TWI775906B - 自黏性電極貼片 - Google Patents
自黏性電極貼片 Download PDFInfo
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- TWI775906B TWI775906B TW107125850A TW107125850A TWI775906B TW I775906 B TWI775906 B TW I775906B TW 107125850 A TW107125850 A TW 107125850A TW 107125850 A TW107125850 A TW 107125850A TW I775906 B TWI775906 B TW I775906B
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Abstract
本發明係關於一種分散體,其包含 i) 聚合物粒子A),該聚合物包含具有以下通式結構之重複單元: -CH2
-CHR1
-COOR2
- 其中 R1
表示H或烷基,及 R2
表示視情況經取代之C1
-C10
-烷基, 其中粒子A)具有至少500 nm之質量平均粒徑(d50
); ii) 導電聚合物粒子B), 其中該等粒子B)具有小於150 nm之質量平均粒徑; iii) 至少一種分散劑; 其中該粒子A)之聚合物與該粒子B)之導電聚合物之重量比為至少5:1。 本發明亦係關於一種層狀體、一種用於產生此層狀體之方法、藉由彼方法可獲得之層狀體及層狀體用於電物理量測之用途。
Description
本發明係關於例如可用作自黏性電極貼片之層狀體、可用於製備此層狀體之分散體、用於生產此層狀體之方法、可藉由彼方法獲得之層狀體、層狀體用於電物理量測之用途以及治療性電流傳送或電流接收系統。
皮膚表面電極為許多醫學診斷系統中之重要組件,包括(例如)心電圖(ECG)、肌電圖(EMG)及腦波圖(EEG)。在此等系統中,電極作為轉換器起重要作用,該轉換器將ECG、EMG及EEG中之生理變數,諸如心臟、肌肉及大腦之生理變數分別轉換為電位。所量測電位接著藉由諸如電子量測電路之儀器及電腦擴增及處理。
短期應用中最佳化之載流及/或散熱體電極領域中之先前技術為基於水性凝膠電解質之系統,諸如揭示於美國9,050,451 B1中之彼等者。然而,此類基於凝膠之電極相對於電極與皮膚之附接以及相對於長期穩定性而言為不利的。當將此等電極附接至患者之皮膚時,必須注意液體電解質不與黏著部分接觸,以便避免電極之黏著特性且因此電極與皮膚之間的接觸產生負面影響。另外,凝膠電解質通常為包含例如抗壞血酸或其衍生物之酸性含水系統。然而,若將電極用於長期應用,則此類酸性化合物之存在將導致諸如紅斑或皮膚刺激之副作用。
作為長期應用之替代方案,先前技術中已知基於包含碳之聚合物的電極,諸如揭示於美國7,136,691 B2中之裝載石墨之聚合物,或基於填充有金屬粒子之導電液體彈性體的電極,諸如揭示於DE 10 2008 050 932 A1中之橡膠組合物。然而,基於此等導電聚合物系統之電極在應用於皮膚之後需要大約30分鐘之一定前導時間,以便獲得可靠結果。此歸因於幾何及濕氣誘發之皮膚介面變化所引起之過渡電阻之變化。
在先前技術中亦已知諸如PEDOT/PSS之經摻雜噻吩可用作體電極中之導電材料。Leleux等人(Adv. Healthcare Mater, 2014, 3, 第1377-1380頁)揭示用於長期皮膚紀錄之離子液體凝膠輔助電極,其中離子液體凝膠併入由Au及PEDOT/PSS製備之電極上。將此等電極沈積於聚對二甲苯C之薄膜上,以使其對皮膚適應性。
然而,此等基於聚合物之電極系統之特徵在於其導電性相當低。出於此原因,複雜的金屬導電結構,諸如揭示於美國7,742,882中之彼等者較佳用於先前技術中,以獲得大部分儘可能均勻的電位分佈。然而,此等金屬導電結構之製造係複雜的且因此成本較高。
本發明係基於克服與皮膚表面電極相關之由先前技術所產生之缺點的目標。
特定而言,本發明係基於提供可用於皮膚表面電極中之皮膚接觸之層狀體的目標,該皮膚表面電極可易於應用於皮膚且即使在長期應用的情況下亦不會對皮膚產生負面影響。此等皮膚表面電極之過渡電阻應較佳不會由於電極之吸濕性而改變,從而使得其特別適合於長期量測。
本發明亦係基於提供可用於皮膚表面電極中之皮膚接觸之層狀體的目標,藉助於該皮膚表面電極可在將電極應用於皮膚之後立即獲得可靠結果。另外,層狀體之特徵在於其可用於長期應用中,且在於其電學特性,尤其係其側向及橫向電阻不受諸如體溫或環境濕度之參數顯著影響。在此情況下,若層狀體可用於皮膚表面電極中之皮膚接觸而無需添加液體電解質,則將係特別有利的。
本發明亦係基於提供可用於製備此層狀體之分散體的目標。本發明之另一目標為提供一種方法,藉助於該方法可以有效及成本效率的方式,較佳以可自動化大批量生產方法製備此層狀體。
藉由形成本發明之申請專利範圍之類別的主題來對達成上述目標中之至少一者作出貢獻。藉由表示本發明之特定實施例之附屬申請專利範圍之主題作出另一貢獻。
實施例 |1| 一種分散體,其包含: i) 聚合物粒子A),該聚合物包含具有以下通式結構之重複單元: -CH2
-CHR1
-COOR2
- 其中 R1
表示H或烷基,較佳為H或CH3
,最佳為H,及 R2
表示視情況經取代之C1
-C10
-烷基,較佳為選自由以下組成之群的基團:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
, 其中粒子A)具有至少500 nm、較佳至少600 nm、更佳至少700 nm、更佳至少800 nm、更佳至少900 nm且最佳至少1000 nm之質量平均粒徑(d50
); ii) 導電聚合物粒子B),較佳為陽離子聚噻吩及聚合陰離子之錯合物粒子B), 其中粒子B)具有小於150 nm、較佳小於145 nm、更佳小於140 nm、更佳小於135 nm、更佳小於130 nm且最佳小於125 nm之質量平均粒徑; iii) 至少一種分散劑,較佳為水; 其中粒子A)中之聚合物與粒子B)中之導電聚合物之重量比,較佳地粒子A)中之聚合物與粒子B)之錯合物中之陽離子聚噻吩及聚合陰離子之總重量之重量比為至少5:1、較佳至少10:1、更佳至少15:1、更佳至少20:1且最佳至少25:1。
|2| 如實施例|1|之分散體,其中粒子A)之聚合物具有小於35℃、較佳小於20℃、更佳小於10℃且最佳小於0℃之玻璃轉變溫度。
|3| 如實施例|1|或|2|之分散體,其中粒子A)具有在1000 nm至5000 nm範圍內、較佳在1000 nm至4000 nm範圍內且最佳在1000 nm至3000 nm範圍內之質量平均粒徑。
|4| 如實施例|1|至|3|中任一項之分散體,其中R1
為H且R2
選自由以下組成之群:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
。
