的。
也即本发明是一种生物体电极组成物,含有(A)具有离子性官能团的单体与碳粒子的反应复合体,
前述(A)成分含有:和具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体键结的碳粒子。
以下针对本发明详细说明,但本发明不限于这些。
<生物体电极组成物>
本发明的生物体电极组成物含有(A)具有离子性官能团的单体(离子性单体)与碳粒子的反应复合体,且较佳为含有(B)粘着性树脂。以下针对各成分更详细说明。
[(A)具有离子性官能团的单体与碳粒子的反应复合体(盐)]
本发明的生物体电极组成物中,(A)具有离子性官能团的单体与碳粒子的反应复合体(离子性单体与粒子的复合体盐),是和具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体键结的碳粒子。较佳为除了上述离子性的结构更利用具氧杂环丙烷基或氧杂环丁烷基的单体、和碳粒子反应而键结成的材料。
选自氟磺酸、氟磺酰亚胺、N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构,宜以下列通式(1)-1至(1)-4表示较佳。
[化4]
式中,Rf1及Rf2为氢原子、氟原子、氧原子、甲基、或三氟甲基,Rf1及Rf2为氧原子时,Rf1及Rf2是键结于1个碳原子而形成羰基的1个氧原子,Rf3及Rf4为氢原子、氟原子、或三氟甲基,Rf1~Rf4中的一者以上为氟原子或三氟甲基。Rf5、Rf6、Rf7为氟原子、碳数1~4的直链状、分支状的烷基,且具有至少1个以上的氟原子。m为1~4的整数。M+是选自铵离子、锂离子、钠离子、钾离子、银离子的离子。
具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体,宜为除了这些结构更具有氧杂环丙烷基或氧杂环丁烷基的单体较佳,下列通式(2)-1~(2)-4表示者较佳。
[化5]
式中,R1为碳数1~8的亚烷基,也可和R3键结而形成环,也可具有醚基。R2为氢原子、碳数1~4的烷基,R3为单键或碳数1~20的直链状、分支状、环状的亚烷基,也可以具有芳香族基、醚键、酯键、羟基、氮原子。R4为单键或亚甲基。R5为单键、或也可以具有醚基、酯基的碳数1~10的(n+1)价烃基。n为1或2。Rf1~Rf7、M+、及m同前所述。
Rf1~Rf7宜为氟原子、氢原子、三氟甲基较佳。
上述通式(2)-1表示的单体具体而言可列举如下。
[化6]
[化7]
[化8]
[化9]
[化10]
[化11]
[化12]
[化13]
[化14]
[化15]
[化16]
[化17]
[化18]
[化19]
[化20]
[化21]
[化22]
[化23]
[化24]
[化25]
[化26]
[化27]
上述通式(2)-2表示的单体具体而言可列举如下。
[化28]
上述通式(2)-3表示的单体具体而言可列举如下。
[化29]
[化30]
[化31]
[化32]
[化33]
上述通式(2)-4表示的单体具体而言可列举如下。
[化34]
[化35]
[化36]
[化37]
[化38]
式中,M+如上所述。
又,(A)成分中,针对构成铵盐的铵离子,尤其,上述通式(2)-1~(2)-4表示的单体中的M+宜含有下列通式(3)表示的铵离子(铵阳离子)较佳。
[化39]
式中,R101d、R101e、R101f、R101g各为氢原子、碳数1~13的直链状、分支状、或环状的烷基、碳数2~12的直链状、分支状、或环状的烯基或炔基、或碳数4~20的芳香族基,也可具有选自醚基、羰基、酯基、羟基、氨基、硝基、磺酰基、亚磺酰基、卤素原子、及硫原子中的1种以上。R101d与R101e、R101d与R101e与R101f,也可和它们所键结的氮原子一起形成环,形成环时,R101d与R101e及R101d与R101e与R101f是形成碳数3~10的亚烷基、或形成环中具有式中的氮原子的杂芳香族环。
上述通式(3)表示的铵离子具体而言可列举如下。
[化40]
[化41]
[化42]
[化43]
[化44]
[化45]
[化46]
[化47]
[化48]
[化49]
[化50]
[化51]
[化52]
[化53]
[化54]
[化55]
上述通式(3)表示的铵离子宜为叔或季铵离子尤佳。
针对和具有离子性官能团的单体(离子性单体)(尤其通式(2)-1~(2)-4的单体)反应的碳粒子(碳粉),可列举炭黑、纳米碳管、石墨(graphite)、石墨烯。纳米碳管、石墨烯可为单层也可具有多层结构。又,碳粒子宜具有羟基、羧基、氨基等反应性基较佳。
(A)成分中的离子性单体宜具有氧杂环丙烷基、氧杂环丁烷基较佳,其会和碳粒子表面的羟基、羧基、氨基反应并键结。
又,(A)成分宜为相对于碳粒子100质量份使离子性单体(尤其通式(2)-1~(2)-4的单体)5质量份以上反应而得者较佳。
通过离子性单体悬吊于碳粉,离子导电性与电子导电性皆提升,不仅生物体电极的感度提升,尚能防止离子性单体萃取到生物体电极膜外,能防止因萃取导致生物体信号感度下降,对于皮肤的渗透性也降低而对皮肤的刺激性下降,故更能防止通过皮肤而引起过敏。
离子性单体通过和碳粉反应,离子性单体会因化学键而附着在碳粉表面。
用以使离子性单体和碳粉复合的反应,可将离子性单体与碳粉混合并于室温或利用加热而使反应进行。可利用加热促进反应,但加热温度若过高,会发生离子性单体分解,故加热温度为300℃以下较佳。
也可添加用以促进反应的催化剂。离子性单体具有氧杂环丙烷基、氧杂环丁烷基且碳粉具有羧基时,催化剂可列举吡啶、2-乙基咪唑、叔胺、2-乙基己酸锌、乙酰基丙酮铝等金属化合物。
本发明的生物体电极组成物中,(A)成分的掺合量相对于后述(B)成分100质量份为0.1~300质量份较佳,1~200质量份更佳。又,(A)成分可单独使用1种也可将2种以上混合使用。
