TW202230411A - 固體電解電容器、固體電解質、導電性高分子分散液、氧化促進劑、固體電解電容器的製造方法及導電性高分子分散液的製造方法 - Google Patents
固體電解電容器、固體電解質、導電性高分子分散液、氧化促進劑、固體電解電容器的製造方法及導電性高分子分散液的製造方法 Download PDFInfo
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- TW202230411A TW202230411A TW110135190A TW110135190A TW202230411A TW 202230411 A TW202230411 A TW 202230411A TW 110135190 A TW110135190 A TW 110135190A TW 110135190 A TW110135190 A TW 110135190A TW 202230411 A TW202230411 A TW 202230411A
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- Prior art keywords
- conductive polymer
- iron
- absorbance
- acid
- iii
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- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 73
- 239000003990 capacitor Substances 0.000 title claims abstract description 63
- 239000007787 solid Substances 0.000 title claims abstract description 33
- 230000003647 oxidation Effects 0.000 title claims description 26
- 238000007254 oxidation reaction Methods 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000004815 dispersion polymer Substances 0.000 title claims description 11
- 238000002835 absorbance Methods 0.000 claims abstract description 32
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 16
- 230000031700 light absorption Effects 0.000 claims abstract description 15
- -1 iron(III) compound Chemical class 0.000 claims description 54
- 239000006185 dispersion Substances 0.000 claims description 40
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- 238000006116 polymerization reaction Methods 0.000 claims description 19
