TWI740121B - 生物體電極組成物、生物體電極、以及生物體電極之製造方法 - Google Patents
生物體電極組成物、生物體電極、以及生物體電極之製造方法 Download PDFInfo
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- TWI740121B TWI740121B TW108111460A TW108111460A TWI740121B TW I740121 B TWI740121 B TW I740121B TW 108111460 A TW108111460 A TW 108111460A TW 108111460 A TW108111460 A TW 108111460A TW I740121 B TWI740121 B TW I740121B
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Abstract
本發明之目的為提供可形成導電性及生物相容性優異,輕量,且能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物、使用了該生物體電極組成物而形成有生物體接觸層的生物體電極、及其製造方法。一種生物體電極組成物,含有(A)離子性材料、及(B)該(A)成分以外之樹脂,其特徵為:該(A)成分具有重複單元a及重複單元b兩者,該重複單元a具有氟磺酸、氟磺醯亞胺、及氟磺醯胺當中的任一者之銀鹽之結構,該重複單元b含有矽。
Description
本發明關於能與生物體之皮膚接觸並藉由來自皮膚之電訊號來檢測心搏數等身體狀態的生物體電極、及其製造方法,以及關於可理想地用於生物體電極的生物體電極組成物。
近年,隨著IoT(物聯網(Internet of Things))之普及,穿戴式器件之開發已有進展。能連接到網際網路的鐘錶、眼鏡為其代表例。又,在醫療領域、運動領域方面也需要能隨時監測身體狀態的穿戴式器件,係為今後的成長領域。
在醫療領域方面,例如已有人研究如利用電訊號來感測心臟搏動的心電圖測定那樣藉由感測微弱電流來監測身體臟器之狀態的穿戴式器件。心電圖之測定係將塗有導電糊劑的電極裝設於身體並進行測定,但此為僅1次之短時間之測定。反觀如上述之醫療用之穿戴式器件之開發,係以連續數週隨時監測健康狀態的器件之開發為目標。是以,對於使用於醫療用穿戴式器件的生物體電極,會要求即便長時間使用時也不會有導電性之變化、不會皮膚過敏。此外,也要求輕量、能以低成本製造。
醫療用穿戴式器件有貼附於身體的類型、與納入於衣服之類型,作為貼附於身體的類型,有人提案使用有係為上述導電糊劑之材料的含有水與電解質的水溶性凝膠的生物體電極(專利文獻1)。關於水溶性凝膠,係在用以保持水之水溶性聚合物中含有鈉、鉀、鈣作為電解質,會將來自皮膚之離子濃度之變化轉換成電。另一方面,作為納入於衣服之類型,有人提案將於纖維納入有如PEDOT-PSS(Poly-3,4-ethylenedioxythiophene-Polystyrenesulfonate:聚-3,4-乙烯二氧噻吩-聚苯乙烯磺酸鹽)之導電性聚合物、銀糊劑的布使用於電極之方法(專利文獻2)。
但,使用上述含有水與電解質的水溶性凝膠時,有因乾燥導致水消失時導電性也會消失之問題。另一方面,使用銅等離子化傾向高的金屬時,有對於有些人而言存在引起皮膚過敏之風險之問題,使用如PEDOT-PSS的導電性聚合物時,也有導電性聚合物之酸性強從而存在引起皮膚過敏的風險之問題。
又,金屬奈米線、碳黑、及奈米碳管等具有優異之導電性,故也有人探討將該等作為電極材料使用(專利文獻3、4、5)。金屬奈米線由於線彼此之接觸機率增高,故少的添加量即可通電。但,金屬奈米線為前端尖的纖細材料,故會成為皮膚過敏發生之原因。基於同樣的理由,奈米碳管也有對生物體的刺激性。碳黑雖沒有像奈米碳管那樣的毒性,但仍有些許對皮膚的刺激性。如上所述,即便該物本身不引起過敏反應,有時仍會因材料之形狀、刺激性導致生物相容性惡化,同時兼有導電性與生物相容性係困難。
據認為金屬膜的導電性非常高故可作為優異的生物體電極並發揮功能,但不見得就是那樣。因心臟之搏動而從皮膚釋出的並不是微弱電流,而是鈉離子、鉀離子、鈣離子。因此須將離子之濃度變化轉換成電流,但就不易離子化的貴金屬而言,將來自皮膚之離子轉換成電流之效率不佳。故使用了貴金屬的生物體電極的阻抗高,與皮膚之通電係為高電阻。
另一方面,有人研究添加有離子性液體之電池(專利文獻6)。離子性液體具有熱穩定性、化學穩定性高且導電性優異之特徵,朝電池用途的應用正在擴大。然而,如專利文獻6所示之分子量小的離子性液體會溶於水,若使用添加有該種離子性液體的生物體電極,則離子性液體會被來自皮膚之汗水萃出,故不僅導電性會降低,而且其會滲透到皮膚而造成皮膚粗糙。
又,也有人探討使用了聚合物型磺醯亞胺之鋰鹽的電池(非專利文獻1)。然而,鋰由於離子移動性高,已應用至電池,但它並非生物相容性高的材料。
又,生物體電極若從皮膚脫離則無法取得來自身體之資訊。甚而,即便只是接觸面積發生變化,通電電量也會產生變動,心電圖(電訊號)之基準線(base line)會變動。是以,為了從身體取得穩定的電訊號,必須使生物體電極一直與皮膚接觸,也必須使其接觸面積不發生變化。為此,生物體電極宜具有黏著性。而且,也需要能追隨皮膚之伸縮、彎曲變化的伸縮性、可撓性。
[先前技術文獻]
[專利文獻]
[專利文獻1]國際公開第WO2013-039151號小冊
[專利文獻2]日本特開2015-100673號公報
[專利文獻3]日本特開平5-095924號公報
[專利文獻4]日本特開2003-225217號公報
[專利文獻5]日本特開2015-019806號公報
[專利文獻6]日本特表2004-527902公報
[非專利文獻]
[非專利文獻1]J.Mater.Chem.A,2016,4,p10038-10069
[發明所欲解決之課題]
本發明係為了解決上述問題而成,目的為提供可形成導電性及生物相容性優異,輕量,且能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物、使用了該生物體電極組成物而形成有生物體接觸層的生物體電極、及其製造方法。
[解決課題之手段]
為了解決上述課題,本發明提供
一種生物體電極組成物,含有:
(A)離子性材料,及
(B)該(A)成分以外之樹脂,
該(A)成分具有重複單元a及重複單元b兩者,該重複單元a具有氟磺酸、氟磺醯亞胺、及氟磺醯胺當中之任一者之銀鹽之結構,該重複單元b含有矽。
若為如此之生物體電極組成物,即為可形成導電性及生物相容性優異,輕量,且能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物。
又,該重複單元a宜具有下列通式(1)-1~(1)-4表示之結構中的任意1個以上;