含有通式(2)-1~(2)-4表示的离子成分及氧杂环丙烷基、氧杂环丁烷基的单体,有时在和碳粉的反应中没有完全消耗。于此情形,未反应的单体可利用碳粉的溶剂洗净来除去。氧杂环丙烷基、氧杂环丁烷基进行阳离子聚合而生成高分子化合物时,不会有作为生物体电极的性能降低、或对于皮肤的刺激性增强的情形。
[(B)粘着性树脂]
本发明的生物体电极组成物中掺合的(B)粘着性树脂,为了和上述(A)离子性碳粉互容并将其固持,并且固持金属粉、碳粉、硅粉、钛酸锂粉等导电性增进剂、离子性聚合物、保湿剂等添加材料并使粘着性展现的成分。又,(B)成分的树脂,宜为热硬化性树脂及光硬化性树脂中的任一、或它们两者较佳,尤其宜为选自聚硅氧系(聚硅氧树脂)、丙烯酸系((甲基)丙烯酸酯树脂)、及氨基甲酸酯系(氨基甲酸酯树脂)的树脂中的1种以上较佳。
粘着性聚硅氧系的树脂可列举加成反应硬化型或自由基交联反应硬化型者。加成反应硬化型,例如可使用日本特开2015-193803号公报记载的含有具有烯基的二有机硅氧烷、具有R3SiO0.5及SiO2单元的MQ树脂、具有多个SiH基的有机氢聚硅氧烷、铂催化剂、加成反应控制剂、及有机溶剂者。又,自由基交联反应硬化型,可使用例如日本特开2015-193803号公报记载的含有可以具有也可不具有烯基的二有机聚硅氧烷、具有R3SiO0.5及SiO2单元的MQ树脂、有机过氧化物、及有机溶剂者。在此,R为碳数1~10的经取代或未经取代的一价烃基。
又,也可使用聚合物末端、侧链具有硅醇的聚硅氧烷和MQ树脂进行缩合反应而形成的聚硅氧烷/树脂一体型化合物。MQ树脂有许多硅醇,故通过添加MQ树脂,粘着力会提高,但无交联性,故不会和聚硅氧烷以分子键结。如上述,通过聚硅氧烷与树脂成为一体型,能够使粘着力增大。
又,聚硅氧系的树脂也可添加具有选自氨基、氧杂环丙烷基、氧杂环丁烷基、聚醚基、羟基、羧基、巯基、甲基丙烯酸基、丙烯酸基、苯酚基、硅醇基、羧酸酐基、芳基、芳烷基、酰胺基、酯基、内酯环中的基团的改性硅氧烷。通过添加改性硅氧烷,(A)成分在聚硅氧树脂中的分散性提高。改性硅氧烷可为硅氧烷的单末端、两末端、侧链中的任一者经改性者。
粘着性丙烯酸系的树脂,可使用例如日本特开2016-011338号公报记载的具有亲水性(甲基)丙烯酸酯、长链疏水性(甲基)丙烯酸酯作为重复单元者。视情形,也可将具有官能团的(甲基)丙烯酸酯、具有硅氧烷键的(甲基)丙烯酸酯予以共聚合。
粘着性氨基甲酸酯系的树脂,可使用例如日本特开2016-065238号公报记载的具有氨基甲酸酯键及聚醚、聚酯键、聚碳酸酯键、硅氧烷键的树脂。
又,为了防止由于(A)成分从生物体接触层脱落导致导电性下降,本发明的生物体电极组成物中,(B)成分的树脂宜为和上述(A)成分相容性高者较佳。又,为了防止生物体接触层从导电性基材剥离,本发明的生物体电极组成物中,(B)成分的树脂宜为对于导电性基材的粘接性高的树脂较佳。为了使(B)成分的树脂成为和导电性基材、盐的相容性高的树脂,使用极性高的树脂是为有效。如此的树脂可列举具有选自醚键、酯键、酰胺键、酰亚胺键、氨基甲酸酯键、硫代氨基甲酸酯键、及硫醇基中的1个以上的树脂、或聚丙烯酸树脂、聚酰胺树脂、聚酰亚胺树脂、聚氨基甲酸酯树脂、及聚硫代氨基甲酸酯树脂等。又,另一方面,生物体接触层和生物体接触,故易受到来自生物体的汗水影响。因此本发明的生物体电极组成物中,(B)成分的树脂宜为拨水性高而不易水解的树脂较佳。为了使(B)成分的树脂成为拨水性高而不易水解的树脂,使用含硅的树脂是有效的。
针对含有硅原子的聚丙烯酸树脂,有主链具有聚硅氧的聚合物及侧链具有硅原子的聚合物,皆能理想地使用。针对主链具有聚硅氧的聚合物,可使用具有(甲基)丙烯酸基丙基的硅氧烷或倍半硅氧烷等。于此情形,可通过添加光自由基发生剂,使(甲基)丙烯酸基部分聚合而使其硬化。
含有硅原子的聚酰胺树脂,例如可理想地使用日本特开2011-079946号公报、美国专利5981680号公报记载的聚酰胺聚硅氧树脂等。如此的聚酰胺聚硅氧树脂,例如可将两末端具有氨基的聚硅氧或两末端具有氨基的非聚硅氧化合物、和两末端具有羧基的非聚硅氧或两末端具有羧基的聚硅氧予以组合而合成。
又,也可使用羧酸酐与胺反应而获得的环化前的聚酰胺酸。聚酰胺酸的羧基的交联可使用环氧系、氧杂环丁烷系的交联剂,也可进行羧基与(甲基)丙烯酸羟基乙酯的酯化反应,再进行(甲基)丙烯酸酯部分的光自由基交联。
针对含有硅原子的聚酰亚胺树脂,可理想地使用例如日本特开2002-332305号公报记载的聚酰亚胺聚硅氧树脂等。聚酰亚胺树脂的粘性非常高,但通过掺合(甲基)丙烯酸系单体作为溶剂且作为交联剂,能成为低粘性。
含有硅原子的聚氨基甲酸酯树脂可列举聚氨基甲酸酯聚硅氧树脂,如此的聚氨基甲酸酯聚硅氧树脂,可通过将两末端具有异氰酸酯基的化合物与末端具有羟基的化合物掺混并加热,而进行利用氨基甲酸酯键所为的交联。又,于此情形,需两末端具有异氰酸酯基的化合物、或末端具有羟基的化合物的任一或两者中含有硅原子(硅氧烷键)。或也可如日本特开2005-320418号公报记载,使聚硅氧烷和氨基甲酸酯(甲基)丙烯酸酯单体掺混而使其进行光交联。又,也可将具有硅氧烷键与氨基甲酸酯键两者且末端具有(甲基)丙烯酸酯基的聚合物进行光交联。尤其日本特开2018-123304号公报、日本特开2019-70109号公报记载的侧链附有聚硅氧链的聚氨基甲酸酯主链的材料,具有高强度且高伸缩的特性,故为理想。
含有硅原子的聚硫代氨基甲酸酯树脂,可通过具有硫醇基的化合物与具有异氰酸酯基的化合物的反应而得,它们中的任一者含有硅原子即可。又,末端具有(甲基)丙烯酸酯基的话,也可使其光硬化。
聚硅氧系的树脂中,添加上述具有烯基的二有机硅氧烷、具有R3SiO0.5及SiO2单元的MQ树脂、具有多个SiH基的有机氢聚硅氧烷以外,更添加具有选自氨基、氧杂环丙烷基、氧杂环丁烷基、聚醚基、羟基、羧基、巯基、甲基丙烯酸基、丙烯酸基、苯酚基、硅醇基、羧酸酐基、芳基、芳烷基、酰胺基、酯基、内酯环的基团的改性硅氧烷,则和上述盐的相容性更高。