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- 150000003839 salts Chemical class 0.000 claims description 10
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- 239000000178 monomer Substances 0.000 claims description 9
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- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本發明的目的在於提高導電性高分子的導電度,並提供使用了高導電度的導電性高分子的固體電解電容器。固體電解電容器使用基於導電性高分子的光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由D=(B+C)/A導出的指標D為4以上的導電性高分子。
Description
本發明是有關於一種固體電解電容器、固體電解質、導電性高分子分散液、氧化促進劑及它們的製造方法。
電容器是藉由靜電電容進行電荷的蓄電及放電的被動元件。於超過數十kHz的高頻區域中的資訊處理已一般化的數位設備中,使用電解電容器的例子亦越來越多。例如,採用高頻平滑用途的電解電容器的例子越來越多。因此,於電解電容器中,要求高頻區域中的良好的等效串聯電阻(equivalent series resistance,ESR)。
作為於高頻區域中具有良好的ESR的電容器,有使用了電解液的電解電容器。電解電容器包括如鉭或鋁等般的閥作用金屬作為陽極箔及陰極箔。陽極箔藉由將閥作用金屬製成燒結體或蝕刻箔等形狀而擴面化,且於擴面化的表面具有電介質氧化皮膜層。電解液介於陽極箔與陰極箔之間。電解液與陽極箔的凹凸面密接,作為真正的陰極發揮功能。
近年來,為了進一步降低ESR,逐漸應用使用了包含聚吡咯、聚苯胺、聚噻吩等導電性高分子的固體電解質的固體電解電容器。尤其是,由於摻雜有聚苯乙烯磺酸(Polystyrene Sulfonic Acid,PSS)的聚乙烯二氧噻吩(Polyethylene Dioxythiophene,PEDOT)具有高導電度,因此對固體電解電容器的低ESR化做出了貢獻。
[現有技術文獻]
[專利文獻]
[專利文獻1]國際公開第2007/091656號
[發明所欲解決之課題]
要求藉由具有比PEDOT/PSS高的導電度的導電性高分子來達成更低的ESR化的固體電解電容器。本發明是為了解決所述課題而提出者,其目的在於提高導電性高分子的導電度,並提供使用了高導電度的導電性高分子的固體電解電容器。
[解決課題之手段]
本發明為了解決所述課題,為一種固體電解電容器,其特徵在於包括:電容器元件,是使陽極箔與陰極箔相向而成;以及導電性高分子,附著於所述電容器元件內,基於所述導電性高分子的光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由以下式子導出的指標D為4以上。
(式) D=(B+C)/A
另外,本發明為一種固體電解質,其特徵在於包含基於光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由以下式子導出的指標D為4以上的導電性高分子。藉由固體電解電容器包括該固體電解質,可製作使用了高導電度的導電性高分子的固體電解電容器。
(式) D=(B+C)/A
另外,本發明為一種導電性高分子的分散液,其特徵在於,基於所述導電性高分子的光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由以下式子導出的指標D為4以上。藉由使用該分散液,可製作使用了高導電度的導電性高分子的固體電解電容器。