【化1】
式中,Rf1
、Rf2
為氫原子、甲基、氟原子、三氟甲基、或氧原子,Rf1
為氧原子時,Rf2
亦為氧原子,並與所鍵結之碳原子一起形成羰基;Rf3
、Rf4
為氫原子、氟原子、或三氟甲基,Rf1
~Rf4
中有1個以上之氟原子;Rf5
、Rf6
、Rf7
為氟原子、碳數1~4之直鏈狀、分支狀之烷基,具有至少1個以上之氟原子;m為1~4之整數。
若重複單元a具有如此的結構,則為可形成導電性及生物相容性更加優異,輕量,且能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物。
又,該(A)成分宜含有選自於下列通式(2)表示之重複單元a1~a7中之1種以上作為該重複單元a,並含有下列通式(3)表示之重複單元b1作為該重複單元b;
【化2】
式中,R1
、R3
、R5
、R8
、R10
、R11
、及R13
各自獨立地為氫原子或甲基,R2
、R4
、R6
、R9
、及R12
各自獨立地為單鍵、酯基、或也可具有醚基或酯基中的任一者或它們兩者之碳數1~13之直鏈狀、分支狀、環狀之烴基中之任一者;R7
為碳數1~4之直鏈狀、分支狀之伸烷基,R7
中的氫原子當中,也可有1個或2個被取代為氟原子;X1
、X2
、X3
、X4
、及X6
各自獨立地為單鍵、伸苯基、伸萘基、醚基、酯基、醯胺基中之任一者,X5
為單鍵、醚基、酯基中之任一者,X7
為單鍵、碳數6~12之伸芳基、或-C(=O)-O-X10
-,X10
為碳數1~12之直鏈狀、分支狀、環狀之伸烷基、或碳數6~10之2價芳香族烴基,X10
中也可含有醚基、羰基、酯基;Y為氧原子、-NR19
-基,R19
為氫原子、碳數1~4之直鏈狀、分支狀之烷基,Y與R4
也可鍵結並形成環;Rf5
、Rf6
、Rf7
為氟原子、碳數1~4之直鏈狀、分支狀之烷基,具有至少1個以上之氟原子;m為1~4之整數,a1、a2、a3、a4、a5、a6、及a7為滿足0≦a1>1.0,0≦a2>1.0,0≦a3>1.0,0≦a4>1.0,0≦a5>1.0,0≦a6>1.0,0≦a7>1.0,0>a1+a2+a3+a4+a5+a6+a7>1.0之數;
【化3】
式中,R14
為氫原子或甲基,X8
為碳數6~12之伸芳基、-C(=O)-O-R18
-基、及-C(=O)-NH-R18
-基中之任一者;R18
為單鍵、碳數2~12之直鏈狀、分支狀、或環狀之伸烷基、及伸苯基中之任一者,也可具有選自於醚基、羰基、酯基、及醯胺基中之1種以上;R15
、R16
、R17
為碳數1~21之直鏈狀、分支狀、或環狀之烷基,或為碳數6~10之芳基,也可具有選自於矽氧烷鍵、矽原子、及鹵素原子中之1種以上;R15
與R16
、R15
與R16
與R17
也可鍵結並形成環或三維結構;b1為滿足0>b1>1.0之數。
若為如此之(A)成分,則可使本發明之效果進一步改善。
又,該(A)成分除了具有該重複單元a、b之外,還具有下列通式(4)表示之重複單元c為較佳;
【化4】
式中,R20
為氫原子或甲基,X9
為單鍵、伸苯基、伸萘基、醚基、酯基、具有酯基之伸苯基、及醯胺基中之任一者,R21
為碳數1~40之直鏈狀、分支狀、環狀之烷基、碳數2~40之直鏈狀、分支狀、環狀之烯基、碳數2~40之直鏈狀、分支狀、環狀之炔基、碳數6~20之芳基,也可具有醚基、酯基、羥基;c為滿足0>c>1.0之數。
若含有如此之重複單元c,則為黏著性更高的生物體電極組成物。
又,該(B)成分宜含有具有Rx
SiO(4-x)/2
單元及SiO2
單元之聚矽氧樹脂、具有烯基之二有機基矽氧烷、及具有SiH基之有機基氫聚矽氧烷;R為碳數1~10之經取代或未經取代之一價烴基,x為2.5~3.5之範圍。
若為如此之(B)成分,則可更確實地防止鹽之溶出,保持碳材等導電性改善劑,並展現黏著性。
又,該生物體電極組成物宜更含有有機溶劑。
若為如此之生物體電極組成物,則生物體電極組成物之塗佈性會更加良好。
又,該生物體電極組成物宜更含有碳材料。
若為如此之生物體電極組成物,則可形成導電性更加良好的生物體接觸層。
此時,該碳材料宜為碳黑及奈米碳管中之任一者或兩者。
在本發明之生物體電極組成物中,可特別理想地使用如此之碳材料。
又,本發明提供一種生物體電極,具有導電性基材及形成於該導電性基材上的生物體接觸層,該生物體接觸層為上述生物體電極組成物之硬化物。
若為如此之生物體電極,即為導電性及生物相容性優異,輕量,且能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的使用了生物體電極組成物而形成有生物體接觸層之生物體電極。
此時,該導電性基材宜為包含選自於金、銀、氯化銀、鉑、鋁、鎂、錫、鎢、鐵、銅、鎳、不銹鋼、鉻、鈦、及碳中之1種以上者。
在本發明之生物體電極中,可特別理想地使用如此之導電性基材。
又,本發明提供一種生物體電極之製造方法,係具有導電性基材及形成於該導電性基材上的生物體接觸層之生物體電極之製造方法,其特徵為:藉由在該導電性基材上塗佈上述之生物體電極組成物並使其硬化,從而形成該生物體接觸層。
若為如此之製造方法,則能以低成本輕易地製造形成有導電性及生物相容性優異,輕量,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體接觸層的生物體電極。
此時,宜使用包含選自於金、銀、氯化銀、鉑、鋁、鎂、錫、鎢、鐵、銅、鎳、不銹鋼、鉻、鈦、及碳中之1種以上者作為該導電性基材。
在本發明之生物體電極之製造方法中,可特別理想地使用如此之導電性基材。
[發明之效果]
如上所述,若為本發明之生物體電極組成物,即為可形成能將來自皮膚的電訊號有效率地傳送至器件(亦即,導電性優異),即便長時間裝設於皮膚也無引起過敏之疑慮(亦即,生物相容性優異),輕量,能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物。又,可藉由添加碳材料以進一步改善導電性,可藉由和具有黏著性與伸縮性的樹脂組合以製造特別高黏著力且伸縮性高的生物體電極。再者,可藉由添加劑等來改善對皮膚之伸縮性、黏著性,也可藉由適當地調節樹脂之組成、生物體接觸層之厚度來調整伸縮性、黏著性。是以,若為使用了如此的本發明之生物體電極組成物而形成有生物體接觸層的本發明之生物體電極,則作為醫療用穿戴式器件所使用的生物體電極特別理想。又,若為本發明之生物體電極之製造方法,則能以低成本輕易地製造如此之生物體電極。
如上述,需要開發可形成導電性及生物相容性優異,輕量,且能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物、使用了該生物體電極組成物而形成有生物體接觸層的生物體電極、及其製造方法。