可使具有烯基的二有机硅氧烷、与具有多个SiH基的有机氢聚硅氧烷,利用使用铂催化剂所为的加成反应进行交联。
针对铂催化剂,可列举氯化铂酸、氯化铂酸的醇溶液、氯化铂酸与醇的反应产物、氯化铂酸与烯烃化合物的反应产物、氯化铂酸与含乙烯基的硅氧烷的反应产物、铂-烯烃错合物、铂-含乙烯基的硅氧烷错合物等铂系催化剂、铑错合物及钌错合物等铂族金属系催化剂等。又,也可使这些催化剂溶解/分散于醇系、烃系、硅氧烷系溶剂再使用。
又,铂催化剂的添加量相对于(B)成分的树脂100质量份为5~2,000ppm,尤其10~500ppm的范围较佳。
本发明的生物体电极组成物中,(B)成分的掺合量相对于(A)成分的离子碳粉100质量份为0~10000质量份较佳,10~5000质量份更佳。又,(B)成分可单独使用1种也可混用2种以上。
又,使用加成硬化型的聚硅氧树脂时,也可添加加成反应控制剂。此加成反应控制剂是作为用以使铂催化剂在溶液中及涂膜形成后的加热硬化前的低温环境下不作用的淬灭剂而添加。具体而言,可列举3-甲基-1-丁炔-3-醇、3-甲基-1-戊炔-3-醇、3,5-二甲基-1-己炔-3-醇、1-乙炔基环己醇、3-甲基-3-三甲基硅氧基-1-丁炔、3-甲基-3-三甲基硅氧基-1-戊炔、3,5-二甲基-3-三甲基硅氧基-1-己炔、1-乙炔基-1-三甲基硅氧基环己烷、双(2,2-二甲基-3-丁炔氧)二甲基硅烷、1,3,5,7-四甲基-1,3,5,7-四乙烯基环四硅氧烷、1,1,3,3-四甲基-1,3-二乙烯基二硅氧烷等。
加成反应控制剂的添加量相对于(B)成分的树脂100质量份为0~10质量份,尤其0.05~3质量份的范围较佳。
这些之中,针对(B)成分的树脂,宜含有具烯基的二有机硅氧烷、及具SiH基的有机氢聚硅氧烷更佳,更含有具有RxSiO(4-x)/2单元(R为碳数1~10的经取代或未经取代的一价烃基、x为2.5~3.5的范围。)及SiO2单元的聚硅氧树脂尤佳。
又,如后述,生物体接触层是生物体电极组成物的硬化物。通过使其硬化,生物体接触层对于皮肤及导电性基材两者的的粘接性会变得良好。又,硬化手段不特别限定,可使用一般的手段,例如可使用热及光中任一者、或其两者、或利用酸或碱催化剂的交联反应等。交联反应可例如适当选择交联反应手册(中山雍晴,丸善出版(2013年)第二章p51~p371)记载的方法进行。
[(C)离子性聚合物]
本发明的生物体电极组成物中,可添加离子性聚合物作为(C)成分,该离子性聚合物含有具离子性重复单元的高分子化合物,较佳为具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、及银盐的结构的重复单元。离子性聚合物的重复单元可使用日本特开2020-002342号公开的段落0058~0130记载者。离子性聚合物的添加量相对于(B)成分的树脂100质量份为0.1~100质量份的范围较佳。
[(D)导电性粉末]
[金属粉]
本发明的生物体电极组成物中,为了提高电子导电性,也可添加选自金、银、铂、铜、锡、钛、镍、铝、钨、钼、钌、铬、铟的金属粉作为(D)成分。金属粉的添加量相对于(B)成分的树脂100质量份为1~50质量份的范围较佳。
针对金属粉的种类,考量导电性的观点,金、银、铂较理想,考量价格的观点,银、铜、锡、钛、镍、铝、钨、钼、钌、铬为较佳。考量生物体适合性的观点,贵金属较理想,综合考量这些观点,银最理想。
金属粉的形状可列举球状、圆盘状、屑片状、针状,但添加屑片状的粉末时,导电性最高,为较理想。金属粉的尺寸为100μm以下、振实密度为5g/cm3以下、比表面积0.5m2/g以上的密度较低且比表面积大的屑片为较佳。
[碳粉]
可添加(A)成分以外的碳材料(碳粉)作为导电性增进剂。碳材料可列举炭黑、石墨、纳米碳管、碳纤维等。纳米碳管为单层、多层皆可,表面经有机基团修饰也可。碳材料的添加量相对于(B)成分的树脂100质量份为1~50质量份的范围较佳。
[硅粉]
本发明的生物体电极组成物中,为了提高离子接受感度,也可添加硅粉。硅粉可列举包括硅、一氧化硅、碳化硅的粉体。粉体的粒径不特别限定,宜小于100μm较理想,更佳为1μm以下。更细小的粒子的表面积大,能接受许多离子,成为高感度的生物体电极。硅粉的添加量相对于树脂100质量份为1~50质量份的范围较佳。
[钛酸锂粉]
本发明的生物体电极组成物中,为了提高离子接受感度,也可添加钛酸锂粉。钛酸锂粉可列举Li2TiO3、LiTiO2、尖晶石结构的Li4Ti5O12的分子式,尖晶石结构品较佳。又,也可使用和碳复合的钛酸锂粒子。粉体的粒径宜小于100μm较理想,更佳为1μm以下。较细小的粒子的表面积大,能接受许多离子,成为高感度的生物体电极。它们也可为和碳的复合粉。钛酸锂粉的添加量相对于树脂100质量份为1~50质量份的范围较佳。
[(E)有机溶剂]