(式) D=(B+C)/A
該些固體電解電容器與導電性高分子分散液的所述導電性高分子可為摻雜有聚苯乙烯磺酸的聚乙烯二氧噻吩。
另外,本發明為一種生成導電性高分子的化學氧化聚合反應的氧化促進劑,其特徵在於包含水楊酸鐵(III)錯合物。藉由使用該氧化促進劑,可製作使用了高導電度的導電性高分子的固體電解電容器。
另外,本發明為一種固體電解電容器的製造方法,其特徵在於包括:製作使一對電極體相向的電容器元件的步驟;以及高分子附著步驟,使導電性高分子附著於所述電容器元件內,於所述高分子附著步驟中,包括聚合步驟,所述聚合步驟是在包含水楊酸鐵(III)錯合物與構成共軛系高分子的單體的溶液內進行化學氧化聚合,而生成導電性高分子。
於所述高分子附著步驟中,可使藉由所述聚合步驟獲得的分散液含浸於所述電容器元件中。
所述聚合步驟可包括氧化促進劑生成步驟,所述氧化促進劑生成步驟是將硼合二水楊酸鹽或水楊酸鹽與鐵(III)化合物添加至所述溶液中,於所述溶液內生成所述水楊酸鐵(III)錯合物。
另外,本發明為一種導電性高分子的分散液的製造方法,其特徵在於,在包含水楊酸鐵(III)錯合物與構成共軛系高分子的單體的溶液內進行化學氧化聚合。藉由包括使用該分散液的步驟,可製作使用了高導電度的導電性高分子的固體電解電容器。
亦可包括氧化促進劑生成步驟,所述氧化促進劑生成步驟是將硼合二水楊酸鹽或水楊酸鹽與鐵(III)化合物添加至所述溶液中,於所述溶液內生成所述水楊酸鐵(III)錯合物。
[發明的效果]
根據本發明,可實現高導電度的導電性高分子。
以下,對本發明的實施方式進行說明。再者,本發明並不限定於以下說明的實施方式。
固體電解電容器是藉由靜電電容進行電荷的蓄電及放電的被動元件。固體電解電容器包括僅使用固體電解質層的固體電解電容器、以及併用了固體電解質層與電解液的混合電解電容器。另外,該固體電解電容器包括僅於陽極側有意形成電介質氧化皮膜的固體電解電容器、於電極兩者形成電介質氧化皮膜的兩極性固體電解電容器。
固體電解電容器是將電容器元件收容於殼體中並利用封口體密封殼體開口而成。電容器元件包括陽極箔、陰極箔、隔板(separator)及固體電解質層。陽極箔與陰極箔隔著隔板相向。陽極箔的表面形成有電介質氧化皮膜。陰極箔亦根據需要形成有電介質氧化皮膜。固體電解質層介於陽極箔與陰極箔之間,與電介質氧化皮膜密接。該固體電解質層藉由將電容器元件含浸於導電性高分子的分散液中並使其乾燥而形成。
陽極箔及陰極箔是將閥作用金屬作為材料的長條的箔體。閥作用金屬為鋁、鉭、鈮、氧化鈮、鈦、鉿、鋯、鋅、鎢、鉍及銻等。關於純度,陽極箔理想為99.9%以上,陰極箔理想為99%左右以上,亦可包含矽、鐵、銅、鎂、鋅等雜質。
陽極箔作為將閥作用金屬的粉體成形而成的成形體、將成形體燒結而成的燒結體、或對經壓延的箔實施蝕刻處理而成的蝕刻箔,表面被擴面化。擴面結構包括隧道狀的凹坑(pit)、海綿狀的凹坑、或密集的粉體間的空隙。典型而言,擴面結構是藉由於鹽酸等存在鹵素離子的酸性水溶液中施加直流或交流的直流蝕刻或交流蝕刻而形成,或者藉由於芯部蒸鍍或燒結金屬粒子等而形成。關於陰極箔,亦可藉由蒸鍍、燒結或蝕刻而具有擴面結構。
電介質氧化皮膜典型而言為於陽極箔的表層形成的氧化皮膜。例如若陽極箔為鋁箔,則電介質氧化皮膜是使擴面結構氧化而成的氧化鋁。電介質氧化皮膜是藉由於己二酸、硼酸或磷酸等的水溶液中進行電壓施加的化學轉化處理而形成。另外,亦可根據需要於陰極箔的表層藉由化學轉化處理而形成薄的電介質氧化皮膜(1 V~10 V左右)。進而,電介質氧化皮膜亦可使用藉由蒸鍍法而形成包含金屬氮化物、金屬碳化物、金屬碳氮化物的層者,或者表面含有碳者來製作。