|5| 如實施例|1|至|4|中任一項之分散體,其中以粒子A)之聚合物中之重複單元之總數目計,粒子A)之聚合物中至少25%、較佳至少35%、更佳至少45%且最佳至少55%之重複單元為單體,其中R1
為H且R2
選自由以下組成之群:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
。
|6| 如實施例|1|至|5|中任一項之分散體,其中粒子A)之聚合物為丙烯酸或丙烯酸鹽或該兩者及丙烯酸酯之共聚物。
|7| 如實施例|1|至|6|中任一項之分散體,其中粒子A)之聚合物為丙烯酸或丙烯酸鹽或該兩者及丙烯酸酯之共聚物,該丙烯酸酯選自由以下組成之群:丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、2-乙基己基丙烯酸酯及丙烯酸正辛酯。
|8| 如實施例|1|至|7|中任一項之分散體,其中分散體包含在10 wt%至80 wt%範圍內、較佳在15 wt%至75 wt%範圍內、更佳在20 wt%至70 wt%範圍內且最佳在25 wt%至65 wt%範圍內之量的粒子A)之聚合物,該等量在各情況下以分散體之總重量計。
|9| 如實施例|1|至|8|中任一項之分散體,其中粒子B)具有在25 nm至125 nm範圍內、較佳在50 nm至125 nm範圍內且最佳在75 nm至125 nm範圍內之質量平均粒徑。
|10| 如實施例|1|至|9|中任一項之分散體,其中粒子B)之導電聚合物包含PEDOT/PSS錯合物。
|11| 如實施例|1|至|10|中任一項之分散體,其中分散體包含總量在0.01 wt%至5 wt%範圍內、較佳在0.025 wt%至3.5 wt%範圍內、更佳在0.05 wt%至2 wt%範圍內且最佳在0.1 wt%至1 wt%範圍內之導電聚合物,較佳為陽離子聚噻吩及聚合陰離子,最佳為PEDOT/PSS,該等總量在各情況下以分散體之總重量計。
|12| 如實施例|1|至|11|中任一項之分散體,其中分散體進一步包含作為組分iv)之具有(在1013毫巴下)至少120℃、較佳至少140℃且最佳至少160℃之沸點的極性高沸點化合物。
|13| 如實施例|12|之分散體,其中極性高沸點化合物選自由以下組成之群:二醇,較佳為伸烷基二醇;三醇,較佳地丙三醇;及亞碸,較佳為DMSO。
|14| 如實施例|13|之分散體,其中極性高沸點化合物為乙二醇。
|15| 如實施例|12|至|14|中任一項之分散體,其中分散體包含在0.1 wt%至20 wt%範圍內、較佳在0.5 wt%至17.5 wt%範圍內、更佳在1 wt%至15 wt%範圍內且最佳在5 wt%至12.5 wt%範圍內之量的極性高沸點化合物,較佳為乙二醇,該等量在各情況下以分散體之總重量計。
|16| 如實施例|12|至|15|中任一項之分散體,其中極性高沸點化合物與粒子B)中之陽離子聚噻吩及聚合陰離子之總重量之重量比(極性高沸點化合物: (陽離子聚噻吩+聚合陰離子))為至少1:1、較佳至少3:1、更佳至少6:1且最佳至少9:1。
|17| 如實施例|1|至|16|中任一項之分散體,其中分散體為包含水作為分散劑之水性分散體。
|18| 一種層狀體,其包含: I) 基板; II) 導電黏著層,較佳為對人類皮膚具有自黏性且疊置在基板之至少一個表面的至少一部分上之導電黏著層,其中導電黏著層包含: IIa) 聚合物,其包含具有以下通式結構之重複單元: -CH2
-CHR1
-COOR2
- 其中 R1
表示H或烷基,較佳為H或CH3
,最佳為H,及 R2
表示視情況經取代之C1
-C10
-烷基,較佳為選自由以下組成之群的基團:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
, 且其中聚合物形成導電黏著層之基質; IIb) 導電聚合物之粒子,較佳為陽離子聚噻吩及聚合陰離子之錯合物之粒子,其分佈於基質中; 其中導電黏著層之特徵在於 - 橫向方向之比電阻(R橫向
)小於500 Ωm、較佳小於100 Ωm且最佳小於50 Ωm, 及 - 側向方向之比電阻(R側向
)小於5000 Ωm、較佳小於50 Ωm且最佳小於5 Ωm。
|19| 如實施例|18|之層狀體,其中基板包含非導電聚合物層及與非導電聚合物層之至少一個表面的至少一部分接觸之另一導電層,其中導電黏著層與另一導電層之至少一部分接觸。
|20| 如實施例|18|或|19|之層狀體,其中非導電聚合物層為具有厚度在1 µm至50 µm範圍內、較佳在3 µm至40 µm範圍內、更佳在6 µm至30 µm範圍內且最佳在10 µm至20 µm範圍內之聚醯亞胺層。
|21| 如實施例|18|至|20|中任一項之層狀體,其中另一導電層為銀柵格。
|22| 如實施例|18|至|21|中任一項之層狀體,其中聚合物IIa)具有小於35℃、較佳小於20℃、更佳小於10℃且最佳小於0℃之玻璃轉變溫度。
|23| 如實施例|16|至|20|中任一項之層狀體,其中R1
為H且R2
選自由以下組成之群:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
。
|24| 如實施例|18|至|23|中任一項之層狀體,其中以聚合物IIa)中之重複單元之總數目計,聚合物IIa)中至少25%、較佳至少35%、更佳至少45%且最佳至少55%之重複單元為單體,其中R1
為H且R2
選自由以下組成之群:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
。
|25| 如實施例|18|至|24|中任一項之層狀體,其中聚合物IIa)為丙烯酸或丙烯酸鹽或該兩者及丙烯酸酯之共聚物。
|26| 如實施例|18|至|25|中任一項之層狀體,其中聚合物IIa)為丙烯酸或丙烯酸鹽或該兩者及丙烯酸酯之共聚物,該丙烯酸酯選自由以下組成之群:丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、2-乙基己基丙烯酸酯及丙烯酸正辛酯。
|27| 如實施例|18|至|26|中任一項之層狀體,其中基質包含聚合物IIa)之複數個島狀物,該等島狀物具有至少1 × 10-6
mm2
、較佳至少1 × 10-5
mm2
、更佳至少1 × 10-4
mm2
且最佳至少1 × 10-3
mm2
之大小。
|28| 如實施例|18|至|27|中任一項之層狀體,其中粒子IIb)為PEDOT/PSS粒子。
|29| 如實施例|18|至|28|中任一項之層狀體,其中導電黏著層中之聚合物IIa)與粒子IIb)中之陽離子聚噻吩及聚合陰離子之總重量的重量比(聚合物IIa): (陽離子聚噻吩+聚合陰離子))為至少5:1、較佳至少10:1、更佳至少15:1、更佳至少20:1且最佳至少25:1。
|30| 如實施例|16|至|28|中任一項之層狀體,其中導電黏著層具有在1 µm至500 µm範圍內、較佳在3 µm至250 µm範圍內、更佳在4 µm至150 µm範圍內且最佳在5 µm至50 µm範圍內之厚度。