又,本发明的生物体电极组成物中可添加有机溶剂作为(E)成分。有机溶剂具体而言可列举甲苯、二甲苯、异丙苯、1,2,3-三甲基苯、1,2,4-三甲基苯、1,3,5-三甲基苯、苯乙烯、α甲基苯乙烯、丁基苯、仲丁基苯、异丁基苯、异丙基甲苯、二乙基苯、2-乙基对二甲苯、2-丙基甲苯、3-丙基甲苯、4-丙基甲苯、1,2,3,5-四甲基甲苯、1,2,4,5-四甲基甲苯、四氢萘、4-苯基-1-丁烯、叔戊基苯、戊基苯、2-叔丁基甲苯、3-叔丁基甲苯、4-叔丁基甲苯、5-异丙基间二甲苯、3-甲基乙基苯、叔丁基-3-乙基苯、4-叔丁基邻二甲苯、5-叔丁基间二甲苯、叔丁基对二甲苯、1,2-二异丙基苯、1,3-二异丙基苯、1,4-二异丙基苯、二丙基苯、五甲基苯、六甲基苯、己基苯、1,3,5-三乙基苯等芳香族系烃系溶剂、正庚烷、异庚烷、3-甲基己烷、2,3-二甲基戊烷、3-乙基戊烷、1,6-庚二烯、5-甲基-1-己炔、降莰烷、降莰烯、二环戊二烯、1-甲基-1,4-环己二烯、1-庚炔、2-庚炔、环庚烷、环庚烯、1,3-二甲基环戊烷、乙基环戊烷、甲基环己烷、1-甲基-1-环己烯、3-甲基-1-环己烯、亚甲基环己烷、4-甲基-1-环己烯、2-甲基-1-己烯、2-甲基-2-己烯、1-庚烯、2-庚烯、3-庚烯、正辛烷、2,2-二甲基己烷、2,3-二甲基己烷、2,4-二甲基己烷、2,5-二甲基己烷、3,3-二甲基己烷、3,4-二甲基己烷、3-乙基-2-甲基戊烷、3-乙基-3-甲基戊烷、2-甲基庚烷、3-甲基庚烷、4-甲基庚烷、2,2,3-三甲基戊烷、2,2,4-三甲基戊烷、环辛烷、环辛烯、1,2-二甲基环己烷、1,3-二甲基环己烷、1,4-二甲基环己烷、乙基环己烷、乙烯基环己烷、异丙基环戊烷、2,2-二甲基-3-己烯、2,4-二甲基-1-己烯、2,5-二甲基-1-己烯、2,5-二甲基-2-己烯、3,3-二甲基-1-己烯、3,4-二甲基-1-己烯、4,4-二甲基-1-己烯、2-乙基-1-己烯、2-甲基-1-庚烯、1-辛烯、2-辛烯、3-辛烯、4-辛烯、1,7-辛二烯、1-辛炔、2-辛炔、3-辛炔、4-辛炔、正壬烷、2,3-二甲基庚烷、2,4-二甲基庚烷、2,5-二甲基庚烷、3,3-二甲基庚烷、3,4-二甲基庚烷、3,5-二甲基庚烷、4-乙基庚烷、2-甲基辛烷、3-甲基辛烷、4-甲基辛烷、2,2,4,4-四甲基戊烷、2,2,4-三甲基己烷、2,2,5-三甲基己烷、2,2-二甲基-3-庚烯、2,3-二甲基-3-庚烯、2,4-二甲基-1-庚烯、2,6-二甲基-1-庚烯、2,6-二甲基-3-庚烯、3,5-二甲基-3-庚烯、2,4,4-三甲基-1-己烯、3,5,5-三甲基-1-己烯、1-乙基-2-甲基环己烷、1-乙基-3-甲基环己烷、1-乙基-4-甲基环己烷、丙基环己烷、异丙基环己烷、1,1,3-三甲基环己烷、1,1,4-三甲基环己烷、1,2,3-三甲基环己烷、1,2,4-三甲基环己烷、1,3,5-三甲基环己烷、烯丙基环己烷、八氢茚、1,8-壬二烯、1-壬炔、2-壬炔、3-壬炔、4-壬炔、1-壬烯、2-壬烯、3-壬烯、4-壬烯、正癸烷、3,3-二甲基辛烷、3,5-二甲基辛烷、4,4-二甲基辛烷、3-乙基-3-甲基庚烷、2-甲基壬烷、3-甲基壬烷、4-甲基壬烷、叔丁基环己烷、丁基环己烷、异丁基环己烷、4-异丙基-1-甲基环己烷、戊基环戊烷、1,1,3,5-四甲基环己烷、环十二烷、1-癸烯、2-癸烯、3-癸烯、4-癸烯、5-癸烯、1,9-癸二烯、十氢萘、1-癸炔、2-癸炔、3-癸炔、4-癸炔、5-癸炔、1,5,9-癸三烯、2,6-二甲基-2,4,6-辛三烯、柠檬烯、香叶烯、1,2,3,4,5-五甲基环戊二烯、α-水芹烯、蒎烯、萜品烯、四氢二环戊二烯、5,6-二氢二环戊二烯、1,4-癸二炔、1,5-癸二炔、1,9-癸二炔、2,8-癸二炔、4,6-癸二炔、正十一烷、戊基环己烷、1-十一碳烯、1,10-十一碳二烯、1-十一炔、3-十一炔、5-十一炔、三环[6.2.1.02,7]十一碳-4-烯、正十二烷、2-甲基十一烷、3-甲基十一烷、4-甲基十一烷、5-甲基十一烷、2,2,4,6,6-五甲基庚烷、1,3-二甲基金刚烷、1-乙基金刚烷、1,5,9-环十二碳三烯、1,2,4-三乙烯基环己烷、ISOPAR C、ISOPARE、ISOPARG、ISOPAR H、ISOPAR L、ISOPAR M、ISOPAR V等异烷烃等脂肪族烃系溶剂、环己酮、环戊酮、2-辛酮、2-壬酮、2-庚酮、3-庚酮、4-庚酮、2-己酮、3-己酮、二异丁基酮、甲基环己酮、甲基正戊基酮等酮系溶剂、3-甲氧基丁醇、3-甲基-3-甲氧基丁醇、1-甲氧基-2-丙醇、1-乙氧基-2-丙醇等醇系溶剂、丙二醇单甲醚、乙二醇单甲醚、丙二醇单乙醚、乙二醇单乙醚、丙二醇二甲醚、二乙二醇单甲醚、二乙二醇单乙醚、二乙二醇单丙醚、二乙二醇单丁醚、二乙二醇单戊醚、二乙二醇单庚醚、二乙二醇二乙醚、二乙二醇二丙醚、二乙二醇二丁醚、二异丙醚、二异丁醚、二异戊醚、二正戊醚、甲基环戊醚、甲基环己醚、二正丁醚、二仲丁醚、二异戊醚、二仲戊醚、二叔戊醚、二正己醚、苯甲醚等醚系溶剂、丙二醇单甲醚乙酸酯、丙二醇单乙醚乙酸酯、乳酸乙酯、丙酮酸乙酯、乙酸丁酯、3-甲氧基丙酸甲酯、3-乙氧基丙酸乙酯、乙酸叔丁酯、丙酸叔丁酯、丙二醇单叔丁醚乙酸酯等酯系溶剂、γ-丁内酯等内酯系溶剂、水等。
又,有机溶剂的添加量相对于(B)成分的树脂100质量份为10~50,000质量份的范围较佳。
[(F)其他添加剂]
本发明的生物体电极组成物中,除了在(B)成分的项目叙述的铂催化剂、加成反应控制剂以外,也可以混合交联剂、交联催化剂、离子性添加剂,此外也可以混合二氧化硅粒子、聚醚聚硅氧、聚甘油聚硅氧。二氧化硅粒子表面为亲水性,和亲水性离子聚合物、聚醚聚硅氧、聚甘油聚硅氧的相容良好,能够提升离子性聚合物、聚醚聚硅氧、聚甘油聚硅氧在疏水性聚硅氧粘着剂的分散性。二氧化硅粒子于干式、湿式皆能理想地使用。
[交联剂]
本发明的生物体电极组成物中也可添加环氧系的交联剂。此时的交联剂,是1分子内有多个环氧基、氧杂环丁烷基的化合物。针对添加量,相对于(B)成分的树脂100质量份,为1~30质量份。
[交联催化剂]
本发明的生物体电极组成物中也可添加用以将环氧基、氧杂环丁烷基予以交联的催化剂。此时的催化剂,可添加日本特表2019-503406号中的段落0027~0029记载者。添加量相对于(B)成分的树脂100质量份为0.01~10质量份。
[离子性添加剂]
本发明的生物体电极组成物中可添加用以提高离子导电性的离子性添加剂。若考量生物体适合性,可列举氯化钠、氯化钾、氯化钙、氯化镁、糖精钠盐、乙酰磺胺酸钾、羧酸钠、羧酸钾、羧酸钙、磺酸钠、磺酸钾、磺酸钙、磷酸钠、磷酸钾、磷酸钙、磷酸镁、甜菜碱、日本特开2018-44147号公开、日本特开2018-59050号公开、日本特开2018-59052号公开、日本特开2018-130534号公开的盐。