隔板可列舉:牛皮紙(kraft)、馬尼拉麻(Manila hemp)、茅草(esparto)、大麻(hemp)、嫘縈(rayon)等纖維素及該些的混合紙、聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸乙二酯、該些的衍生物等聚酯系樹脂、聚四氟乙烯系樹脂、聚偏二氟乙烯系樹脂、維尼綸(vinylon)系樹脂、脂肪族聚醯胺、半芳香族聚醯胺、全芳香族聚醯胺等聚醯胺系樹脂、聚醯亞胺系樹脂、聚乙烯樹脂、聚丙烯樹脂、三甲基戊烯樹脂、聚苯硫醚樹脂、丙烯酸樹脂、聚乙烯醇樹脂等,可將該些樹脂單獨或混合使用。
固體電解質層包含固體電解質而成,固體電解質包含導電性高分子。導電性高分子是將聚苯乙烯磺酸(PSS)作為摻雜劑取入的共軛系高分子。所謂作為摻雜劑取入,是指共軛系高分子與摻雜劑分別帶有正電荷及負電荷且共軛系高分子成為極化子或雙極子的狀態,導電性高分子顯現出導電性。
導電性高分子具有由下式1導出的指標D為4以上的光吸收光譜。光吸收光譜只要可藉由紫外線可見分光法(UV-vis)獲得即可。式1中,A為585 nm的吸光度,B為800 nm的吸光度,C為1200 nm的吸光度。導電性高分子藉由處於該指標D滿足4以上的光吸收光譜所表示的摻雜狀態,固體電解質層的導電度變高,將固體電解電容器的ESR抑制得低。
(式1)
D=(B+C)/A
導電性高分子較佳為凝聚體被解開至粒徑達到0.1 μm以下的程度。於90%的導電性高分子通過0.1 μm的網眼的過濾器的情況下,導電性高分子的粒徑為0.1 μm以下。於導電性高分子為該粒徑時,於電介質氧化皮膜的凹坑內或空隙內可附著很多導電性高分子,固體電解電容器於120 Hz等低頻區域中的Cap(靜電電容)、ESR及tanδ(損耗正切)亦變得良好。
作為共軛系高分子,可無特別限定地使用公知者。例如可列舉:聚吡咯、聚噻吩、聚呋喃、聚苯胺、聚乙炔、聚伸苯、聚伸苯伸乙烯(polyphenylene vinylene)、多並苯(polyacene)、聚噻吩伸乙烯等。該些共軛系高分子可單獨使用,亦可組合兩種以上,進而亦可為兩種以上單體的共聚物。
於所述共軛系高分子中,較佳為噻吩或其衍生物聚合而成的共軛系高分子,較佳為3,4-伸乙基二氧噻吩(即2,3-二氫噻吩並[3,4-b][1,4]二噁英)、3-烷基噻吩、3-烷氧基噻吩、3-烷基-4-烷氧基噻吩、3,4-烷基噻吩、3,4-烷氧基噻吩或該些的衍生物聚合而成的共軛系高分子。作為噻吩衍生物,較佳為選自於3位及4位具有取代基的噻吩中的化合物,噻吩環的3位及4位的取代基可與3位及4位的碳一同形成環。烷基或烷氧基的碳數適合為1~16。
作為烷基或烷氧基的碳數為1~16的噻吩衍生物,亦可為於3,4-伸乙基二氧噻吩上加成有烷基的烷基化伸乙基二氧噻吩,例如可列舉:甲基化伸乙基二氧噻吩(即2-甲基-2,3-二氫-噻吩並〔3,4-b〕〔1,4〕二噁英)、乙基化伸乙基二氧噻吩(即2-乙基-2,3-二氫-噻吩並〔3,4-b〕〔1,4〕二噁英)等。
尤其是,作為共軛系高分子,尤佳為被稱為EDOT的3,4-乙烯二氧噻吩的聚合物、即被稱為PEDOT的聚(3,4-乙烯二氧噻吩)。PEDOT於導電性高分子中亦顯示出優異的導電度,且顯示出高耐熱性。
該固體電解質層藉由使分散液含浸於電容器元件中而形成。分散液是分散有具有指標D為4以上的光吸收光譜的導電性高分子的導電性高分子分散液。藉由使分散液含浸於電容器元件中,該導電性高分子附著於電介質氧化皮膜,於電容器元件形成包含導電性高分子的固體電解質層。為了促進向電容器元件的含浸,亦可根據需要而實施減壓處理或加壓處理。含浸步驟可重覆多次。