本案發明人等著眼離子性液體以作為用以形成生物體電極用之生物體接觸層之生物體電極組成物中所摻合之離子性材料(導電性材料)。離子性液體具有熱穩定性、化學穩定性高,且導電性優異之特徵,朝電池用途之應用正在擴大。又,離子性液體已知有鋶、鏻、銨、啉鎓、吡啶鎓、吡咯啶鎓、咪唑鎓之鹽酸鹽、溴酸鹽、碘酸鹽、三氟甲烷磺酸鹽、九氟丁烷磺酸鹽、雙(三氟甲烷磺醯基)醯亞胺酸鹽、六氟磷酸鹽、四氟硼酸鹽等。然而,一般而言該等鹽(尤其分子量小者)的水合性高,故使用了添加有該等鹽的生物體電極組成物而形成有生物體接觸層的生物體電極,有因汗水、洗滌導致鹽被萃出,導電性降低之缺點。又,四氟硼酸鹽係毒性高,其它鹽則是水溶性高,故有容易滲透至皮膚中並造成皮膚粗糙(亦即對皮膚的刺激性強)之問題。
若形成中和鹽的酸的酸性度高,則離子係強極化,離子導電性會提升。就鋰離子電池而言,雙(三氟甲烷磺醯基)醯亞胺酸、參(三氟甲烷磺醯基)甲基化酸之鋰鹽會展現高的離子導電性就是這個緣故。另一方面,有酸強度越高則該鹽的生物體刺激性越強之問題。亦即,離子導電性與生物體刺激性係為取捨關係。但,使用於生物體電極的鹽須兼有高離子導電特性與低生物體刺激性。
於是,本案發明人等針對上述課題努力進行研究,發現具有選自於氟磺酸、氟磺醯亞胺、氟磺醯胺中之銀鹽之重複單元之高分子化合物係高離子導電性,且沒有對皮膚之滲透性從而沒有對皮膚之刺激性,故藉由使用將該高分子化合物與含有矽之單體進行共聚合並將其與例如聚矽氧系、丙烯酸系、胺甲酸酯系之黏著劑(樹脂)混合而得之物來形成生物體接觸層,會製成不僅能兼有導電性及生物相容性,被水沾濕或予以乾燥時導電性也不會大幅降低,而且能一直與皮膚密合並獲得長時間穩定的電訊號的生物體電極並發揮功能,乃完成本發明。
亦即,本發明為一種生物體電極組成物,含有:
(A)離子性材料,及
(B)該(A)成分以外之樹脂,
該(A)成分具有重複單元a及重複單元b兩者,該重複單元a具有氟磺酸、氟磺醯亞胺、及氟磺醯胺當中之任一者之銀鹽之結構,該重複單元b含有矽。
以下,針對本發明進行詳細說明,但本發明不限於該等。
>生物體電極組成物>
本發明之生物體電極組成物含有(A)離子性材料及(B)(A)成分以外之樹脂。以下,針對各成分進一步詳細說明。
[(A)離子性材料(鹽)]
作為(A)離子性材料而摻合於本發明之生物體電極組成物中的聚合物型之鹽所含有的具有氟磺酸、氟磺醯亞胺、氟磺醯胺當中之任一者之銀鹽之結構的重複單元a,宜具有下列通式(1)-1~(1)-4表示之結構中之任意1個以上。
【化5】
(式中,Rf1
、Rf2
為氫原子、甲基、氟原子、三氟甲基、或氧原子,Rf1
為氧原子時,Rf2
亦為氧原子,並與所鍵結之碳原子一起形成羰基。Rf3
、Rf4
為氫原子、氟原子、或三氟甲基,Rf1
~Rf4
中有1個以上之氟原子。Rf5
、Rf6
、Rf7
為氟原子、碳數1~4之直鏈狀、分支狀之烷基,具有至少1個以上之氟原子。m為1~4之整數。)
(重複單元a)
本發明之生物體電極組成物之(A)成分,宜含有選自於下列通式(2)表示之重複單元a1~a7中之1種以上。
【化6】
(式中,R1
、R3
、R5
、R8
、R10
、R11
、及R13
各自獨立地為氫原子或甲基,R2
、R4
、R6
、R9
、及R12
各自獨立地為單鍵、酯基、或也可具有醚基或酯基中的任一者或它們兩者之碳數1~13之直鏈狀、分支狀、環狀之烴基中之任一者。R7
為碳數1~4之直鏈狀、分支狀之伸烷基,R7
中的氫原子當中,也可有1個或2個被取代為氟原子。X1
、X2
、X3
、X4
、及X6
各自獨立地為單鍵、伸苯基、伸萘基、醚基、酯基、醯胺基中之任一者,X5
為單鍵、醚基、酯基中之任一者,X7
為單鍵、碳數6~12之伸芳基、或-C(=O)-O-X10
-,X10
為碳數1~12之直鏈狀、分支狀、環狀之伸烷基、或碳數6~10之2價芳香族烴基,X10
中也可含有醚基、羰基、酯基。Y為氧原子、-NR19
-基,R19
為氫原子、碳數1~4之直鏈狀、分支狀之烷基,Y與R4
也可鍵結並形成環。Rf5
、Rf6
、Rf7
為氟原子、碳數1~4之直鏈狀、分支狀之烷基,具有至少1個以上之氟原子。m為1~4之整數。a1、a2、a3、a4、a5、a6、及a7為滿足0≦a1>1.0,0≦a2>1.0,0≦a3>1.0,0≦a4>1.0,0≦a5>1.0,0≦a6>1.0,0≦a7>1.0,0>a1+a2+a3+a4+a5+a6+a7>1.0之數。)
用以獲得上述通式(2)表示之重複單元a1~a7當中的重複單元a1~a5的氟磺酸鹽單體,具體可例示下列者。
用以獲得上述通式重複單元a6之磺醯亞胺鹽單體,具體可例示如下。
就用以獲得上述通式(2)表示之重複單元a1~a7之銀鹽單體的合成方法而言,例如可列舉藉由在有機溶劑中將由上述之氟磺酸陰離子或氟醯亞胺酸陰離子或氟醯胺酸陰離子與銨陽離子構成之銨鹽與氯化銀進行混合而獲得之方法。此時,宜將副產物即所生成的氯化銨利用水洗予以去除。
(重複單元b)
本發明之生物體電極組成物之(A)成分除了具有上述重複單元a以外,還具有含有矽之重複單元b。
重複單元b宜包含下列通式(3)表示之重複單元b1。用以獲得通式(3)中的重複單元b1之單體係下列通式(5)表示者。
【化35】
(式中,R14
為氫原子或甲基,X8
為碳數6~12之伸芳基、-C(=O)-O-R18
-基、及-C(=O)-NH-R18
-基中之任一者。R18
為單鍵、碳數2~12之直鏈狀、分支狀、或環狀之伸烷基、及伸苯基中之任一者,也可具有選自於醚基、羰基、酯基、及醯胺基中之1種以上。R15
、R16
、R17
為碳數1~21之直鏈狀、分支狀、或環狀之烷基,或為碳數6~10之芳基,也可具有選自於矽氧烷鍵、矽原子、及鹵素原子中之1種以上。R15
與R16
、R15
與R16
與R17
也可鍵結並形成環或三維結構。b1為滿足0>b1>1.0之數。)
上述通式(5)表示之單體,具體可例示下列者。
(重複單元c)
本發明之生物體電極組成物之(A)成分中,除了具有上述重複單元a、b以外,尚可共聚合下列通式(4)記載之具有烷基之重複單元c。
【化38】
(式中,R20
為氫原子或甲基,X9
為單鍵、伸苯基、伸萘基、醚基、酯基、具有酯基之伸苯基、及醯胺基中之任一者,R21
為碳數1~40之直鏈狀、分支狀、環狀之烷基、碳數2~40之直鏈狀、分支狀、環狀之烯基、碳數2~40之直鏈狀、分支狀、環狀之炔基、碳數6~20之芳基,也可具有醚基、酯基、羥基。c為滿足0>c>1.0之數。)
用以獲得重複單元c之單體,具體可例示下列者。
本發明之生物體電極組成物之(A)成分中,也可進一步共聚合交聯性之單體。就用以獲得交聯性之重複單元d之單體而言,其特徵為具有羥基、羧基、氧雜環丙烷基、氧雜環丁烷基,具體可例示如下。
也可共聚合具有多個聚合性雙鍵的單體e。藉此可在聚合後進行聚合物間之交聯。具有多個雙鍵的單體e具體可例示如下。