|31| 一種用於產生層狀體之方法,該方法包含: a1) 提供如實施例|1|至|17|中任一項所定義之分散體,較佳提供如實施例|12|至|16|中任一項所定義之分散體; a2) 將分散體塗覆於基板之至少一個表面之至少一部分上; a3) 至少部分移除分散劑iii)以形成導電黏著層,較佳形成對人類皮膚具有自黏性且疊置在基板之至少一個表面之至少一部分上的導電黏著層,其中分散劑之至少部分移除藉由將已經塗覆在基板上之分散體加熱至高於粒子A)之聚合物之玻璃轉變溫度的溫度來實現。
|32| 如實施例|31|之方法,其中粒子A)之聚合物具有小於35℃、較佳小於20℃、更佳小於10℃且最佳小於0℃之玻璃轉變溫度。
|33| 如實施例|31|或|32|之方法,其中基板如實施例|19|至|21|中所定義。
|34| 一種層狀體,其可藉由如實施例|31|至|33|中任一項之方法獲得。
|35| 如實施例|34|之層狀體,其中導電黏著層包含粒子A)之聚合物之基質,其中導電聚合物粒子B),較佳陽離子聚噻吩及聚合陰離子之錯合物粒子為分散的。
|36| 如實施例|34|或|35|之層狀體,其中導電黏著層之特徵在於 - 橫向方向之比電阻(R橫向
)小於500 Ωm、較佳小於100 Ωm且最佳小於50 Ωm, 及 - 側向方向之比電阻(R側向
)小於5000 Ωm、較佳小於50 Ωm且最佳小於5 Ωm。
|37| 如實施例|34|至|36|中任一項之層狀體,其中導電黏著層具有在1 µm至500 µm範圍內、較佳在3 µm至150 µm範圍內、更佳在4 µm至150 µm範圍內且最佳在5 µm至50 µm範圍內之厚度。
|38| 如實施例|18|至|30|及|34|至|37|中任一項之層狀體用於電物理量測之用途,其中導電黏著層與皮膚直接接觸。
|39| 如實施例|38|之用途,其中電物理量測包含心電圖(ECG)、腦波圖(EEG)、電阻抗斷層攝影(EIT)、肌電圖(EMG)及眼電圖(EOG)。
|40| 一種治療性電流傳送或電流接收系統,其包含: - 治療性電流傳送或電流接收裝置; - 至少一個電纜連接器,其連接至治療性電流傳送或電流接收裝置; - 至少一個電極,其包含連接至至少一個電纜連接器之如實施例|18|至|30|及|34|至|37|中任一項之層狀體。
藉由分散體對達成上述目標作出貢獻,該分散體包含: i) 聚合物粒子A),該聚合物包含具有以下通式結構之重複單元: -CH2
-CHR1
-COOR2
- 其中 R1
表示H或烷基,較佳為H或CH3
,最佳為H, 及 R2
表示視情況經取代之C1
-C10
-烷基,較佳為選自由以下組成之群的基團:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
, 其中粒子A)具有至少500 nm、較佳至少600 nm、更佳至少700 nm、更佳至少800 nm、更佳至少900 nm且最佳至少1000 nm之質量平均粒徑(d50
); ii) 導電聚合物粒子B),較佳為陽離子聚噻吩及聚合陰離子之錯合物粒子B), 其中粒子B)具有小於150 nm、較佳小於145 nm、更佳小於140 nm、更佳小於135 nm、更佳小於130 nm且最佳小於125 nm之質量平均粒徑; iii) 至少一種分散劑,較佳為水; 其中粒子A)中之聚合物與粒子B)中之導電聚合物之重量比,較佳粒子A)中之聚合物與粒子B)之錯合物中之陽離子聚噻吩及聚陰離子之總重量之重量比為至少5:1、較佳至少10:1、更佳至少15:1、更佳至少20:1且最佳至少25:1。
令人驚訝地,已發現具有小於150 nm之d50
值的較細粒徑之導電聚合物粒子(尤其PEDOT/PSS粒子)與具有至少500 nm之d50
值的基於聚丙烯酸酯之粒子的極特殊組合允許形成對人類皮膚具有自黏性且以傑出電學特性表徵,尤其以純歐姆特性表徵之導電黏著層。此等導電黏著層並不需要添加液體電解質,且相關電阻亦低於已知之基於電解質的電極系統。另外,此等導電黏著層在潮濕氛圍下儲存時僅展示可忽略之吸水性,此反過來亦使其特別適合用作體電極之接觸材料,此係因為過渡電阻不受濕氣所誘發之皮膚介面之變化的影響。組分 i)
根據本發明之分散體包含作為組分i)的聚合物粒子A),該聚合物包含具有以下通式結構之重複單元: -CH2
-CHR1
-COOR2
- 其中 R1
表示H或烷基,較佳為H或CH3
,最佳為H, 及 R2
表示視情況經取代之C1
-C10
-烷基,較佳為選自由以下組成之群的基團:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
, 其中粒子A)具有至少500 nm、較佳至少600 nm、更佳至少700 nm、更佳至少800 nm、更佳至少900 nm且最佳至少1000 nm之質量平均粒徑(d50
)。如根據本發明之分散體之尤佳實施例,粒子A)具有在1000 nm至5000 nm範圍內、較佳在1000 nm至4000 nm範圍內且最佳在1000 nm至3000 nm範圍內之質量平均粒徑。
粒子A)之聚合物為丙烯酸酯或甲基丙烯酸酯之聚合物或(甲基)丙烯酸酯及可與(甲基)丙烯酸酯共聚合之一或多種烯系不飽和單體之共聚物。術語「(甲基)丙烯酸」在本文中表示甲基丙烯酸及丙烯酸,較佳為丙烯酸。適合之粒子A)之聚合物包括以下聚合物,諸如聚((甲基)丙烯酸甲酯) (PMMA或PMA)、聚((甲基)丙烯酸乙酯)、聚((甲基)丙烯酸丁酯)、聚((甲基)丙烯酸異丁酯)、聚((甲基)丙烯酸己酯)、聚((甲基)丙烯酸異癸酯)、聚((甲基)丙烯酸月桂酯)、聚((甲基)丙烯酸苯酯)、聚(丙烯酸甲酯)、聚(丙烯酸異丙酯)、聚(丙烯酸異丁酯)、聚(丙烯酸十八烷基酯) (在本文中聯合稱作「聚丙烯酸」);或其共聚物及混合物。
尤佳的粒子A)之聚合物為包含上文所展示之通式結構之重複單元的聚合物,其中R1
為H且R2
選自由以下組成之群:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
,亦即基於丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、2-乙基己基丙烯酸酯、丙烯酸正辛酯或此等化合物之混合物作為單體的聚合物或共聚物。在此情況下,尤佳的為以粒子A)之聚合物中之重複單元之總數目計,粒子A)之聚合物中至少25%、較佳至少35%、更佳至少45%且最佳至少55%之重複單元為其中R1
為H且R2
選自由以下組成之群之單體:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
。在此情況下,更佳的為粒子A)之聚合物為丙烯酸或丙烯酸鹽或該兩者與丙烯酸酯之共聚物,尤佳為丙烯酸或丙烯酸鹽或該兩者與選自由以下組成之群之丙烯酸酯的共聚物:丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、2-乙基己基丙烯酸酯、丙烯酸正辛酯。