再者,若可於電容器元件形成固體電解質層,則亦可應用除了使製造完畢的分散液含浸於電容器元件中的以外的方法。例如,亦可使分散液附著於選自陽極箔、或陰極箔及隔板中的一個以上的構件,並去除溶媒的一部分,使用該構件來構成電容器元件。
該分散液是藉由將構成共軛系高分子的單體、作為摻雜劑的聚苯乙烯磺酸(PSS)、以及氧化促進劑添加至溶媒中並進行化學氧化聚合而生成。化學氧化聚合的溫度並無嚴格的限制,但一般為0℃~60℃的範圍內。聚合時間一般為10分鐘~30小時的範圍內。可藉由進行超濾、攪拌、超濾及濃度調整等來對分散液進行精製。進而,可於分散液中適宜加入添加劑,另外亦可進行分散液的pH調整。亦可藉由陽離子交換及陰離子交換等精製方法自分散液中去除氧化促進劑及殘留單體。
氧化促進劑是水楊酸鐵(III)錯合物。水楊酸鐵(III)錯合物是水楊酸根離子與鐵(III)離子配位而成的螯合物錯合物,配位體所具有的鄰位的羥基及羧基與鐵(III)離子配位鍵結。藉由與該氧化促進劑一同添加構成共軛系高分子的單體,進行化學氧化聚合,而生成指標D為4以上的光吸收光譜的導電性高分子。
該氧化促進劑是藉由將鐵(III)化合物及水楊酸鹽或硼合二水楊酸鹽混合至溶媒中而生成。水楊酸是相對於苯甲酸的羧基而鄰位的氫原子被取代為羥基的鄰羥基苯甲酸。該水楊酸與鐵(III)離子一同形成作為氧化促進劑的錯合物。再者,間羥基苯甲酸鹽或對羥基苯甲酸鹽無法形成作為氧化促進劑的錯合物。
另外,為了製造氧化促進劑,使水楊酸鹽或硼合二水楊酸鹽溶解於作為溶媒的水中。即便向溶媒中添加水楊酸或硼合二水楊酸而並非添加鹽,亦無法形成作為氧化促進劑的錯合物。水楊酸鹽及硼合二水楊酸鹽只要根據水楊酸鐵(III)錯合物的配位數以化學計量比添加至鐵(III)化合物中即可。或者,由於鐵(III)化合物單獨作為氧化促進劑發揮功能,因此亦可比化學計量比過剩地添加鐵(III)化合物。
作為構成水楊酸鹽及硼合二水楊酸鹽的鹽,例如可列舉銨鹽、四級銨鹽、四級化脒鹽、胺鹽、鈉鹽、鉀鹽等。作為四級銨鹽的四級銨離子,可列舉四甲基銨、三乙基甲基銨、四乙基銨等。作為四級化脒鹽,可列舉乙基二甲基咪唑鎓、四甲基咪唑鎓等。作為胺鹽,可列舉一級胺、二級胺、三級胺的鹽。作為一級胺,可列舉甲胺、乙胺、丙胺等,作為二級胺,可列舉二甲胺、二乙胺、乙基甲胺、二丁胺等,作為三級胺,可列舉三甲胺、三乙胺、三丁胺、乙基二甲胺、乙基二異丙胺等。
作為鐵(III)化合物,無機酸鐵可列舉硫酸鐵(III)、氯化鐵(III)、過氯酸鐵(III)、硝酸鐵(III)、磷酸鐵(III)、六氰酸鐵(III)等。另外,作為有機酸鐵,可列舉檸檬酸鐵(III)、草酸鐵(III)等羧酸系的鐵、甲苯磺酸鐵(III)、烷基苯磺酸鐵(III)、烷基萘磺酸鐵(III)、蒽醌磺酸(III)等磺酸系的鐵。該些鐵(III)化合物可混合多個來使用。
再者,除了水楊酸鐵(III)錯合物以外,還可併用其他氧化促進劑。作為其他氧化促進劑,較佳為無機酸及有機酸的鐵鹽、過硫酸鹽。例如可列舉:氯化鐵六水合物、無水氯化鐵、硝酸鐵九水合物、硝酸鐵、硫酸鐵、硫酸鐵n水合物、硫酸鐵銨十二水合物、過氯酸鐵n水合物、四氟硼酸鐵、氯化銅、硫酸銅、四氟硼酸銅、四氟硼酸亞硝、過硫酸銨、過硫酸鈉、過硫酸鉀、過碘酸鉀、過氧化氫、臭氧、六氰基鐵鉀、硫酸四銨鈰(IV)二水合物、溴、碘、十二烷基苯磺酸鐵、對甲苯磺酸鐵、萘磺酸鐵、蒽醌磺酸鐵、過碘酸、碘酸等。
就降低高頻區域中的ESR的觀點而言,構成共軛系高分子的單體不需要特別設定濃度的限制,但較佳為以1 mM以上且6.25 mM以下的濃度添加至分散液中。於為該範圍內時,導電性高分子難以凝聚,導電性高分子的粒徑成為0.1 μm以下。另外,於為該範圍內時,耐熱性提高,即便固體電解質暴露於高溫環境下,亦可抑制電容器的各特性的劣化。