作為合成(A)成分之高分子化合物(離子性材料)的方法之一,可列舉將提供重複單元a1~a7、b、c、d、e之單體當中所期望之單體在有機溶劑中加入自由基聚合起始劑並進行加熱聚合,而獲得共聚物之高分子化合物之方法。
就聚合時使用的有機溶劑而言,可例示甲苯、苯、四氫呋喃、二乙醚、二㗁烷等。就聚合起始劑而言,可例示2,2’-偶氮雙異丁腈(AIBN)、2,2’-偶氮雙(2,4-二甲基戊腈)、2,2-偶氮雙(2-甲基丙酸)二甲酯、過氧化苯甲醯、過氧化月桂醯等。加熱溫度宜為50~80℃,反應時間宜為2~100小時,更佳為5~20小時。
在此,就重複單元a1~a7、b、c、d、e之比例而言,為0≦a1>1.0,0≦a2>1.0,0≦a3>1.0,0≦a4>1.0,0≦a5>1.0,0≦a6>1.0,0≦a7>1.0,0>a1+a2+a3+a4+a5+a6+a7>1.0,0>b>1.0,0≦c>1.0,0≦d>1.0,0≦e>1.0,較佳為0≦a1≦0.9,0≦a2≦0.9,0≦a3≦0.9,0≦a4≦0.9,0≦a5≦0.9,0≦a6≦0.9,0≦a7≦0.9,0.1≦a1+a2+a3+a4+a5+a6+a7≦0.9,0.1≦b≦0.9,0≦c≦0.6,0≦d≦0.6,0≦e≦0.6,更佳為0≦a1≦0.8,0≦a2≦0.8,0≦a3≦0.8,0≦a4≦0.8,0≦a5≦0.8,0≦a6≦0.8,0≦a7≦0.8,0.2≦a1+a2+a3+a4+a5+a6+a7≦0.8,0.15≦b≦0.8,0≦c≦0.5,0≦d≦0.5,0≦e≦0.5。
另外,例如a1+a2+a3+a4+a5+a6+a7+b+c+d+e=1表示在含有重複單元a1、a2、a3、a4、a5、a6、a7、b、c、d、e之高分子化合物中,重複單元a1、a2、a3、a4、a5、a6、a7、b、c、d、e之合計量相對於全部重複單元之合計量為100莫耳%;a1+a2+a3+a4+a5+a6+a7+b+c+d+e>1表示重複單元a1、a2、a3、a4、a5、a6、a7、b、c、d、e之合計量相對於全部重複單元之合計量未達100莫耳%,除了a1、a2、a3、a4、a5、a6、a7、b、c、d、e以外尚具有其它重複單元。
(A)成分之分子量以重量平均分子量計宜為500以上,更佳為1,000以上、1,000,000以下,又更佳為2,000以上、500,000以下。又,聚合後未納入(A)成分的離子性單體(殘存單體)為少量的話,則無在生物相容試驗中殘存單體滲入至皮膚而引起過敏之疑慮,故宜減少殘存單體的量。殘存單體的量相對於(A)成分全體100質量份宜為10質量份以下。
本發明之生物體電極組成物中,(A)成分之摻合量相對於(B)成分100質量份宜設為0.1~300質量份,設為1~200質量份更佳。又,針對(A)成分可單獨使用1種,也可混用2種以上。
[(B)(A)成分以外之樹脂]
摻合於本發明之生物體電極組成物中的(B)成分,係用以和上述(A)離子性材料(鹽)相容而防止鹽之溶出,保持碳材等導電性改善劑,並使黏著性顯現之成分。另外,(B)成分只要為上述(A)成分以外之樹脂即可,宜為熱硬化性樹脂及光硬化性樹脂中之任一者,或它們兩者,為選自於聚矽氧系、丙烯酸系、及胺甲酸酯系之樹脂中之1種以上尤佳。
就黏著性之聚矽氧系之樹脂而言,可列舉加成反應硬化型或自由基交聯反應硬化型之樹脂。就加成反應硬化型而言,例如可使用日本特開2015-193803號公報記載之含有具有烯基之二有機基矽氧烷、具有R3
SiO0.5
及SiO2
單元之MQ樹脂、具有多個SiH基之有機基氫聚矽氧烷、鉑觸媒、加成反應控制劑、及有機溶劑者。又,就自由基交聯反應硬化型而言,例如可使用日本特開2015-193803號公報記載之含有可具有或不具有烯基之二有機基聚矽氧烷、具有R3
SiO0.5
及SiO2
單元之MQ樹脂、有機過氧化物、及有機溶劑者。在此R為碳數1~10之經取代或未經取代之一價烴基。
又,也可使用使聚合物末端、側鏈具有矽醇基的聚矽氧烷、與MQ樹脂進行縮合反應而形成之聚矽氧烷・樹脂一體型化合物。MQ樹脂由於含有許多矽醇基故藉由添加此樹脂會改善黏著力,但因無交聯性故並未與聚矽氧烷分子層級地鍵結。可藉由如上述使聚矽氧烷與樹脂成為一體型以增大黏著力。
又,聚矽氧系之樹脂中也可添加具有選自於胺基、氧雜環丙烷基、氧雜環丁烷基、聚醚基、羥基、羧基、巰基、甲基丙烯酸基、丙烯酸基、苯酚基、矽醇基、羧酸酐基、芳基、芳烷基、醯胺基、酯基、內酯環中之基之改性矽氧烷。藉由添加改性矽氧烷會改善(A)成分在聚矽氧樹脂中的分散性。改性矽氧烷可使用矽氧烷之單側末端、兩側末端、側鏈中之任一經改性者。
就黏著性之丙烯酸系之樹脂而言,例如可使用日本特開2016-011338號公報記載之具有親水性(甲基)丙烯酸酯、長鏈疏水性(甲基)丙烯酸酯作為重複單元者。因應情況也可共聚合具有官能基之(甲基)丙烯酸酯、具有矽氧烷鍵之(甲基)丙烯酸酯。
就黏著性之胺甲酸酯系之樹脂而言,例如可使用日本特開2016-065238號公報記載之具有胺甲酸酯鍵、與聚醚、聚酯鍵、聚碳酸酯鍵、矽氧烷鍵者。
又,為了防止(A)成分從生物體接觸層溶出所導致之導電性的降低,在本發明之生物體電極組成物中,(B)成分宜為和上述(A)成分之相容性高者。又,為了防止生物體接觸層從導電性基材剝離,在本發明之生物體電極組成物中,(B)成分宜為對導電性基材之黏接性高者。為了使(B)成分成為和導電性基材、鹽之相容性高者,使用極性高的樹脂係有效。如此的樹脂可列舉具有選自於醚鍵、酯鍵、醯胺鍵、醯亞胺鍵、胺甲酸酯鍵、硫代胺甲酸酯鍵、及硫醇基中之1個以上之樹脂、或聚丙烯酸樹脂、聚醯胺樹脂、聚醯亞胺樹脂、聚胺甲酸酯樹脂、及聚硫代胺甲酸酯樹脂等。又,另一方面,生物體接觸層會與生物體接觸,故容易受到來自生物體的汗水之影響。是以,本發明之生物體電極組成物中,(B)成分宜為撥水性高且不易水解者。為了使樹脂成為撥水性高且不易水解者,使用含有矽之樹脂係有效。
就含有矽原子之聚丙烯酸樹脂而言,有在主鏈具有聚矽氧之聚合物與在側鏈具有矽原子之聚合物,皆可適用。就在主鏈具有聚矽氧之聚合物而言,可使用具有(甲基)丙烯酸丙酯基之矽氧烷或矽倍半氧烷等。此時,可藉由添加光自由基產生劑來使(甲基)丙烯酸部分進行聚合而使樹脂硬化。
就含有矽原子之聚醯胺樹脂而言,例如可適用日本特開2011-079946號公報、美國專利5981680號公報記載之聚醯胺聚矽氧樹脂等。如此的聚醯胺聚矽氧樹脂例如可將兩側末端具有胺基之聚矽氧或兩側末端具有胺基之非聚矽氧化合物,與兩側末端具有羧基之非聚矽氧或兩側末端具有羧基之聚矽氧予以組合並進行合成。
又,也可使用使羧酸酐與胺進行反應而得之環化前之聚醯胺酸。於進行聚醯胺酸之羧基之交聯時,可使用環氧系、氧雜環丁烷系之交聯劑,也可實施羧基與(甲基)丙烯酸羥乙酯之酯化反應後進行(甲基)丙烯酸酯部分之光自由基交聯。
就含有矽原子之聚醯亞胺樹脂而言,例如可適用日本特開2002-332305號公報記載之聚醯亞胺聚矽氧樹脂等。聚醯亞胺樹脂的黏性非常高,可藉由摻合(甲基)丙烯酸系單體作為溶劑及交聯劑以調整成低黏性。