如根據本發明之分散體之另一實施例,粒子A)之聚合物僅略微交聯,或根據尤佳實施例完全不交聯。在此情況下,亦較佳的為粒子A)之聚合物在鹽水中藉由重量法根據NWSP 240.0.R2 (15)測定具有小於10 g/g、更佳小於1 g/g且最佳小於0.1 g/g之自由溶脹能力。
尤佳的粒子A)之聚合物為具有小於35℃、較佳小於20℃、更佳小於10℃且最佳小於0℃之玻璃轉變溫度的聚合物。
適合之粒子A)之聚合物為可商購的諸如可獲自Rudolf GmbH, Geretsried, Germany之RUCO-COAT®
AC 1010或RUCO-COAT®
AC 2510的聚丙烯酸酯分散體或諸如可獲自Alberdingk Boley GmbH, Krefeld, Germany之AQUA POLYMER AQP 275的聚丙烯酸酯分散體中之聚合物粒子。
較佳地,根據本發明之分散體包含在10 wt%至80 wt%範圍內、較佳在15 wt%至75 wt%範圍內、更佳在20 wt%至70 wt%範圍內且最佳在25 wt%至65 wt%範圍內之量的粒子A)之聚合物,該等量在各情況下以分散體之總重量計。組分 ii)
根據本發明之分散體包含作為組分ii)之導電聚合物粒子B),較佳為陽離子聚噻吩及聚合陰離子之錯合物粒子B), 其中粒子B)具有小於150 nm、較佳小於145 nm、更佳小於140 nm、更佳小於135 nm、更佳小於130 nm且最佳小於125 nm之質量平均粒徑。
如根據本發明之分散體之尤佳實施例,粒子B)具有在25 nm至125 nm範圍內、較佳在50 nm至125 nm範圍內且最佳在75 nm至125 nm範圍內之質量平均粒徑。
導電聚合物可為選自由以下組成之群的聚合物:視情況經取代之聚噻吩、視情況經取代之聚苯胺及視情況經取代之聚吡咯,其中視情況經取代之聚噻吩作為導電聚合物尤佳。
較佳聚噻吩為具有以下通式之彼等者:其中 A 表示視情況經取代之C1
-C5
伸烷基, R 表示直鏈或分支鏈視情況經取代之C1
-C18
烷基、視情況經取代之C5
-C12
環烷基、視情況經取代之C6
-C14
芳基、視情況經取代之C7
-C18
芳烷基、視情況經取代之C1
-C4
羥烷基或羥基,其中0至8個基團R可鍵結至A且在超過一個基團之情況下可相同或不同。
聚噻吩較佳在各情況下在末端基團上帶有H。
在本發明之上下文中,C1
-C5
伸烷基A較佳為亞甲基、伸乙基、伸正丙基、伸正丁基或伸正戊基。C1
-C18
烷基R較佳表示直鏈或分支鏈C1
-C18
烷基,諸如甲基、乙基、正丙基或異丙基、正丁基、異丁基、第二丁基或第三丁基、正戊基、1-甲基丁基、2-甲基丁基、3-甲基丁基、1-乙基丙基、1,1-二甲基丙基、1,2-二甲基丙基、2,2-二甲基丙基、正己基、正庚基、正辛基、2-乙基己基、正壬基、正癸基、正十一烷基、正十二烷基、正十三烷基、正十四烷基、正十六烷基或正十八烷基;C5
-C12
環烷基R表示例如環戊基、環己基、環庚基、環辛基、環壬基或環癸基;C5
-C14
芳基R表示例如苯基或萘基;且C7
-C18
芳烷基R表示例如苯甲基、鄰甲苯基、間甲苯基、對甲苯基、2,3-二甲苯基、2,4-二甲苯基、2,5-二甲苯基、2,6-二甲苯基、3,4-二甲苯基、3,5-二甲苯基或基。前述清單用以舉例說明本發明且不應視為結論性的。
在本發明之上下文中,許多有機基團為基團A及/或基團R之可能的視情況選用之其他取代基,例如烷基、環烷基、芳基、芳烷基、烷氧基、鹵基、醚基、硫醚基、二硫基、亞碸基、碸基、磺酸酯基、胺基、醛基、酮基、羧酸酯基、羧酸基、碳酸酯基、羧酸酯基、氰基、烷基矽烷基及烷氧基矽烷基及羧醯胺基。
尤其較佳的為其中A表示視情況經取代之C2
-C3
伸烷基之聚噻吩。聚(3,4-伸乙二氧基噻吩)作為聚噻吩為極其較佳的。
聚噻吩可為中性或陽離子,其中陽離子聚噻吩尤佳。術語「陽離子」僅與聚噻吩主鏈上的電荷有關。視在基團R上之取代基而定,在結構單元中聚噻吩可帶有正電荷及負電荷,正電荷位於聚噻吩主鏈上且負電荷視情況在經磺酸酯或羧酸酯基團取代之基團R上。在此情況下,聚噻吩主鏈之正電荷可部分或完全由視情況存在於基團R上之陰離子基團滿足。總體而言,在此等情況下,聚噻吩可為陽離子型、中性或甚至陰離子型。然而,在本發明之上下文中,其均視為陽離子聚噻吩,因為聚噻吩主鏈上之正電荷為決定因素。正電荷未在式中示出,因為不能絕對地判定其精確數目及位置。然而,正電荷之數目為至少1且至多n,其中n為聚噻吩內所有重現單元(相同或不同)之總數。
為補償陽離子聚噻吩之正電荷,較佳的為粒子B)進一步包含聚合陰離子,該聚合陰離子較佳基於用酸基官能化之聚合物。聚陰離子尤其可能為以下之陰離子:聚合羧酸,諸如聚丙烯酸、聚甲基丙烯酸或聚順丁烯二酸;或聚合磺酸,諸如聚苯乙烯磺酸及聚乙烯磺酸。此等聚羧酸及聚磺酸亦可為乙烯羧酸及乙烯磺酸與其他可聚合單體(諸如丙烯酸酯及苯乙烯)之共聚物。此外可能的聚陰離子為全氟化膠體形成之聚陰離子,其可例如以商品名Nafion®
商業上獲得。用酸基官能化且供應聚陰離子之聚合物之分子量較佳為1,000至2,000,000,尤其較佳為2,000至500,000。用酸基或其鹼金屬鹽官能化之聚合物可商業上獲得(例如聚苯乙烯磺酸及聚丙烯酸),或可藉由已知方法製備(參見例如Houben Weyl, Methoden der organischen Chemie, 第E 20卷 Makromolekulare Stoffe, 第2部分, (1987), 第1141頁等)。尤其較佳之聚陰離子為聚苯乙烯磺酸之陰離子。
粒子B)較佳包含陽離子聚噻吩及聚合陰離子之錯合物,尤其較佳PEDOT/PSS錯合物。此類錯合物可藉由在聚合陰離子存在下在水溶液中氧化聚合噻吩單體,較佳3,4-伸乙二氧基噻吩,較佳藉由在聚苯乙烯磺酸之陰離子存在下氧化聚合3,4-伸乙基-二氧噻吩來獲得。
較佳地,根據本發明之分散體包含在0.01 wt%至5 wt%範圍內、較佳在0.025 wt%至3.5 wt%範圍內、更佳在0.05 wt%至2 wt%範圍內且最佳在0.1 wt%至1 wt%範圍內之總量的導電聚合物,較佳為陽離子聚噻吩及聚合陰離子,較佳為PEDOT/PSS,該等總量在各情況下以分散體之總重量計(在陽離子聚噻吩及聚合陰離子之錯合物之情況下,上文所給出之量係指陽離子聚噻吩及聚合陰離子之總重量)。組分 iii)
根據本發明之分散體包含作為組分iii)之至少一種分散劑。
較佳分散劑為水,可與水混溶之溶劑,尤其選自由以下組成之群的彼等溶劑:脂族醇,諸如甲醇、乙醇、正丙醇及異丙醇、二丙酮醇;脂族酮,諸如丙酮及甲基乙基酮或此等溶劑中之至少兩者之混合物。然而,最佳溶劑為水,此意謂根據本發明之分散體較佳為含水分散體。在此情況下,尤佳的為分散體中分散劑總量之至少75 wt%、更佳至少80 wt%、甚至更佳至少85 wt%且甚至更佳至少90 wt%為水。組分 iv)