作為分散液的溶媒,只要是分散有導電性高分子的粒子或粉末者即可。例如,可使用水或有機溶媒或它們的混合物作為溶媒。作為有機溶媒,可較佳地例示極性溶媒、酮類、醇類、酯類、烴類、碳酸酯化合物、醚化合物、鏈狀醚類、雜環化合物、腈化合物等。
作為極性溶媒,可列舉N-甲基-2-吡咯啶酮、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、二甲基亞碸等。作為酮類,可列舉丙酮。作為醇類,可列舉甲醇、乙醇、丙醇、丁醇等。作為酯類,可列舉乙酸乙酯、乙酸丙酯、乙酸丁酯、甲酸乙酯等。作為烴類,可列舉戊烷、己烷、庚烷、苯、甲苯、二甲苯等。作為碳酸酯化合物,可列舉碳酸乙烯酯、碳酸丙烯酯等。作為醚化合物,可列舉二噁烷、二乙醚、四氫呋喃等。作為鏈狀醚類,可列舉乙二醇二烷基醚、丙二醇二烷基醚、聚乙二醇二烷基醚、聚丙二醇二烷基醚等。作為雜環化合物,可列舉3-甲基-2-噁唑啶酮等。作為腈化合物,可列舉乙腈、戊二腈、甲氧基乙腈、丙腈、苄腈等。
作為添加劑,分散液中可含有多元醇。作為多元醇,可列舉:山梨糖醇、乙二醇、二乙二醇、三乙二醇、分子量為200左右的聚乙二醇、聚氧乙二醇、丙三醇、聚氧乙烯甘油、木糖醇、赤藻糖、甘露醇、二季戊四醇、季戊四醇、或該些的兩種以上的組合。多元醇由於沸點高,因此於乾燥步驟後亦可殘留於固體電解質層中,可提高導電性,可獲得ESR減低或耐電壓提高效果。進而亦可包含其他化合物。例如亦可添加有機黏合劑、界面活性劑、消泡劑、偶合劑、抗氧化劑、紫外線吸收劑等慣用的添加物。
分散液較佳為自弱酸性調整為中性。作為pH調整劑,並無特別限制,可列舉氨及氫氧化鈉等。於pH為弱酸性至中性的範圍內時,包含將聚苯乙烯磺酸(PSS)作為摻雜劑取入的共軛系高分子的導電性高分子的凝聚被解開,導電性高分子的粒徑成為0.1 μm以下。即,PSS的磺基所具有的氫原子進行氫鍵結,引起導電性高分子的凝聚。但是,由於該氫原子藉由中和反應被置換為鈉或氨等,或者由於處於難以進行氫鍵結的弱酸性環境下,不會引起氫鍵結,可抑制導電性高分子的凝聚。其中,若處於鹼側,則容易自共軛系高分子中產生脫摻雜,因此欠佳。
使電容器元件的空隙中含浸電解液,於併用電解液的固體電解電容器的情況下,電解液是於溶媒中添加了陰離子成分及陽離子成分的溶液。陰離子成分及陽離子成分典型而言為有機酸的鹽、無機酸的鹽、或者有機酸與無機酸的複合化合物的鹽,藉由解離為陰離子成分與陽離子成分的離子解離性鹽而添加至溶媒中。作為陰離子成分的酸及作為陽離子成分的鹼可分別添加至溶媒中。另外,電解液中,陰離子成分或陽離子成分、陰離子成分與陽離子成分兩者可不包含於溶媒中。
電解液的溶媒並無特別限定,可使用質子性的有機極性溶媒或非質子性的有機極性溶媒。作為質子性的有機溶媒,可列舉一元醇類、多元醇類及氧基醇化合物類等。作為一元醇類,可列舉:乙醇、丙醇、丁醇、戊醇、己醇、環丁醇、環戊醇、環己醇、苄醇等。作為多元醇類及氧基醇化合物類,可列舉:乙二醇、二乙二醇、丙二醇、甘油、甲基溶纖劑、乙基溶纖劑、甲氧基丙二醇、二甲氧基丙醇、聚乙二醇或聚氧乙烯甘油等多元醇的環氧烷加成物等。
作為非質子性的有機極性溶媒,可使用碸系、醯胺系、內酯類、環狀醯胺系、腈系、亞碸系等。作為碸系,可列舉:二甲基碸、乙基甲基碸、二乙基碸、環丁碸、3-甲基環丁碸、2,4-二甲基環丁碸等。作為醯胺系,可列舉:N-甲基甲醯胺、N,N-二甲基甲醯胺、N-乙基甲醯胺、N,N-二乙基甲醯胺、N-甲基乙醯胺、N,N-二甲基乙醯胺、N-乙基乙醯胺、N,N-二乙基乙醯胺、六甲基磷醯胺等。作為內酯類、環狀醯胺系,可列舉:γ-丁內酯、γ-戊內酯、δ-戊內酯、N-甲基-2-吡咯啶酮、碳酸乙烯酯、碳酸丙烯酯、碳酸丁烯酯、碳酸異丁烯酯等。作為腈系,可列舉乙腈、3-甲氧基丙腈、戊二腈等。作為亞碸系,可列舉二甲基亞碸等。