(具有聚甘油结构的聚硅氧化合物)
本发明的生物体电极组成物中,为了提升膜的保湿性而使从皮肤放出的离子的感受性及离子导电性更好,也可添加具有聚甘油结构的聚硅氧化合物。具有聚甘油结构的聚硅氧化合物的掺合量相对于(A)成分与(B)成分的合计100质量份为0.01~100质量份较佳,0.5~60质量份更佳。又,具有聚甘油结构的聚硅氧化合物可单独使用1种,也可将2种以上混合使用。
具有聚甘油结构的聚硅氧化合物宜为下列通式(4)’及(5)’表示者较佳。
[化56]
式(4)’及(5)’中,R1’各自独立,可彼此相同也可不同,为氢原子或碳数1~50的直链状或分支状的烷基、或苯基,也可含有醚基,也可为通式(6)’表示的聚硅氧链,R2’为式(4)’-1或式(4)’-2表示的具聚甘油基结构的基团,R3’各自独立,可互为相同也可不同,为前述R1’基团或前述R2’基团,R4’各自独立,可互为相同也可不同,为前述R1’基团、前述R2’基团或氧原子。R4’为氧原子时,2个R4’基团也可键结成1个醚基并和硅原子一起形成环。a’可相同也可不同,为0~100,b’为0~100,a’+b’为0~200。但b’为0时,R3’的至少1个为前述R2’基团。式(4)’-1及(4)’-2、(5)’、(6)’中,R5’为碳数2~10的亚烷基或碳数7~10的亚芳烷基,R6’、R7’为碳数2~6的亚烷基,R7’可为醚键,c’为0~20,d’为1~20。
如此的具有聚甘油结构的聚硅氧化合物,例如可列举如下。
[化57]
[化58]
[化59]
[化60]
[化61]
[化62]
[化63]
[化64]
[化65]
[化66]
式中,a‘、b’、c’及d’如上所述。
若含有如此的具有聚甘油结构的聚硅氧化合物,则能显示更优良的保湿性,其结果,能成为可形成对于从皮肤放出的离子呈现更优良的感度的生物体接触层的生物体电极组成物。
如以上,若为本发明的生物体电极组成物,可成为能形成可将来自皮肤的电信号以良好效率传递到器件(也即导电性优异)、即使长期间装设于皮肤也无引起过敏之虞(也即生物体适合性优异)、轻量,且能以低成本制造,即使被水沾湿、即使干燥,导电性仍不大幅下降的生物体电极用的生物体接触层的生物体电极组成物。又,通过添加导电性粉末(碳粉、金属粉),能够使导电性更好,通过和有粘着性及伸缩性的树脂组合,可制造尤其高粘着力且高伸缩性的生物体电极。又,能利用添加剂等使得对于皮肤的伸缩性、粘着性更好,通过适当调节树脂的组成、生物体接触层的厚度,能够调整伸缩性、粘着性。
<生物体电极>
又,本发明提供一种生物体电极,具有导电性基材及形成在该导电性基材上的生物体接触层,前述生物体接触层是上述本发明的生物体电极组成物的硬化物。
以下针对本发明的生物体电极,边参照图式边详细说明,但本发明不限于这些。
图1显示本发明的生物体电极的一例的概略剖面图。图1的生物体电极1,具有:导电性基材2,及形成在该导电性基材2上的生物体接触层3。生物体接触层3,由本发明的生物体电极组成物的硬化物构成。构成生物体接触层3的离子单体复合碳粒子4是具有离子性官能团的单体与碳粒子的反应复合体(例如经该离子单体修饰的碳粉)。生物体接触层3可更含有前述离子单体复合碳粒子4以外的粘着性树脂6、离子性聚合物5。以下参照图1、2,针对生物体接触层3为离子单体复合碳粒子4及离子性聚合物5分散于粘着性树脂6中而得的层的情形说明,但本发明的生物体电极不限于此态样。
使用如此的图1的生物体电极1时,如图2,使生物体接触层3(也即离子单体复合碳粒子4及离子性聚合物5分散于粘着性树脂6中而得的层)接触生物体7,利用离子单体复合碳粒子4与离子性聚合物5从生物体7取出电信号,将其经由导电性基材2来传导到感测器器件等(未图示)。如此,若为本发明的生物体电极,能利用上述离子单体复合碳粒子4兼顾导电性及生物体适合性,也具有粘着性,故和皮肤的接触面积固定,能稳定地以高感度获得来自皮肤的电信号。
以下针对本发明的生物体电极的各构成材料更详细说明。
[导电性基材]
本发明的生物体电极具有导电性基材。此导电性基材通常和感测器器件等电连接,将经由生物体接触层从生物体取出的电信号传导到感测器器件等。
导电性基材只要有导电性即可,不特别限定,例如宜含有选自金、银、氯化银、铂、铝、镁、锡、钨、铁、铜、镍、不锈钢、铬、钛、碳及导电聚合物中的1种以上较佳。
又,导电性基材不特别限定,可为硬质的导电性基板等,也可为有可挠性的导电性薄膜、表面涂了导电性糊剂的布料、混入了导电性聚合物的布料。导电性基材可为平坦、也可为有凹凸、也可为织了金属线的网目状,可因应生物体电极的用途等适当选择。
[生物体接触层]
本发明的生物体电极具有形成于导电性基材上的生物体接触层。此生物体接触层,当使用生物体电极时是实际和生物体接触的部分,具有导电性及粘着性。生物体接触层是上述本发明的生物体电极组成物的硬化物,也即是由含有上述(A)成分、与视需要的(B)成分、(C)成分、(D)成分、(E)成分、其他(F)成分的组成物的硬化物构成的的粘着性的树脂层。
又,生物体接触层的粘着力宜为0.5N/25mm以上20N/25mm以下的范围较佳。粘着力的测定方法,一般是JIS Z 0237所示的方法,基材可使用如SUS(不锈钢)的金属基板、PET(聚对苯二甲酸乙二醇酯)基板,但也可使用人的皮肤进行测定。人皮肤的表面能量低于金属、各种塑胶,为接近特氟龙(注册商标)的低能量,是不易粘着的性质。
生物体电极的生物体接触层的厚度为1μm以上5mm以下较理想,2μm以上3mm以下更理想。生物体接触层越薄则粘着力越低,但可挠性提升,且变轻,对于皮肤的相容性变好。可综合考虑粘着性、对于皮肤的触感来选择生物体接触层的厚度。