根據本發明之分散體可進一步包含作為組分iv)之具有(在1013毫巴下)至少120℃、較佳至少140℃且最佳至少160℃之沸點的極性高沸點化合物。可用作組分iv)之較佳化合物為二醇,較佳為伸烷基二醇;三醇,較佳為丙三醇;及亞碸,較佳為DMSO。尤佳伸烷基二醇為乙二醇、二甘醇、三甘醇、丙二醇、二丙二醇或此等伸烷基二醇中之至少兩者之混合物,其中乙二醇最佳。較佳地,極性高沸點化合物與粒子B)中之陽離子聚噻吩及聚合陰離子之總重量之重量比(極性高沸點化合物: (陽離子聚噻吩+聚合陰離子))為至少1:1、較佳至少3:1、更佳至少6:1且最佳至少9:1。
根據本發明之分散體中之極性高沸點化合物(較佳為乙二醇)之量較佳在0.1 wt%至20 wt%範圍內、更佳在0.5 wt%至17.5 wt%範圍內、更佳在1 wt%至15 wt%範圍內且最佳在5 wt%至12.5 wt%範圍內,該等量在各情況下以分散體之總重量計。組分 v)
根據本發明之分散體可進一步包含作為組分v)之與組分i)至iv)不同的至少一種其他添加劑。適合之添加劑v)為 - 界面活性物質,例如陰離子界面活性劑,諸如烷基苯磺酸及烷基苯磺酸鹽、烷烴磺酸鹽、醇磺酸鹽、醚磺酸鹽、磺基丁二酸鹽、磷酸酯鹽、烷基醚羧酸或烷基醚羧酸鹽;陽離子界面活性劑,諸如烷基四級銨鹽;非離子界面活性劑,諸如直鏈醇乙氧基化物、側氧基醇乙氧基化物、烷基酚乙氧基化物或烷基聚葡萄糖苷,尤其以商標Dynol®
及Zonyl®
可商購之界面活性劑, - 黏著促進劑,諸如有機官能性矽烷或其水解產物,例如3-縮水甘油氧丙基三烷氧基矽烷、3-胺基-丙基三乙氧基矽烷、3-巰基丙基三甲氧基矽烷、3-甲基丙烯醯氧丙基三甲氧基-矽烷、乙烯基三甲氧基矽烷或辛基三乙氧基矽烷, - 交聯劑,諸如三聚氰胺化合物、封閉異氰酸鹽、官能化矽烷(例如四乙氧基矽烷、例如基於四乙氧基矽烷之烷氧基矽烷水解產物、環氧矽烷(諸如3-縮水甘油氧基丙基三烷氧基矽烷)), - 導電性增強劑,例如含有醚基團之化合物,諸如四氫呋喃;含有內酯基團之化合物,諸如γ-丁內酯、γ-戊內酯;含有醯胺或內醯胺基團之化合物,諸如己內醯胺、N-甲基己內醯胺、N,N-二甲基-乙醯胺、N-甲基乙醯胺、N,N-二甲基甲醯胺(DMF)、N-甲基-甲醯胺、N-甲基甲醯苯胺、N-甲基吡咯啶酮(NMP)、N-辛基-吡咯啶酮、吡咯啶酮;碸及亞碸,諸如環丁碸(四亞甲基碸)、二甲亞碸(DMSO);糖或糖衍生物,諸如蔗糖、葡萄糖、果糖、乳糖;糖醇,諸如山梨醇、甘露醇;呋喃衍生物,諸如2-呋喃甲酸、3-呋喃甲酸、丙三醇、二甘油、三甘油或四甘油。
根據本發明之分散體中之此類其他添加劑之量較佳在0.1 wt%至15 wt%範圍內、更佳在0.5 wt%至12.5 wt%範圍內、更佳在0.75 wt%至10 wt%範圍內且最佳在1 wt%5 wt%範圍內,該等量在各情況下以分散體之總重量計。
根據本發明之分散體可藉由將包含上述粒子A)之分散體(較佳為水性分散體) (例如諸如RUCO-COAT®
AC 1010 AQUA POLYMER AQP 275之分散體)與包含上述粒子B)之分散體(較佳為水性分散體) (例如PEDOT/PSS分散體,諸如Heraeus Clevios™ P HC V6 Screen、Heraeus Clevios™ P、Heraeus Clevios™ P HC V4、Heraeus Clevios™ P Jet、Heraeus Clevios™ P Jet 700、Heraeus Clevios™ P Jet HC、Heraeus Clevios™ P Jet HC V2、Heraeus Clevios™ P Jet N、Heraeus Clevios™ P Jet N V2、Heraeus Clevios™ P Jet UA、Heraeus Clevios™ P T2、Heraeus Clevios™ P VP AI 4083、Heraeus Clevios™ P VP CH 8000、Heraeus Clevios™ PH 1000、Heraeus Clevios™ PH 500、Heraeus Clevios™ PH 510、Heraeus Clevios™ PH、Heraeus Clevios™ S HAT、Heraeus Clevios™ S V3、Heraeus Clevios™ S V3 HV或Heraeus Clevios™ S V4)簡單混合來製備。此類PEDOT/PSS分散體可購自Heraeus Deutschland GmbH, Hanau, Germany。任選地,伸烷基二醇(組分iv))及其他添加劑(組分v))可在其經混合之前添加至此等分散體中之一或兩者中或可分別添加至此等分散體之混合物中。
藉由層狀體對達成上述目標作出貢獻,該層狀體包含: (I) 基板; (II) 導電黏著層,較佳為對人類皮膚具有自黏性且疊置在基板之至少一個表面的至少一部分上之導電黏著層,其中導電黏著層包含: IIa) 聚合物,其包含具有以下通式結構之重複單元: -CH2
-CHR1
-COOR2
- 其中 R1
表示H或烷基,較佳為H或CH3
,最佳為H, 及 R2
表示視情況經取代之C1
-C10
-烷基,較佳為選自由以下組成之群的基團:-CH3
、-CH2
CH3
、-C4
H9
、-CH2
CH(C2
H5
)(C4
H9
)及-C8
H17
, 且其中聚合物形成導電黏著層之基質; IIb) 導電聚合物粒子,較佳為陽離子聚噻吩及聚合陰離子之錯合物粒子,其分佈於基質中; 其中導電黏著層之特徵在於 - 橫向方向之比電阻(R橫向
)小於500 Ωm、較佳小於100 Ωm且最佳小於50 Ωm, 及 - 側向方向之比電阻(R側向
)小於5000 Ωm、較佳小於50 Ωm且最佳小於5 Ωm。
此層狀體例如可藉由將根據本發明之分散體塗覆於基板上且藉由隨後去除分散劑之至少一部分以形成導電黏著層獲得。組件 I)
根據本發明之層狀體包含作為組件I)之基板。
基板較佳為可撓性基板,其特徵在於對人類皮膚具有足夠適應性。基板之較佳材料為塑膠膜,其習知地具有在2 µm至200 µm範圍內、較佳在3 µm至150 µm範圍內、更佳在4 µm至100 µm範圍內且最佳在5 µm至100 µm範圍內之厚度。此類塑膠膜可基於(例如)諸如聚碳酸酯之聚合物、諸如聚對苯二甲酸伸乙酯(PET)及聚萘二甲酸乙二醇酯(PEN)之聚酯、共聚碳酸酯、聚碸、聚醚碸(PES)、聚醯亞胺、聚醯胺、聚乙烯、聚丙烯或環狀聚烯烴或環狀烯烴共聚物(COC)、聚氯乙烯、聚苯乙烯、氫化苯乙烯聚合物或氫化苯乙烯共聚物。基板之特別適合之材料為諸如myclar、撓曲PC、Kapton或聚合物厚膜(PTF)之材料。根據本發明之層狀體之一尤佳實施例,諸如可商購之Kapton箔片之聚醯亞胺膜用作可撓性基板。可替代地,薄聚合物層可由適當的聚合物前驅體沈積於無機載體基板(諸如玻璃)上。聚醯亞胺膜可例如藉由聚醯胺羧酸之熱聚縮合形成於玻璃載體基板上。此在大約10 μm之區域中產生特別薄的基板層,其特徵在於可忽略的機械硬度及對皮膚表面之良好適應性。