就含有矽原子之聚胺甲酸酯樹脂而言,可列舉聚胺甲酸酯聚矽氧樹脂,如此的聚胺甲酸酯聚矽氧樹脂可藉由將兩側末端具有異氰酸酯基之化合物與末端具有羥基之化合物予以混摻並加熱以實施利用胺甲酸酯鍵所為之交聯。另外,此時兩側末端具有異氰酸酯基之化合物、或末端具有羥基之化合物中之任一者或兩者必須含有矽原子(矽氧烷鍵)。或也可如日本特開2005-320418號公報所記載,在聚矽氧烷中混摻胺甲酸酯(甲基)丙烯酸酯單體並使其光交聯。也可使具有矽氧烷鍵與胺甲酸酯鍵兩者且末端具有(甲基)丙烯酸酯基之聚合物進行光交聯。
就含有矽原子之聚硫代胺甲酸酯樹脂而言,可藉由具有硫醇基之化合物與具有異氰酸酯基之化合物之反應獲得,只要它們之中任一者含有矽原子即可。又,若末端具有(甲基)丙烯酸酯基,也能使其光硬化。
聚矽氧系之樹脂中,除了含有上述具有烯基之二有機基矽氧烷、具有R3
SiO0.5
及SiO2
單元之MQ樹脂、具有多個SiH基之有機基氫聚矽氧烷以外,還添加具有選自於胺基、氧雜環丙烷基、氧雜環丁烷基、聚醚基、羥基、羧基、巰基、甲基丙烯酸基、丙烯酸基、苯酚基、矽醇基、羧酸酐基、芳基、芳烷基、醯胺基、酯基、內酯環中的基的改性矽氧烷的話,則和上述鹽的相容性會提高。
另外,如後述,生物體接觸層為生物體電極組成物之硬化物。藉由使其硬化,生物體接觸層對皮膚及導電性基材兩者的黏接性會變得良好。另外,硬化方法並不特別限定,可使用一般的方法,例如可使用利用熱及光中之任一者或其兩者、或酸或鹼觸媒所為之交聯反應等。針對交聯反應,例如可適當選擇交聯反應手冊 中山雍晴 丸善出版(2013年)第二章p51~p371所記載之方法來實施。
具有烯基之二有機基矽氧烷與具有多個SiH基之有機基氫聚矽氧烷可藉由利用鉑觸媒所為之加成反應使其交聯。
就鉑觸媒而言可列舉:氯鉑酸、氯鉑酸之醇溶液、氯鉑酸和醇之反應產物、氯鉑酸和烯烴化合物之反應產物、氯鉑酸和含有乙烯基之矽氧烷之反應產物、鉑-烯烴錯合物、鉑-含有乙烯基之矽氧烷錯合物等鉑系觸媒;銠錯合物及釕錯合物等鉑族金屬系觸媒等。也可使用將該等觸媒溶解、分散於醇系、烴系、矽氧烷系溶劑而得者。
另外,鉑觸媒之添加量相對於樹脂100質量份宜為5~2,000ppm,尤其是設定為10~500ppm之範圍較理想。
又,使用加成硬化型之聚矽氧樹脂時,也可添加加成反應控制劑。此加成反應控制劑係作為用來在溶液中及在塗膜形成後加熱硬化前的低溫環境下使鉑觸媒不會作用之淬滅劑而予以添加。具體而言可列舉: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-乙炔基環己醇、3-甲基-3-三甲基矽氧基-1-丁炔、3-甲基-3-三甲基矽氧基-1-戊炔、3,5-二甲基-3-三甲基矽氧基-1-己炔、1-乙炔基-1-三甲基矽氧基環己烷、雙(2,2-二甲基-3-丁炔氧基)二甲基矽烷、1,3,5,7-四甲基-1,3,5,7-四乙烯基環四矽氧烷、1,1,3,3-四甲基-1,3-二乙烯基二矽氧烷等。
加成反應控制劑之添加量相對於樹脂100質量份宜為0~10質量份,尤其是設定為0.05~3質量份之範圍較理想。
就實施光硬化之方法而言可列舉:使用具有(甲基)丙烯酸酯末端、烯烴末端之樹脂、或添加末端為(甲基)丙烯酸酯、烯烴、或硫醇基之交聯劑,並同時添加利用光以使自由基產生之光自由基產生劑之方法;使用具有氧雜環丙烷基、氧雜環丁烷基、乙烯基醚基之樹脂、交聯劑,並添加利用光以使酸產生之光酸產生劑之方法。
就光自由基產生劑而言可列舉:苯乙酮、4,4’-二甲氧基二苯基乙二酮、二苯基乙二酮、苯偶姻、二苯甲酮、2-苯甲醯基苯甲酸、4,4’-雙(二甲基胺基)二苯甲酮、4,4’-雙(二乙基胺基)二苯甲酮、苯偶姻甲醚、苯偶姻乙醚、苯偶姻異丙醚、苯偶姻丁醚、苯偶姻異丁醚、4-苯甲醯基苯甲酸、2,2’-雙(2-氯苯基)-4,4’,5,5’-四苯基-1,2’-聯咪唑、2-苯甲醯基苯甲酸甲酯、2-(1,3-苯并二氧雜環戊烯-5-基)-4,6-雙(三氯甲基)-1,3,5-三、2-苄基-2-(二甲基胺基)-4’-啉代苯丁酮、4,4’-二氯二苯甲酮、2,2-二乙氧基苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、2,4-二乙基噻噸-9-酮、二苯基(2,4,6-三甲基苯甲醯基)氧化膦(BAPO)、1,4-二苯甲醯基苯、2-乙基蒽醌、1-羥基環己基苯基酮、2-羥基-2-甲基苯丙酮、2-羥基-4’-(2-羥基乙氧基)-2-甲基苯丙酮、2-異亞硝基苯丙酮、2-苯基-2-(對甲苯磺醯氧基)苯乙酮。
也可藉由添加熱分解型之自由基產生劑以使其硬化。熱自由基產生劑可列舉:2,2’-偶氮雙(異丁腈)、2,2’-偶氮雙(2,4-二甲基戊腈)、2,2’-偶氮雙(2-甲基丁腈)、4,4’-偶氮雙(4-氰基戊酸)、2,2’-偶氮雙(甲基丙脒)鹽酸、2,2’-偶氮雙[2-(2-咪唑啉-2-基)丙烷]鹽酸、2,2’-偶氮雙(4-甲氧基-2,4-二甲基戊腈)、2,2’-偶氮雙(環己烷-1-甲腈)、1[(1-氰基-1-甲基乙基)偶氮]甲醯胺、2,2’-偶氮雙[2-甲基-N-(2-羥基乙基)丙醯胺]、2,2’-偶氮雙[N-(2-丙烯基)-2-甲基丙醯胺]、2,2’-偶氮雙(N-丁基-2-甲基丙醯胺)、2,2’-偶氮雙(異丁酸)二甲酯、4,4’-偶氮雙(4-氰基戊酸)、2,2’-偶氮雙(2-甲基丙酸)二甲酯、過氧化苯甲醯、第三丁基過氧化氫、過氧化氫異丙苯、二(第三丁基)過氧化物、二(第三戊基)過氧化物、二(正丁基)過氧化物、2,2’-偶氮雙(2-甲基丙酸)二甲酯、過氧化二異丙苯等。
就光酸產生劑而言可列舉:鋶鹽、錪鹽、磺醯基重氮甲烷、N-磺醯氧基醯亞胺、肟-O-磺酸酯型酸產生劑等。光酸產生劑之具體例,例如可列舉日本特開2008-111103號公報之段落[0122]~[0142]、日本特開2009-080474號公報所記載者。
另外,自由基產生劑、光酸產生劑之添加量相對於樹脂100質量份宜設定為0.1~50質量份之範圍。
它們之中,就(B)成分之樹脂而言,含有具有Rx
SiO(4-x)/2
單元(R為碳數1~10之經取代或未經取代之一價烴基,x為2.5~3.5之範圍。)及SiO2
單元之聚矽氧樹脂、具有烯基之二有機基矽氧烷、以及具有SiH基之有機基氫聚矽氧烷者特佳。
[黏著性賦予劑]
又,本發明之生物體電極組成物中,為了賦予對於生物體之黏著性,也可添加黏著性賦予劑。如此的黏著性賦予劑例如可列舉:聚矽氧樹脂、非交聯性之矽氧烷、非交聯性之聚(甲基)丙烯酸酯、非交聯性之聚醚等。
[有機溶劑]