又,本发明的生物体电极,和以往的生物体电极(例如:日本特开2004-033468号公报记载的生物体电极)同样,为了防止使用时生物体电极从生物体剥离,也可在生物体接触层上另外设置粘着膜。另外设置粘着膜时,使用丙烯酸型、氨基甲酸酯型、聚硅氧型等粘着膜材料来形成粘着膜即可,尤其聚硅氧型因透氧性高,皮肤在贴附状态下仍能呼吸,拨水性亦高,故因汗导致粘着性下降少,而且对于皮肤的刺激性低,故为理想。又,本发明的生物体电极,如上述,通过对于生物体电极组成物添加粘着性赋予剂、或使用对于生物体的粘着性良好的树脂,能够防止从生物体剥离,因此并非一定需要上述另外设置的粘着膜。
本发明的生物体电极制成穿戴式器件使用时,针对生物体电极与感测器器件的配线、其他构件,无特殊限定,例如可以采用日本特开2004-033468号公报记载者。
如以上,若为本发明的生物体电极,以上述本发明的生物体电极组成物的硬化物来形成生物体接触层,故可成为来自皮肤的电信号能够以良好效率传递到器件(也即导电性优异)、即使长期间装设于皮肤仍无引起过敏之虞(也即生物体适合性优异)、轻量,能够以低成本制造,即使被水沾湿、即使干燥,导电性仍不大幅下降的生物体电极。又,通过添加导电性粉末,能够使导电性更好,通过和有粘着性及伸缩性的树脂组合,能够制造特别高粘着力且伸缩性高的生物体电极。又,能够利用添加剂等使得对于皮肤的伸缩性、粘着性更好,能通过将树脂的组成、生物体接触层的厚度予以适当调节,来调整伸缩性、粘着性。因此,如此的若为本发明的生物体电极特别适合作为医疗用穿戴式器件中使用的生物体电极。
<生物体电极的制造方法>
又,本发明提供一种生物体电极的制造方法,是具有导电性基材及形成在该导电性基材上的生物体接触层的生物体电极的制造方法,通过在前述导电性基材上涂布上述本发明的生物体电极组成物并使其硬化,以形成前述生物体接触层。
又,本发明的生物体电极的制造方法使用的导电性基材等可和上述者相同。
在导电性基材上涂布生物体电极组成物的方法不特别限定,例如浸涂、喷涂、旋涂、辊涂、流涂、刮刀涂布、网版印刷、柔版印刷、照相凹版印刷、喷墨印刷等方法为宜。
树脂的硬化方法不特别限定,可视生物体电极组成物使用的(A)、(B)成分适当选择,例如利用热及光中任一者,或利用它们来使其硬化较佳。又,也可预先于上述生物体电极组成物添加会产生酸、碱的催化剂,借此产生交联反应并使其硬化。
又,加热时的温度不特别限定,可视生物体电极组成物使用的(A)、(B)成分适当选择,例如50~250℃左右较佳。
又,组合加热及照光时,可同时进行加热及照光,也可于照光后进行加热,也可于加热后进行照光。又,涂膜后的加热前,为了使溶剂蒸发,也可进行风干。
若于硬化后的膜表面滴水、或吹送水蒸气、雾滴,则和皮肤的互容性会提升,且能迅速地获得生物体信号。为了使水蒸气、雾滴的水滴的尺寸细小,也可使用混有醇的水。也可和含水的脱脂绵、布接触而沾湿膜表面。
沾湿硬化后的膜表面的水也可含有盐。和水混合的水溶性盐,是选自钠盐、钾盐、钙盐、镁盐、甜菜碱。
前述水溶性盐,具体而言,可为选自氯化钠、氯化钾、氯化钙、氯化镁、糖精钠盐、乙酰磺胺酸钾、羧酸钠、羧酸钾、羧酸钙、磺酸钠、磺酸钾、磺酸钙、磷酸钠、磷酸钾、磷酸钙、磷酸镁、甜菜碱的盐。又,前述水溶性盐不包括上述(A)成分及(C)成分。
更具体而言,除上述以外,尚可列举乙酸钠、丙酸钠、三甲基乙酸钠、甘醇酸钠、丁酸钠、戊酸钠、己酸钠、庚酸钠、辛酸钠、壬酸钠、癸酸钠、十一基酸钠、月桂酸钠、十三基酸钠、肉豆蔲酸钠、十五基酸钠、棕榈酸钠、十七酸钠、硬脂酸钠、苯甲酸钠、己二酸二钠、马来酸二钠、邻苯二甲酸二钠、2-羟基丁酸钠、3-羟基丁酸钠、2-氧代丁酸钠、葡萄糖酸钠、甲磺酸钠、1-壬烷磺酸钠、1-癸烷磺酸钠、1-十二烷磺酸钠、1-十一烷磺酸钠、椰子油脂基羟乙磺酸钠、月桂酰基甲基丙氨酸钠、椰子油脂基甲基牛磺酸钠、椰子油脂基谷氨酸钠、椰子油脂基钠、月桂酰基甲基牛磺酸钠、月桂酰胺丙基甜菜碱、异丁酸钾、丙酸钾、三甲基乙酸钾、甘醇酸钾、葡萄糖酸钾、甲磺酸钾、硬脂酸钙、甘醇酸钙、葡萄糖酸钙、3-甲基-2-氧代丁酸钙、甲磺酸钙。甜菜碱是分子内盐的总称,具体而言,是氨基酸的氨基加成了3个甲基的化合物,更具体而言,可列举三甲基甘氨酸、肉碱、脯氨酸甜菜碱。
沾湿硬化后的膜表面的水可更含有碳数1~4的一元醇或多元醇,前述醇宜是选自乙醇、异丙醇、乙二醇、二乙二醇、三乙二醇、甘油、聚乙二醇、聚丙二醇、聚甘油、二甘油、或具有聚甘油结构的聚硅氧化合物者较佳,前述具有聚甘油结构的聚硅氧化合物为上述通式(4)’、(5)’表示者更佳。
利用含水溶性盐的水溶液所为的前处理方法,可在硬化后的生物体电极膜上藉喷雾法、水滴点胶法等来涂布生物体电极膜。也可如桑拿般于高温高湿状态进行涂布。涂布后为了防止干燥,也可于浸透层之上进一步叠层保护薄膜以进行覆盖。保护薄膜需在即将贴于皮肤前剥离,所以,可使用涂有剥离剂、或剥离性的特氟龙(注册商标)薄膜。以剥离薄膜覆盖的干燥电极,为了长期间保存,宜以覆有铝等的袋子密封较佳。为了防止在覆有铝的袋中干燥,宜预先于其中封入水分较佳。
本发明的生物体电极贴于皮肤前,也可将皮肤侧以水、醇等沾湿、或以含有水、醇等的布、脱脂绵来擦拭皮肤。水、醇中也可含有前述盐。
如以上,若为本发明的生物体电极的制造方法,则能以低成本轻易地制造导电性及生物体适合性优异、轻量、即使被水沾湿、即使干燥,导电性仍不大幅下降的本发明的生物体电极。
实施例
以下使用实施例及比较例对于本发明具体说明,但本发明不限于这些。又,“Me”代表甲基,“Vi”代表乙烯基。
(离子性单体)
实施例使用的离子性单体1~14如下所示。
[化67]
(复合碳粒子)
于甲基异丁基酮(MIBK)100g中添加0.2g吡啶及5g炭黑:电化公司制DENKABLACKLi-400并搅拌,于其中滴加1g离子性单体1,于60℃搅拌20小时之后过滤,以MIBK溶液洗净2次并干燥,合成离子性单体1复合炭黑。