根據本發明之層狀體之一較佳實施例,基板包含非導電聚合物層及與非導電聚合物層之至少一個表面的至少一部分接觸之另一導電層,其中導電黏著層與另一導電層之至少一部分接觸。另一導電層用以改良層狀體之側嚮導電性。較佳地,另一導電層為基於碳、金屬或金屬粒子之層,其中此等導電材料較佳以柵格之形式存在。在此上下文中,可能的金屬為習知用於產生線性金屬結構(所謂的「母線」)之電子組件中之所有金屬,諸如鋁、銀、金或銅。在包含金屬粒子之另一導電層的情況下,此等金屬粒子較佳以包含具有小於10 µm粒徑之此類金屬粒子之糊狀物形式施用。就此而論,導電之銀粒子或銅粒子極其較佳。若除金屬粒子之外,糊狀物尤其可包含待使用之溶劑及黏結劑,則經由網版印刷製程塗覆此等糊狀物更佳。亦適合於形成另一導電層的為可藉由真空沈積塗覆於非導電聚合物層上之金屬層,諸如銅層、金層或鋁層。另外,另一導電層亦可藉助於基於金屬有機材料之墨形成,例如包含金屬羧酸鹽之墨及/或包含金屬奈米粒子或奈米線之墨。此類墨可例如藉由數位噴墨列印塗覆在基板上。
根據本發明之層狀體之一尤佳實施例,非導電聚合物層為具有在1 µm至50 µm範圍內、較佳在3 µm至40 µm範圍內、更佳在6 µm至30 µm範圍內且最佳在10 µm至20 µm範圍內之厚度的聚醯亞胺層。另一導電層較佳為銀柵格,更佳為藉助於銀漿料塗覆於此聚醯亞胺層上之銀柵格。組件 II)
根據本發明之層狀體包含作為組件II)之導電黏著層,較佳為對人類皮膚具有自黏性且疊置在基板之至少一個表面之至少一部分上的導電黏著層。此導電黏著層包含聚合物IIa),該聚合物IIa)在其化學組成方面且亦在其玻璃轉變溫度方面較佳對應於上文結合根據本發明之分散體詳細描述之粒子A)之聚合物。在根據本發明之層狀體之導電黏著層中,聚合物IIa)形成導電黏著層之基質,其中分佈導電聚合物粒子IIb),較佳為陽離子聚噻吩及聚合陰離子之錯合物粒子IIb)。較佳導電聚合物以及陽離子聚噻吩及聚合陰離子之較佳錯合物又為已於上文結合根據本發明之分散體描述為較佳導電聚合物及粒子B)之錯合物之彼等導電聚合物及彼等錯合物。
根據本發明之層狀體之一尤佳實施例,導電黏著層之基質包含聚合物IIa)之複數個島狀物,該等島狀物具有至少1 × 10- 6
mm2
、較佳至少1 × 10- 5
mm2
、更佳至少1 × 10- 4
mm2
且最佳至少1 × 10- 3
mm2
之大小。此結構可例如在形成導電黏著層時,將除組分i)、ii)及iii)之外亦包含作為組分iv)之伸烷基二醇(諸如乙二醇)之根據本發明之分散體塗覆在基板上,且若隨後藉由在高於粒子A)之聚合物之玻璃轉變溫度的溫度下乾燥來移除分散劑iii)時獲得。儘管不希望受理論束縛,但據信若在高於聚合物IIa)之玻璃轉變溫度之溫度下在基板上乾燥此分散體,則分散體中極性高沸點溶劑(諸如乙二醇)之存在在某種程度上有助於相鄰粒子A)之退火同時形成聚合物IIa)之較大島狀物,從而導電聚合物之粒子IIb),較佳地包含陽離子聚噻吩及聚合陰離子之錯合物之粒子IIb),在該乾燥階段期間仍以濕潤狀態移動,且隨後在繼續乾燥時填充聚合物IIa)之此等經退火聚合物島狀物之間的中間空間。此結構導致側向方向之電導率C側向
與正交方向之電導率C正交
的比率特別高。在此類極性高沸點溶劑不存在之情況下,聚合物IIa)之粒子相當快速地乾燥,此乾燥製程在某種程度上將粒子固定在表面上且使相鄰粒子之退火幾乎不可能發生。
根據本發明之層狀體中之導電黏著層之厚度較佳在1 µm至500 µm範圍內、較佳在3 µm至250 µm範圍內、更佳在4 µm至150 µm範圍內且最佳在5 µm至50 µm範圍內。
根據本發明之層狀體之一較佳實施例,導電黏著層中之聚合物IIa)與粒子IIb)中之陽離子聚噻吩及聚合陰離子之總重量的重量比(聚合物IIa): (陽離子聚噻吩+聚陰離子))為至少5:1、較佳至少10:1、更佳至少15:1、更佳至少20:1且最佳至少25:1。
根據本發明之層狀體之另一較佳實施例,此層狀體之特徵在於當在25℃及80%相對濕度下儲存層狀體22小時時,導電黏著層吸收小於10 wt%、較佳小於7.5 wt%、更佳小於5 wt%且最佳小於2.5 wt%之水。
亦藉由產生層狀體之方法對達成上述目標作出貢獻,該方法包含: a1) 提供根據本發明之分散體; a2) 將分散體塗覆於基板之至少一個表面之至少一部分上; a3) 至少部分移除分散劑iii)以形成導電黏著層,較佳形成對人類皮膚具有自黏性且疊置在基板之至少一個表面之至少一部分上的導電黏著層,其中分散劑之至少部分移除藉由將已經塗覆在基板上的分散體加熱至高於粒子A)之聚合物之玻璃轉變溫度的溫度來實現。
在根據本發明之方法的方法步驟a1)中,提供根據本發明之分散體。在此上下文中,尤佳的為粒子A)之聚合物具有小於35℃、較佳小於20℃、更佳小於10℃且最佳小於0℃之玻璃轉變溫度。在此上下文中,亦較佳的為分散體包含作為組分iv)之伸烷基二醇,諸如乙二醇。如上文所陳述,此分散體可例如藉由使包含上述粒子A)之分散體(較佳為水性分散體) (例如諸如RUCO-COAT®
AC 1010 AQUA POLYMER AQP 275之分散體)與包含上述粒子B)之分散體(較佳為水性分散體) (例如可購自Heraeus Holding GmbH, Hanau, Germany之PEDOT/PSS分散體中之一者)混合來製備。較佳地,上述極性高沸點化合物(尤其伸烷基二醇)及任選地其他添加劑可在其經混合之前添加至此等分散體中之一或兩者中或可分別添加至此等分散體之混合物中。
在根據本發明之方法的方法步驟a2)中,將分散體塗覆於基板之至少一個表面之至少一部分上。將分散體塗覆於基板之至少一個表面的至少一部分上可在0.1 µm至250 µm範圍內、較佳在0.5 µm至50 µm範圍內之厚度的濕膜中藉由已知之方法來實現,該等方法例如旋轉塗佈、浸塗、澆注、滴液、注射、噴塗、膜傳送塗覆、刮刀塗覆、散佈或列印,例如噴墨、篩檢、凹版、平版或移印。
可用於根據本發明之方法中之較佳基板為上文已提及之與根據本發明之層狀體相關的較佳基板中之彼等基板。
在根據本發明之方法之方法步驟a3)中,分散劑經至少部分移除以形成導電黏著層,較佳形成對人類皮膚具有自黏性且疊置在基板之至少一個表面之至少一部分上的導電黏著層,其中分散劑之至少部分移除藉由將已經塗覆在基板上的分散體加熱至高於粒子A)之聚合物之玻璃轉變溫度的溫度來實現。分散劑iii)之部分移除可藉由僅乾燥疊置層,較佳藉由將基板加熱至例如35℃至200℃、較佳75℃至150℃範圍內之溫度來達成。
亦藉由可藉由本發明之方法獲得之層狀體對達成上述目標作出貢獻。較佳地,此層狀體之性質與上文已描述之根據本發明之層狀體之性質一致。
因此,藉由根據本發明之方法可獲得之層狀體之較佳特徵在於導電黏著層包含粒子A)之聚合物之基質,其中導電聚合物之粒子B),較佳地陽離子聚噻吩及聚合陰離子之錯合物粒子為分散的。在此上下文中,亦較佳的為導電黏著層包含聚合物IIa)之複數個島狀物,該等島狀物具有至少1 × 10- 6
mm2
、較佳至少1 × 10- 5
mm2
、更佳至少1 × 10- 4
mm2