又,本發明之生物體電極組成物中可添加有機溶劑。作為有機溶劑具體可列舉:甲苯、二甲苯、異丙苯、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、丁苯、第二丁苯、異丁苯、異丙基甲苯、二乙基苯、2-乙基對二甲苯、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、四氫萘、4-苯基-1-丁烯、第三戊基苯、戊基苯、2-第三丁基甲苯、3-第三丁基甲苯、4-第三丁基甲苯、5-異丙基間二甲苯、3-甲基乙基苯、第三丁基-3-乙基苯、4-第三丁基鄰二甲苯、5-第三丁基間二甲苯、第三丁基對二甲苯、1,2-二異丙基苯、1,3-二異丙基苯、1,4-二異丙基苯、二丙基苯、3,9-十二碳二炔、五甲基苯、六甲基苯、己基苯、1,3,5-三乙基苯等芳香族系烴系溶劑;正庚烷、異庚烷、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、二環戊二烯、1-甲基-1,4-環己二烯、1-庚炔、2-庚炔、環庚烷、環庚烯、1,3-二甲基環戊烷、乙基環戊烷、甲基環己烷、1-甲基-1-環己烯、3-甲基-1-環己烯、亞甲基環己烷、4-甲基-1-環己烯、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、環辛烷、環辛烯、1,2-二甲基環己烷、1,3-二甲基環己烷、1,4-二甲基環己烷、乙基環己烷、乙烯基環己烷、異丙基環戊烷、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-甲基環己烷、1-乙基-3-甲基環己烷、1-乙基-4-甲基環己烷、丙基環己烷、異丙基環己烷、1,1,3-三甲基環己烷、1,1,4-三甲基環己烷、1,2,3-三甲基環己烷、1,2,4-三甲基環己烷、1,3,5-三甲基環己烷、烯丙基環己烷、八氫茚(hydrindane)、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、第三丁基環己烷、丁基環己烷、異丁基環己烷、4-異丙基-1-甲基環己烷、戊基環戊烷、1,1,3,5-四甲基環己烷、環十二烷、1-癸烯、2-癸烯、3-癸烯、4-癸烯、5-癸烯、1,9-癸二烯、十氫萘、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、檸檬烯、香葉烯(myrcene)、1,2,3,4,5-五甲基環戊二烯、α-水芹烯(α-phellandrene)、蒎烯、萜品烯(terpinene)、四氫二環戊二烯、5,6-二氫二環戊二烯、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、戊基環己烷、1-十一烯、1,10-十一碳二烯、1-十一炔、3-十一炔、5-十一炔、三環[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、1,3-二甲基金剛烷、1-乙基金剛烷、1,5,9-環十二碳三烯、1,2,4-三乙烯基環己烷、異鏈烷烴(isoparaffin)等脂肪族烴系溶劑;環己酮、環戊酮、2-辛酮、2-壬酮、2-庚酮、3-庚酮、4-庚酮、2-己酮、3-己酮、二異丁酮、甲基環己酮、甲基正戊酮等酮系溶劑;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-丙醇等醇系溶劑;丙二醇單甲醚、乙二醇單甲醚、丙二醇單乙醚、乙二醇單乙醚、丙二醇二甲醚、二乙二醇二甲醚、二異丙醚、二異丁醚、二異戊醚、二正戊醚、甲基環戊醚、甲基環己醚、二正丁醚、二第二丁醚、二第二戊醚、二第三戊醚、二正己醚、苯甲醚等醚系溶劑;丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、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、乙酸第三丁酯、丙酸第三丁酯、丙二醇單第三丁醚乙酸酯等酯系溶劑;γ-丁內酯等內酯系溶劑等。
另外,有機溶劑之添加量相對於樹脂100質量份宜設定為10~50,000質量份之範圍。
[碳材料]
本發明之生物體電極組成物中,為了進一步提高導電性,可添加碳材料作為導電性改善劑。就碳材料而言可列舉碳黑、奈米碳管、碳纖維等。奈米碳管可為單層、多層中之任一者,表面經有機基修飾亦無妨。碳材料之添加量相對於樹脂100質量份宜設定為1~50質量份之範圍。
[碳材料以外的導電性改善劑]
又,本發明之生物體電極組成物中也可添加碳材料以外的導電性改善劑。具體而言可列舉:以金、銀、鉑等貴金屬塗覆樹脂而得之粒子、纖維、奈米線、或金、銀、鉑等之奈米粒子、氧化銦錫(ITO)、氧化銦鋅(IZO)、氧化錫、氧化鋅等金屬氧化物之粒子等。
如上所述,若為本發明之生物體電極組成物,即為可形成能將來自皮膚的電訊號有效率地傳送至器件(亦即,導電性優異),即便長時間裝設於皮膚也無引起過敏之疑慮(亦即,生物相容性優異),輕量,能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極用之生物體接觸層的生物體電極組成物。又,可藉由添加碳材料以進一步改善導電性,可藉由和具有黏著性與伸縮性的樹脂組合以製造特別高黏著力且伸縮性高的生物體電極。再者,可藉由添加劑等來改善對皮膚的伸縮性、黏著性,也可藉由適當地調節樹脂之組成、生物體接觸層之厚度來調整伸縮性、黏著性。
>生物體電極>
又,本發明提供一種生物體電極,其具有導電性基材及形成於該導電性基材上的生物體接觸層,該生物體接觸層為上述本發明之生物體電極組成物之硬化物。
以下,針對本發明之生物體電極邊參照圖式邊詳細說明,但本發明不限於該等。
圖1係顯示本發明之生物體電極之一例的概略剖面圖。圖1之生物體電極1具有導電性基材2及形成於該導電性基材2上的生物體接觸層3。生物體接觸層3為離子性聚合物(離子性材料)4與碳材料5分散於樹脂6中而成之層。
使用如此的圖1之生物體電極1時,如圖2所示,使生物體接觸層3(亦即,離子性聚合物4與碳材料5分散於樹脂6中而成之層)與生物體7接觸,藉由離子性聚合物4與碳材料5以從生物體7取出電訊號,將此電訊號經由導電性基材2傳導至感測器件等(未圖示)。如上述,若為本發明之生物體電極,可藉由上述離子性聚合物(離子性材料)而兼有導電性及生物相容性,而且視需要可藉由添加碳材料等導電性改善劑以進一步改善導電性,且又因為具有黏著性故與皮膚之接觸面積為一定,可穩定且高感度地取得來自皮膚之電訊號。
以下,針對本發明之生物體電極之各構成材料更詳細說明。
[導電性基材]
本發明之生物體電極具有導電性基材。此導電性基材通常與感測器件等電性連接,將從生物體經由生物體接觸層取出之電訊號傳導至感測器件等。
導電性基材只要為具導電性者即可,不特別限定,例如宜為包含選自於金、銀、氯化銀、鉑、鋁、鎂、錫、鎢、鐵、銅、鎳、不銹鋼、鉻、鈦、及碳中之1種以上者。