按同样的方法,合成离子性单体2复合炭黑~离子性单体14复合炭黑。
于甲基异丁基酮(MIBK)100g中,添加羧基化多层纳米碳管(SIGMA-Aldrich公司、平均直径9.5nm、平均长度1.5μm)5g及吡啶0.2g,搅拌并于其中滴加1g离子性单体5,于60℃搅拌20小时后过滤,以MIBK溶液洗净2次并干燥,合成离子性单体5复合多层纳米碳管。
于甲基异丁基酮(MIBK)100g中添加氧化石墨烯(SIGMA-Aldrich公司)5g及吡啶0.2g,搅拌并于其中滴加1g离子性单体10,于60℃搅拌20小时后过滤,以MIBK溶液洗净2次并干燥,合成离子性单体10复合氧化石墨烯。
于甲基异丁基酮(MIBK)100g中添加石墨(SIGMA-Aldrich公司)5g及吡啶0.2g,搅拌并于其中滴加1g离子性单体10,于60℃搅拌20小时后过滤,以MIBK溶液洗净2次并干燥,合成离子性单体10复合石墨。
(离子性聚合物)
作为生物体电极组成物溶液掺合的离子性聚合物1溶液,按以下方式合成。将各单体的20质量%环戊酮溶液装入到反应容器并混合,将反应容器于氮气环境下冷却到-70℃,重复3次减压脱气、吹氮。升温到室温后,添加作为聚合起始剂的偶氮双异丁腈(AIBN),其量为相对于单体全体1摩尔添加0.01摩尔,升温到60℃后,使其反应15小时,利用蒸发器使环戊酮蒸发。获得的聚合物的组成是将聚合物溶液的一部分干燥后,利用1H-NMR确认的。又,获得的聚合物的分子量(Mw)及分散度(Mw/Mn),利用使用四氢呋喃(THF)作为溶剂的凝胶渗透层析(GPC)来确认。离子性聚合物1如下所示。
离子性聚合物1
Mw=39,100
Mw/Mn=1.91
[化68]
式中的重复数代表平均值。
依和离子性聚合物1的合成方法同样的方法合成下列离子性聚合物2~5。
离子性聚合物2
Mw=33,300
Mw/Mn=1.83
[化69]
式中的重复数代表平均值。
离子性聚合物3
Mw=87,500
Mw/Mn=2.01
[化70]
式中的重复数代表平均值。
离子性聚合物4
Mw36,100
Mw/Mn=1.55
[化71]
式中的重复数代表平均值。
离子性聚合物5
Mw=38,300
Mw/Mn=2.01
[化72]
式中的重复数代表平均值。
(硅氧烷化合物)
在生物体电极组成物溶液中掺合作为聚硅氧系的树脂的硅氧烷化合物1~4如下所示。
(硅氧烷化合物1)
将于30%甲苯溶液的粘度为27,000mPa·s,烯基含量为0.007摩尔/100g,分子链末端经SiMe2Vi基封端的含乙烯基的聚二甲基硅氧烷,作为硅氧烷化合物1。
(硅氧烷化合物2)
将由Me3SiO0.5单元及SiO2单元构成的MQ树脂的聚硅氧烷(Me3SiO0.5单元/SiO2单元=0.8)的60%甲苯溶液,作为硅氧烷化合物2。
(硅氧烷化合物3)
令使30%甲苯溶液的粘度为42,000mPa·s、烯基含量为0.007摩尔/100g、分子链末端经OH封端的含乙烯基的聚二甲基硅氧烷40质量份、由Me3SiO0.5单元及SiO2单元构成的MQ树脂的聚硅氧烷(Me3SiO0.5单元/SiO2单元=0.8)的60%甲苯溶液100质量份、及甲苯26.7质量份所构成的溶液边干馏边加热4小时后予以冷却,而使聚二甲基硅氧烷键结于MQ树脂而得者为硅氧烷化合物3。
(硅氧烷化合物4)
使用信越化学工业制KF-99作为甲基氢聚硅氧油。
(聚甘油聚硅氧化合物)
聚甘油聚硅氧化合物1~7如下列所示。
[化73]
(有机溶剂)
在生物体电极组成物溶液中掺合的有机溶剂如下所示。
ISOPAR G:异烷烃系溶剂标准石油制
ISOPAR M:异烷烃系溶剂标准石油制
(添加剂)
在生物体电极组成物溶液中掺合作为添加剂的钛酸锂粉、铂催化剂、导电性增进剂(炭黑、纳米碳管、石墨、银粉)如下所示。
金属粉银粉:Sigma-Aldrich公司制银屑片,直径10μm
钛酸锂粉、尖晶石:Sigma-Aldrich公司制,尺寸200nm以下
铂催化剂:信越化学工业制,CAT-PL-50T
炭黑:电化公司制DENKABLACK Li-400
多层纳米碳管:Sigma-Aldrich公司制,直径110~170nm、长度5~9μm
石墨:Sigma-Aldrich公司制直径20μm以下
[实施例1~17、比较例1、2]
按表1至表3记载的组成,将离子性单体复合炭黑、离子性单体复合多层纳米碳管、离子性单体复合氧化石墨烯、离子性单体复合石墨、树脂、离子性聚合物、有机溶剂、及添加剂(铂催化剂、导电性增进剂)掺混,制备成生物体电极组成物溶液(生物体电极组成物溶液1~17、比较生物体电极组成物溶液1、2)。
[表1]
[表2]
[表3]
(生物体电极的制作)
如图3,在百美贴(Bemis)公司的热塑性氨基甲酸酯(TPU)薄膜20的ST-604上,利用网版印刷涂布藤仓化成制的导电糊剂、DOTITE FA-333,于120℃在烘箱中烘烤10分钟,印刷圆直径2cm的锁孔状的导电图案2。将表1~3记载的生物体电极组成物溶液以网版印刷涂布重叠于该导电图案之上的圆形部分,于室温风干10分钟后,使用烘箱于125℃进行20分钟烘烤,使溶剂蒸发并使其硬化,形成生物体接触层3,制得生物体电极1。然后,如图4所示,切取已印刷生物体电极1的氨基甲酸酯薄膜,并对其贴附双面贴带21,就1份组成物溶液制得3个生物体电极样本10。
(生物体接触层的厚度测定)
使用测微计测定上述制作的生物体电极中的生物体电极层的厚度。结果示于表4。
(生物体信号的测定)
将生物体电极的利用导电糊剂得到的导电配线图案与欧姆龙健康事业(股)制可携式心电计HCG-901以导电线连接,将心电计的正电极贴在图5中的人体的LA处、负电极贴在LL处、接地贴在RA处。贴附后即开始测定心电图,量测直到出现图6所示的由P、Q、R、S、T波构成的心电图波形的时间,结果示于表4。