且最佳至少1 × 10- 3
mm2
之大小。
另外,藉由根據本發明之方法可獲得之層狀體之較佳特徵在於導電黏著層由以下表徵 - 橫向方向之比電阻(R橫向
)小於500 Ωm、較佳小於100 Ωm且最佳小於50 Ωm, 及 - 側向方向之比電阻(R側向
)小於5000 Ωm、較佳小於50 Ωm且最佳小於5 Ωm。
除此之外,藉由根據本發明之方法可獲得之層狀體之較佳特徵在於在25℃及80%相對濕度下儲存層狀體22小時時,導電黏著層吸收小於10 wt%、較佳小於7.5 wt%、更佳小於5 wt%且最佳小於2.5 wt%之水。
亦藉由使用根據本發明之層狀體或使用藉由根據本發明之方法可獲得的用於電物理量測之層狀體來對達成上述目標作出貢獻,其中導電黏著劑層與皮膚直接接觸。較佳電物理量測包含心電圖(ECG)、腦波圖(EEG)、電阻抗斷層攝影術(EIT)、肌電圖(EMG)及眼電圖(EOG)。
亦藉由治療性電流傳送或電流接收系統來對達成上述目標作出貢獻,其包含: - 治療性電流傳送或電流接收裝置; - 至少一個電纜連接器,其連接至該治療性電流傳送或電流接收裝置; - 至少一個電極,其包含本發明之層狀體或由藉由本發明之方法可獲得之層狀體製備。
治療性電流傳送或電流接收裝置可為熟習此項技術者所已知的任何類型之監測或刺激裝置,諸如心電圖(ECG)裝置、腦電波裝置、肌電圖裝置、經皮電神經刺激裝置、電肌肉刺激裝置、肌神經刺激裝置或功能性電刺激裝置。
現藉助於測試方法及非限制性圖式及實例更詳細地解釋本發明。
如在圖1及圖2中可見,根據本發明之層狀體1包含基板2,根據本發明之導電黏著層3疊置在該基板2上。基板2較佳包含非導電聚合物層2a,其在本申請案之實例中為薄的聚醯亞胺膜,另一導電層2b疊置在其上。在本申請案之實例中,另一導電層2b為藉助於銀漿料已塗覆於聚醯亞胺膜上之銀柵格。
測試方法粒子 A ) 及粒子 B ) 之 d50 值之判定
經由超速離心判定粒子A)及粒子B)之d50
值。根據Schlotan等人(Kolloid-Z und Z Polymer; 250 (1972)第782頁, 「Bestimmung der Teilchengr öß enverteilung von Latices mit der Ultrazentrifuge
」)及Müller (Colloid & Polymer Science; 267 (1989)第1113頁)描述方法之細節。必要時,可藉由熟習此項技術者所已知之技術(諸如密度梯度離心、凝膠滲透層析法或凝膠電泳)將粒子A)及/或粒子B)與可能干擾d50
值之判定的其他粒子分離。
玻璃轉變溫度之判定
玻璃轉變溫度藉助於差分量熱法(DSC) (ISO 11357-2)量測。嚴格地說,此係延伸超過溫度範圍之玻璃轉變區域。參考本發明中之玻璃轉變溫度錶示平均值。
濕氣吸收之判定
在鋁托盤中給定8 g與9 g之間的根據本發明之分散體,且在120℃之溫度下在具有再循環空氣烘箱中乾燥托盤135分鐘。乾燥膜保留在托盤中,該托盤之重量藉由稱重來判定(托盤before storage
)。
隨後,將鋁托盤儲存於25℃之溫度下藉助於飽和鹽溶液所產生的80%相對濕度之封閉乾燥器中。在22個小時之後,再次稱重鋁托盤(托盤after storage
)且濕氣吸收(以wt%為單位)計算如下: 水分吸收 = 100 % ´ (托盤after storage
- 托盤before storage
)/ 托盤before storage
側向及橫向電阻之判定
導電黏著層側向方向之比電阻(R側向
)藉由藉助於ACL 800數位兆歐計(ACL Staticide, Chicago, IL, USA)量測表面電阻(以W/為單位)來判定。比電阻藉由將表面電阻與導電黏著層之厚度(以m為單位)相乘來計算。導電黏著層之厚度係基於用於製備導電黏著層之分散體之固體含量及塗覆在基板上之分散體的濕膜厚度來計算。
導電黏著層橫向方向之比電阻(R橫向
)藉由使用SP-300恆電位器/恆電流儀(Bio-Logic SAS, Claix, France)之阻抗光譜測定法判定。附接在導電黏著層之表面上的鉑電極充當銀柵極之對立電極,該銀柵極定位於導電黏著劑層下方。導電黏著層橫向方向之比電阻在1 kHz之頻率下判定。
實例實例 1 :導電黏著組合物之製備
製備導電聚合物、陰離子丙烯酸酯共聚物分散體及視情況選用之乙二醇之混合物。出於彼目的,高導電含水PEDOT/PSS分散體(Clevios™ P HC V6篩檢;固體含量1 wt%)引入至燒杯中。隨後,逐滴添加含水丙烯酸酯分散體Rucocoat AC 1010 (固體含量65 wt%)、AQP 275(固體含量60 wt%)及Acronal S728 (固體含量50 wt%%),隨後添加乙二醇。隨後攪拌混合物30分鐘。
出於表徵,藉助於具有40 μm之濕膜厚度地手動刮板且將在強制風乾機櫃中在120℃下乾燥5分鐘而將樣本塗佈在Melinex PET膜基板上。量測電表面電阻(Ohm/sq;ACL 800, Staticide)且用手指定性地判定黏著力(需要提舉具有約20 cm × 30 cm之大小的膜的手指壓力/手指數目)。另外,就用此等樣本製備之乾燥膜之濕氣吸收而言,分析藉助於此等樣本製備之黏著層。
實例 2 : 電極之製備
玻璃支撐基板用PAA (聚醯胺羧酸)塗佈,隨後將其熱縮聚以獲得PI (聚醯亞胺)。所得聚合物膜具有10 μm之厚度。接著藉助於如圖2中所展示之網版印刷來網版印刷用於電位均質化之基於PI的銀漿料。
此系統隨後用實例1中所獲得之樣本A至G塗佈。出於此目的,藉由漆塗層將樣本塗佈在具有90 μm濕膜厚度之聚醯亞胺電極基板上,且隨後在120℃下在循環風乾機櫃中乾燥5分鐘。第二次執行此操作以獲得厚的導電黏著層。由此獲得之樣本設置有由Pt箔片製成的非偏振電極,以便檢測在5 MHz至100 mHz的範圍內之阻抗特性。然而,所有樣本顯示具有由引線所引起之輕微電感分量之純歐姆特性。
如可見,添加乙二醇對各向異性正交於側嚮導電性之PEDOT/PSS的定向具有影響。藉由添加乙二醇,可撓性基板上所要的金屬柵格之比例可因此減小。
相比於先前技術之電極,根據本發明之電極展示純歐姆特性且相關電阻亦低於已知的基於電解質之電極系統。
1‧‧‧層狀體2‧‧‧基板2a‧‧‧非導電聚合物層2b‧‧‧另一導電層3‧‧‧導電黏著層
圖1展示根據本發明之較佳層狀體之橫截面。 圖2展示可用於自頂部形成根據本發明之層狀體之基板。
1‧‧‧層狀體
2‧‧‧基板
2a‧‧‧非導電聚合物層
2b‧‧‧另一導電層
3‧‧‧導電黏著層
Claims (19)
- 一種分散體,其包含:i)聚合物粒子A),該聚合物包含具有以下通式結構之重複單元:-CH2-CHR1-COOR2-其中R1 表示H或烷基,及R2 表示視情況經取代之C1-C10-烷基,其中粒子A)具有至少800nm之質量平均粒徑(d50);ii)導電聚合物粒子B),其中該等粒子B)具有小於150nm之質量平均粒徑;iii)至少一種分散劑;其中粒子A)中之該聚合物與粒子B)中之該導電聚合物之重量比為至少15:1。