又,導電性基材不特別限定,可為硬質的導電性基板等,也可為具可撓性的導電性薄膜、表面塗佈有導電性糊劑之布料、混入有導電性聚合物之布料。導電性基材可為平坦也可有凹凸,也可為編織金屬線而成之網目狀,因應生物體電極之用途等適宜地選擇即可。
[生物體接觸層]
本發明之生物體電極具有形成於導電性基材上之生物體接觸層。此生物體接觸層係在使用生物體電極時實際與生物體接觸之部分,具有導電性及黏著性。生物體接觸層為上述本發明之生物體電極組成物之硬化物,亦即,係為含有上述(A)離子性材料(鹽)及(B)樹脂並視需要更含有碳材料等添加劑之黏著性之樹脂層。
另外,生物體接觸層之黏著力宜為0.5N/25mm以上20N/25mm以下之範圍。就黏著力之測定方法而言,一般採用JIS Z 0237所示之方法,基材可使用如SUS(不銹鋼)之金屬基板、PET(聚對苯二甲酸乙二酯)基板,但也可使用人之皮膚進行測定。人之皮膚之表面能量比金屬、各種塑膠低,係接近於特氟龍(註冊商標)的低能量,係為不易黏著的性質。
生物體電極之生物體接觸層之厚度較佳為1μm以上5mm以下,更佳為2μm以上3mm以下。生物體接觸層越薄黏著力越低,但可撓性越提升,越輕量,對於皮膚之順應性越佳。可同時考慮黏著性、給予皮膚之質感來選擇生物體接觸層之厚度。
又,本發明之生物體電極,也可與以往之生物體電極(例如日本特開2004-033468號公報記載之生物體電極)同樣,在生物體接觸層上另外設置黏著膜以防止使用時生物體電極從生物體脫落。另外設置黏著膜時,使用丙烯酸型、胺甲酸酯型、聚矽氧型等之黏著膜材料來形成黏著膜即可,尤其聚矽氧型因透氧性高,皮膚可在維持貼附之狀態進行呼吸,且又因撥水性高,汗水導致之黏著性降低少,再者對於皮膚之刺激性低,故為理想。另外,本發明之生物體電極,如上述,可藉由在生物體電極組成物中添加黏著性賦予劑、或使用對於生物體之黏著性良好的樹脂以防止從生物體脫落,故並非一定要設置上述另外設置的黏著膜。
針對將本發明之生物體電極製成穿戴式器件來使用時的生物體電極與感測器件之配線、其他構件並不特別限定,例如可使用日本特開2004-033468號公報記載者。
如上所述,若為本發明之生物體電極,由於係用上述本發明之生物體電極組成物之硬化物來形成生物體接觸層,故為能將來自皮膚的電訊號有效率地傳送至器件(亦即,導電性優異),即便長時間裝設於皮膚也無引起過敏之疑慮(亦即,生物相容性優異),輕量,能以低成本製造,無論被水沾濕或予以乾燥,導電性也不會大幅降低的生物體電極。又,可藉由添加碳材料以進一步改善導電性,可藉由和具有黏著性與伸縮性的樹脂組合以製造特別高黏著力且伸縮性高的生物體電極。再者,可藉由添加劑等來改善對皮膚之伸縮性、黏著性,也可藉由適當地調節樹脂之組成、生物體接觸層之厚度來調整伸縮性、黏著性。是以,若為如此的本發明之生物體電極,則作為醫療用穿戴式器件所使用的生物體電極特別理想。
>生物體電極之製造方法>
又,本發明提供一種生物體電極之製造方法,係具有導電性基材及形成於該導電性基材上的生物體接觸層之生物體電極之製造方法,其特徵為:藉由在該導電性基材上塗佈上述本發明之生物體電極組成物並使其硬化,從而形成該生物體接觸層。
另外,本發明之生物體電極之製造方法中使用之導電性基材、生物體電極組成物等,與上述者同樣即可。
於導電性基材上塗佈生物體電極組成物之方法不特別限定,例如浸塗、噴塗、旋塗、輥塗、流塗、刮刀塗佈、網版印刷、柔版印刷、凹版印刷、噴墨印刷等方法為較佳。
樹脂之硬化方法不特別限定,依生物體電極組成物中使用的(B)成分之種類適當地選擇即可,例如宜利用熱及光中之任一者或它們兩者來使樹脂硬化。又,於上述生物體電極組成物中添加有促使酸、鹼產生的觸媒,藉此亦可使交聯反應發生並使樹脂硬化。
另外,加熱時之溫度不特別限定,依生物體電極組成物中使用的(B)成分之種類適當地選擇即可,例如較佳為約50~250℃。
又,組合加熱與照光時,可同時進行加熱與照光,也可於照光後進行加熱,也可於加熱後進行照光。又,也可基於使溶劑蒸發之目的而於塗膜後加熱之前進行風乾。
如上所述,若為本發明之生物體電極之製造方法,能以低成本輕易地製造導電性及生物相容性優異,輕量,無論被水沾濕或予以乾燥,導電性也不會大幅降低的本發明之生物體電極。
[實施例]
以下,以實施例及比較例具體說明本發明,但本發明不限於該等。另外,「Me」表示甲基,「Vi」表示乙烯基。
作為離子性材料(導電性材料)而摻合於生物體電極組成物溶液中的離子性聚合物1~10、及比較離子性聚合物1、2係以如下方式合成。將各單體之30質量%PGMEA溶液放入反應容器並混合,將反應容器於氮氣環境下冷卻到-70℃,重複3次減壓脫氣、吹氮。升溫至室溫後,相對於單體全體1莫耳,加入0.01莫耳之偶氮雙異丁腈(AIBN)作為聚合起始劑,升溫至60℃後,使其反應15小時。將溶劑乾燥後,利用1
H-NMR來確認得到的聚合物之組成。又,得到的聚合物之分子量(Mw)及分散度(Mw/Mn)係利用使用了四氫呋喃(THF)作為溶劑之凝膠滲透層析(GPC)來確認。以此方式合成的離子性聚合物1~10、及比較離子性聚合物1、2係如下所示。
作為聚矽氧系之樹脂而摻合於生物體電極組成物溶液中的矽氧烷化合物1~4係如下所示。
(矽氧烷化合物1)
令30%甲苯溶液黏度為27,000mPa・s,烯基含量為0.007莫耳/100g,且分子鏈末端經以SiMe2
Vi基封端的含乙烯基之聚二甲基矽氧烷為矽氧烷化合物1。
(矽氧烷化合物2)
令由Me3
SiO0.5
單元及SiO2
單元構成之MQ樹脂之聚矽氧烷(Me3
SiO0.5
單元/SiO2
單元=0.8)之60%甲苯溶液為矽氧烷化合物2。
(矽氧烷化合物3)
令將30%甲苯溶液黏度為42,000mPa・s,烯基含量為0.007莫耳/100g,且分子鏈末端經以OH封端的含乙烯基之聚二甲基矽氧烷40質量份、由Me3
SiO0.5
單元及SiO2
單元構成之MQ樹脂之聚矽氧烷(Me3
SiO0.5
單元/SiO2
單元=0.8)之60%甲苯溶液100質量份、及甲苯26.7質量份所構成之溶液在乾餾的狀態下加熱4小時後予以冷卻,使聚二甲基矽氧烷鍵結於MQ樹脂而得者為矽氧烷化合物3。
(矽氧烷化合物4)
使用係為甲基氫矽油的信越化學工業製 KF-99。
又,使用係為聚醚型矽油的側鏈聚醚改性之信越化學工業製 KF-353作為聚矽氧系之樹脂。
摻合於生物體電極組成物溶液中的有機溶劑係如下所示。
PGMEA:丙二醇-1-單甲醚-2-乙酸酯
PGME:丙二醇-1-單甲醚
PGEE:丙二醇-1-單乙醚
作為添加劑而摻合於生物體電極組成物溶液中的自由基產生劑、鉑觸媒、導電性改善劑(碳黑、奈米碳管、覆金之粒子、覆銀之粒子、ITO粒子)係如下所示。
自由基產生劑:和光純藥工業公司製 V-601
鉑觸媒:信越化學工業製 CAT-PL-50T
碳黑:Denka公司製 Denka Black HS-100
多層奈米碳管:Sigma-Aldrich公司製 直徑110~170nm,長度5~9μm者