[表4]
如表4,使用掺合了离子聚合物与碳粉的复合体的本发明的生物体电极组成物来形成生物体接触层的实施例1~17,贴附在身体后能于短时间获得生物体信号。另一方面,仅添加碳粒子的比较例1无法获得生物体信号,仅添加离子性聚合物及碳粒子的比较例2,从贴于皮肤直到展现生物体信号为止的时间长。
又,本发明不限于上述实施形态。上述实施形态是例示的,和本发明的权利要求书记载的技术思想有实质上相同一构成且发挥同样作用效果者,皆包括在本发明的技术范围内。
附图标记说明
1:生物体电极
2:导电性基材(导电图案)
3:生物体接触层
4:离子单体复合碳粒子
5:离子性聚合物
6:粘着性树脂
7:生物体
10:生物体电极样本
20:热塑性氨基甲酸酯薄膜
21:双面贴带
LA:正电极贴附处
LL:负电极贴附处
RA:接地贴附处。
Claims (23)
1.一种生物体电极组成物,含有(A)具有离子性官能团的单体与碳粒子的反应复合体,该(A)成分含有:和具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体键结的碳粒子。
2.根据权利要求1所述的生物体电极组成物,其中,该碳粒子选自炭黑、纳米碳管、石墨、石墨烯。
3.根据权利要求1或2所述的生物体电极组成物,其中,该具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体,具有下列通式(1)-1至(1)-4中任一者表示的结构;
式中,Rf1及Rf2为氢原子、氟原子、氧原子、甲基、或三氟甲基,Rf1及Rf2为氧原子时,Rf1及Rf2是键结于1个碳原子而形成羰基的1个氧原子,Rf3及Rf4为氢原子、氟原子、或三氟甲基,Rf1~Rf4中的1个以上为氟原子或三氟甲基;
Rf5、Rf6、Rf7为氟原子、碳数1~4的直链状、分支状的烷基,且具有至少1个以上的氟原子;
m为1~4的整数;
M+是选自铵离子、锂离子、钠离子、钾离子、银离子的离子。
5.根据权利要求1或2所述的生物体电极组成物,其中,该(A)成分是相对于该碳粒子100质量份使该具有离子性官能团的单体5质量份以上反应而得的。
6.根据权利要求1或2所述的生物体电极组成物,其中,该(A)成分含有下列通式(3)表示的铵离子作为构成该铵盐的铵离子;
式中,R101d、R101e、R101f、R101g各为氢原子、碳数1~13的直链状、分支状、或环状的烷基、碳数2~12的直链状、分支状、或环状的烯基或炔基、或碳数4~20的芳香族基,也可具有选自醚基、羰基、酯基、羟基、氨基、硝基、磺酰基、亚磺酰基、卤素原子、及硫原子中的1种以上;
R101d与R101e、R101d与R101e与R101f也可和它们所键结的氮原子一起形成环,形成环时,R101d与R101e及R101d与R101e与R101f为碳数3~10的亚烷基、或形成环中具有式中的氮原子的杂芳香族环。
7.根据权利要求1或2所述的生物体电极组成物,更含有粘着性树脂作为(B)成分。
8.根据权利要求7所述的生物体电极组成物,其中,该(B)成分选自聚硅氧树脂、(甲基)丙烯酸酯树脂、氨基甲酸酯树脂中的1种以上。
9.根据权利要求7所述的生物体电极组成物,其中,该(B)成分含有具烯基的二有机硅氧烷、及具有SiH基的有机氢聚硅氧烷。
10.根据权利要求9所述的生物体电极组成物,其中,该(B)成分更含有具有RxSiO(4-x)/2单元及SiO2单元的聚硅氧树脂,R为碳数1~10的经取代或未经取代的一价烃基,x为2.5~3.5的范围。
11.根据权利要求1或2所述的生物体电极组成物,更含有具有离子性重复单元的高分子化合物作为(C)成分。
12.根据权利要求11所述的生物体电极组成物,其中,该(C)成分的该离子性重复单元含有具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、及银盐的结构的重复单元。
13.根据权利要求1或2所述的生物体电极组成物,更含有碳粉及/或金属粉作为(D)成分。
14.根据权利要求13所述的生物体电极组成物,其中,该碳粉是炭黑及纳米碳管中的任一者或两者。
15.根据权利要求13所述的生物体电极组成物,其中,该金属粉是选自金、银、铂、铜、锡、钛、镍、铝、钨、钼、钌、铬、铟中的金属粉。
16.根据权利要求15所述的生物体电极组成物,其中,该金属粉为银粉。
17.根据权利要求1或2所述的生物体电极组成物,更含有有机溶剂作为(E)成分。
18.一种生物体电极,具有导电性基材及形成在该导电性基材上的生物体接触层,其特征为:该生物体接触层是根据权利要求1至17中任一项所述的生物体电极组成物的硬化物。
19.根据权利要求18所述的生物体电极,其中,该导电性基材含有选自金、银、氯化银、铂、铝、镁、锡、钨、铁、铜、镍、不锈钢、铬、钛、碳、及导电性聚合物中的1种以上。
20.一种生物体电极的制造方法,是具有导电性基材及形成在该导电性基材上的生物体接触层的生物体电极的制造方法,其特征为:在该导电性基材上涂布根据权利要求1至17中任一项所述的生物体电极组成物并使其硬化,以形成该生物体接触层。
21.根据权利要求20所述的生物体电极的制造方法,是使用含有选自金、银、氯化银、铂、铝、镁、锡、钨、铁、铜、镍、不锈钢、铬、钛、碳、及导电性聚合物中的1种以上者作为该导电性基材。
22.一种反应复合体,是具有离子性官能团的单体与碳粒子的反应复合体,其特征为:
该反应复合体是和具有选自氟磺酸、氟磺酰亚胺、及N-羰基氟磺酰胺中的任一的铵盐、锂盐、钠盐、钾盐、银盐的结构的单体键结的碳粒子。
23.根据权利要求22所述的反应复合体,其中,该碳粒子选自炭黑、纳米碳管、石墨、石墨烯。
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