- 如請求項1之分散體,其中該導電聚合物粒子B)係陽離子聚噻吩及聚合陰離子之錯合物之粒子,且其中粒子A)中之該聚合物與粒子B)之該錯合物中之該陽離子聚噻吩及該聚合陰離子之總重量的重量比為至少15:1。
- 如請求項1之分散體,其中該分散劑為水。
- 如請求項1或2之分散體,其中粒子A)中之該聚合物與粒子B)中之該導電聚合物之重量比為至少20:1。
- 如請求項1或2之分散體,其中粒子A)中之該聚合物與粒子B)中之該導電聚合物之重量比為至少25:1。
- 如請求項1或2之分散體,其中粒子A)具有至少900nm之質量平均粒徑(d50)。
- 如請求項1或2之分散體,其中粒子A)具有至少1000nm之質量平均粒徑(d50)。
- 如請求項1或2之分散體,其中粒子A)之該聚合物具有小於35℃之玻璃轉變溫度。
- 如請求項1或2之分散體,其中R1為H且R2選自由以下組成之群:-CH3、-CH2CH3、-C4H9、-CH2CH(C2H5)(C4H9)及-C8H17。
- 如請求項1或2之分散體,其中以粒子A)之該聚合物中之重複單元總數目計,粒子A)之該聚合物中之該等重複單元的至少25%為其中R1為H且R2選自由以下組成之群的單體:-CH3、-CH2CH3、-C4H9、-CH2CH(C2H5)(C4H9)及-C8H17。
- 如請求項1或2之分散體,其中粒子A)之該聚合物為丙烯酸或丙烯酸鹽或該兩者與選自由以下組成之群之丙烯酸酯的共聚物:丙烯酸甲酯、丙 烯酸乙酯、丙烯酸正丁酯、2-乙基己基丙烯酸酯及丙烯酸正辛酯。
- 如請求項1或2之分散體,其中粒子B)之該導電聚合物包含PEDOT/PSS錯合物。
- 如請求項1或2之分散體,其中該分散體進一步包含作為組分iv)之具有(在1013毫巴下)至少120℃之沸點之極性高沸點化合物。
- 如請求項13之分散體,其中該極性高沸點化合物為乙二醇。
- 一種用於產生層狀體(1)之方法,該方法包含:α1)提供如請求項1至14中任一項所定義之分散體;α2)將該分散體塗覆於基板(2)之至少一個表面之至少一部分上;α3)至少部分移除該分散劑iii)以形成導電黏著層,其中該分散劑之該至少部分移除係藉由將已經塗覆在該基板上的該分散體加熱至高於粒子A)之該聚合物之玻璃轉變溫度的溫度來實現。
- 如請求項15之方法,其中該導電黏著層對人類皮膚具有自黏性且疊置在該基板(2)之至少一個表面之至少一部分上。
- 一種層狀體(1),其可藉由如請求項15之方法獲得。
- 一種如請求項17之層狀體(1)用於電物理量測之用途,其中該導電黏 著層(3)與皮膚直接接觸。
- 一種治療性電流傳送或電流接收系統,其包含:治療性電流傳送或電流接收裝置;至少一個電纜連接器,其連接至該治療性電流傳送或電流接收裝置;至少一個電極,其包含連接至該至少一個電纜連接器之如請求項17之層狀體(1)。
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TWI512000B (zh) | 2013-02-15 | 2015-12-11 | Shinetsu Polymer Co | A conductive composition, a method for producing a conductive composition, an antistatic resin composition, and an antistatic resin film |
US20160196892A1 (en) * | 2015-01-07 | 2016-07-07 | Nagase Chemtex Corporation | Conductive resin composition and transparent conductive laminated body |
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EP3318589A1 (en) | 2016-11-02 | 2018-05-09 | Heraeus Deutschland GmbH & Co. KG | Pedot/pss with coarse particle size and high pedot-content |
EP3354689B1 (en) | 2017-01-30 | 2024-01-24 | Heraeus Epurio GmbH | Compositions useful for the formation of an antistatic layer or an electromagnetic radiation shield |
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TW201546979A (zh) * | 2014-01-28 | 2015-12-16 | Nippon Telegraph & Telephone | 電極構件及裝置 |
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Title |
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期刊 Kim, Byeonggwan et al. Waterborne polyacrylic/PEDOT nanocomposites for conductive transparent adhesives Journal of Nanoscience and Nanotechnology Volume 13, Number 11 Journal of Nanoscience and Nanotechnology November 2013 Pages 7631-7636 * |
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KR20200027979A (ko) | 2020-03-13 |
KR102403191B1 (ko) | 2022-05-31 |
CN111148790A (zh) | 2020-05-12 |
US20200214632A1 (en) | 2020-07-09 |
JP2020527974A (ja) | 2020-09-17 |
EP3434177A1 (en) | 2019-01-30 |
WO2019020571A1 (en) | 2019-01-31 |
US11980478B2 (en) | 2024-05-14 |
JP7216702B2 (ja) | 2023-02-01 |
TW201920457A (zh) | 2019-06-01 |
EP3434177B1 (en) | 2022-01-26 |
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