覆金之粒子:積水化學公司製 Micropearl AU(直徑100μm)
覆銀之粒子:三菱綜合材料公司製 覆銀粉(直徑30μm)
ITO粒子:三菱綜合材料公司製 ITO粉(直徑0.03μm)
[實施例1~14、比較例1~8]
按表1及表2記載之組成,混摻離子性材料(鹽)、樹脂、有機溶劑、及添加劑(自由基產生劑、鉑觸媒、導電性改善劑),製備生物體電極組成物溶液(生物體電極組成物溶液1~14、比較生物體電極組成物溶液1~8)。
(導電性評價)
使用塗抹器將生物體電極組成物溶液塗佈於直徑3cm、厚度0.2mm之鋁製圓板之上,於室溫進行6小時風乾後,使用烘箱於氮氣環境下於120℃烘烤30分鐘而使其硬化,每1種生物體電極組成物溶液製作4片生物體電極。以此方式得到之生物體電極,如圖3(a)、(b)所示,係於一面具有生物體接觸層3並於另一面具有作為導電性基材之鋁製圓板8者。其次,如圖3(b)所示,以黏著膠帶將銅配線9貼附於未覆有生物體接觸層之側之鋁製圓板8之表面而做成引出電極,將其連接至阻抗測定裝置。如圖4所示,以使人之手臂之皮膚與生物體接觸層側接觸的方式貼附2片生物體電極1’,並使其間隔為15cm。使用Solartron公司製之交流阻抗測定裝置SI1260,邊改變頻率邊測定初始阻抗。其次,將剩餘的2片生物體電極浸漬於純水中1小時,使水乾燥後,以與上述同樣之方法測定皮膚上之阻抗。將頻率1,000Hz時之阻抗示於表3。
(黏著性評價)
使用塗抹器將生物體電極組成物溶液塗佈於厚度100μm之PEN(聚萘二甲酸乙二酯)基板上,於室溫進行6小時風乾後,使用烘箱於氮氣環境下於120℃烘烤30分鐘而使其硬化,製作成黏著薄膜。從此黏著薄膜切出25mm寬之貼帶,使其壓接於不銹鋼版(SUS304),並於室溫放置20小時後,使用拉伸試驗機測定以角度180度、300mm/分鐘之速度將由黏著薄膜製作而得之貼帶從不銹鋼版剝離所需之力(N/25mm)。將結果示於表3。
(生物體接觸層之厚度測定)
對於上述導電性評價試驗中製作而得之生物體電極,使用測微計測定其生物體接觸層之厚度。將結果示於表3。
如表3所示,使用摻合了具特定結構之鹽(離子性材料)及樹脂的本發明之生物體電極組成物來形成生物體接觸層的實施例1~14,初始阻抗低,浸漬於水並予以乾燥後也未出現大幅的阻抗變化。亦即,實施例1~14獲得初始之導電性高,被水沾濕或予以乾燥時也未出現導電性之大幅降低的生物體電極。而且,如此的實施例1~14之生物體電極,具有與摻合了習知的鹽及樹脂的比較例1~5、比較例7、8之生物體電極同程度之良好的黏著力。
反觀使用摻合了習知的鹽及樹脂的生物體電極組成物來形成生物體接觸層的比較例1~4,雖然初始阻抗相對較低,但經在水中浸漬並予以乾燥後,出現了數量級改變之程度之大幅的阻抗增加。亦即,比較例1~4僅獲得初始之導電性高,但被水沾濕或予以乾燥時導電性大幅降低的生物體電極。
又,使用未摻合鹽而摻合了樹脂的生物體電極組成物來形成生物體接觸層的比較例5,由於未含有鹽,經在水中浸漬並予以乾燥後,也未出現數量級改變之程度之大幅的阻抗增加,但初始阻抗高。亦即,比較例5僅獲得初始之導電性低的生物體電極。
又,使用未摻合樹脂而摻合了鹽的生物體電極組成物來形成生物體接觸層的比較例6,由於含有和實施例同樣的鹽,經在水中浸漬並予以乾燥後,也未出現數量級改變之程度之大幅的阻抗增加,但由於未含有黏著性之樹脂,因此完全沒有黏著力,結果與皮膚之阻抗(初始阻抗)高。亦即,比較例6僅獲得初始之導電性低的生物體電極。
又,添加了不是本發明之重複單元的離子聚合物的比較例7及8,雖然黏著性高,但係為低的初始導電性。
由以上可知,若為使用了本發明之生物體電極組成物而形成有生物體接觸層的生物體電極,則導電性、生物相容性、對於導電性基材之黏接性優異,且由於離子性材料之保持力優異,無論被水沾濕或予以乾燥,導電性也不會大幅降低,而且輕量,且能以低成本製造。
另外,本發明不限於上述實施形態。上述實施形態係為例示,和本發明之申請專利範圍記載之技術思想有實質上相同構成且發揮同樣作用效果者皆包括在本發明之技術範圍內。
1‧‧‧生物體電極
1’‧‧‧生物體電極
2‧‧‧導電性基材
3‧‧‧生物體接觸層
4‧‧‧離子性聚合物(離子性材料)
5‧‧‧碳材料
6‧‧‧樹脂((A)成分以外之樹脂)
7‧‧‧生物體
8‧‧‧鋁製圓板
9‧‧‧銅配線
[圖1]係顯示本發明之生物體電極之一例的概略剖面圖。
[圖2]係顯示將本發明之生物體電極裝設於生物體時之一例的概略剖面圖。
[圖3]係將本發明之實施例中製作而得之生物體電極(a)從生物體接觸層側觀看之概略圖及(b)從導電性基材側觀看之概略圖。
[圖4]係以本發明之實施例中製作而得之生物體電極測定皮膚表面之阻抗時所拍攝的照片。
1‧‧‧生物體電極
2‧‧‧導電性基材
3‧‧‧生物體接觸層
4‧‧‧離子性聚合物(離子性材料)
5‧‧‧碳材料
6‧‧‧樹脂((A)成分以外之樹脂)
Claims (10)
- 一種生物體電極組成物,含有:(A)離子性材料,及(B)該(A)成分以外之樹脂,其特徵為:該(A)成分具有重複單元a及重複單元b兩者,其中,該(A)成分含有選自於下列通式(2)表示之重複單元a1~a7中之1種以上作為該重複單元a,並含有下列通式(3)表示之重複單元b1作為該重複單元b;
- 如申請專利範圍第1或2項之生物體電極組成物,其中,該(B)成分含有具有RxSiO(4-x)/2單元及SiO2單元之聚矽氧樹脂、具有烯基之二有機基矽氧烷、及具有SiH基之有機基氫聚矽氧烷;R為碳數1~10之經取代或未經取代之一價烴基,x為2.5~3.5之範圍。
- 如申請專利範圍第1或2項之生物體電極組成物,其中,該生物體電極組成物更含有有機溶劑。
- 如申請專利範圍第1或2項之生物體電極組成物,其中,該生物體電極組成物更含有碳材料。
- 如申請專利範圍第5項之生物體電極組成物,其中,該碳材料為碳黑及奈米碳管中之任一者或兩者。
- 一種生物體電極,具有導電性基材及形成於該導電性基材上的生物體接觸層,其特徵為:該生物體接觸層為如申請專利範圍第1至6項中任一項之生物體電極組成物之硬化物。
- 如申請專利範圍第7項之生物體電極,其中,該導電性基材包含選自於金、銀、氯化銀、鉑、鋁、鎂、錫、鎢、鐵、銅、鎳、不銹鋼、鉻、鈦、及碳中之1種以上。
- 一種生物體電極之製造方法,係具有導電性基材及形成於該導電性基材上的生物體接觸層之生物體電極之製造方法,其特徵為:藉由在該導電性基材上塗佈如申請專利範圍第1至6項中任一項之生物體電極組成物並使其硬化,從而形成該生物體接觸層。
- 如申請專利範圍第9項之生物體電極之製造方法,係使用包含選自於金、銀、氯化銀、鉑、鋁、鎂、錫、鎢、鐵、銅、鎳、不銹鋼、鉻、鈦、及碳中之1種以上者作為該導電性基材。
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