作為溶質的成為陰離子成分的有機酸可列舉:草酸、琥珀酸、戊二酸、庚二酸、辛二酸、癸二酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、馬來酸、己二酸、苯甲酸、甲苯甲酸、庚酸、丙二酸、1,6-癸烷二羧酸、1,7-辛烷二羧酸、壬二酸、間苯二酚酸、2,4,6-三羥基苯甲酸(phloroglucinic acid)、沒食子酸、龍膽酸(gentisic acid)、原兒茶酸(protocatechuic acid)、兒茶酚甲酸(pyrocatechuic acid)、偏苯三甲酸、均苯四甲酸等羧酸,或酚類、磺酸。另外,作為無機酸,可列舉:硼酸、磷酸、亞磷酸、次磷酸、碳酸、矽酸等。作為有機酸與無機酸的複合化合物,可列舉:硼合二水楊酸、硼合二草酸、硼合二乙醇酸、硼合二丙二酸、硼合二琥珀酸、硼合二己二酸、硼合二壬二酸、硼合二苯甲酸、硼合二馬來酸、硼合二乳酸、硼合二蘋果酸、硼合二酒石酸、硼合二檸檬酸、硼合二鄰苯二甲酸、硼合二(2-羥基)異丁酸、硼合二間苯二酚酸、硼合二甲基水楊酸、硼合二萘甲酸、硼合二苦杏仁酸及硼合二(3-羥基)丙酸等。
另外,作為有機酸、無機酸以及有機酸與無機酸的複合化合物的至少一種的鹽,例如可列舉銨鹽、四級銨鹽、四級化脒鹽、胺鹽、鈉鹽、鉀鹽等。作為四級銨鹽的四級銨離子,可列舉四甲基銨、三乙基甲基銨、四乙基銨等。作為四級化脒鹽,可列舉乙基二甲基咪唑鎓、四甲基咪唑鎓等。作為胺鹽,可列舉一級胺、二級胺、三級胺的鹽。作為一級胺,可列舉甲胺、乙胺、丙胺等,作為二級胺,可列舉二甲胺、二乙胺、乙基甲胺、二丁胺等,作為三級胺,可列舉三甲胺、三乙胺、三丁胺、乙基二甲胺、乙基二異丙胺等。
進而,亦可於液體中添加其他添加劑。作為添加劑,可列舉:硼酸與多糖類(甘露醇、山梨糖醇等)的錯合化合物、硼酸與多元醇的錯合化合物、硼酸酯、硝基化合物(鄰硝基苯甲酸、間硝基苯甲酸、對硝基苯甲酸、鄰硝基酚、間硝基酚、對硝基酚、對硝基苄醇等)、磷酸酯等。該些可單獨使用,亦可將兩種以上組合使用。
[實施例]
以下,基於實施例更詳細地說明本發明的導電性高分子的分散液及使用該分散液製作的電解電容器。再者,本發明並不限定於以下說明的實施例。
(分散液)
如以下般製作實施例1及實施例2以及比較例1至比較例3的分散液。所有實施例及所有比較例的分散液的製作中共通的事項如以下般。即,導電性高分子的分散液的溶媒設為500 ml的水。於溶媒中添加2.5 mmol的EDOT(3,4-乙烯二氧噻吩)、5 mmol的聚苯乙烯磺酸(PSS)、3 mmol的過硫酸銨(Ammonium Persulfate,APS)、2 mmol的硫酸鐵[Fe
2(SO
4)
3]、以及下表1中所示的添加物。
(表1)
添加物 | 添加量/mmol | |
實施例1 | 硼合二水楊酸銨 | 1.5 |
實施例2 | 水楊酸銨 | 1.5 |
比較例1 | 無 | 0 |
比較例2 | 鄰苯二甲酸銨 | 5 |
比較例3 | 苯甲酸銨 | 5 |
如表1所示,實施例1中,進一步向溶媒中添加1.5 mmol的硼合二水楊酸銨。實施例2中,進一步向溶媒中添加1.5 mmol的水楊酸銨。比較例1中,無進一步添加的添加物。比較例2中,進一步向溶媒中添加5 mmol的鄰苯二甲酸銨。比較例3中,進一步向溶媒中添加5 mmol的苯甲酸銨。
此處,關於實施例1及實施例2的溶液,於將硫酸鐵及硼合二水楊酸銨或水楊酸銨混合時呈紫紅色。該溶液的顏色變化表示硫酸鐵的鐵離子與硼合二水楊酸銨或水楊酸銨的水楊酸根離子進行錯合形成,生成了水楊酸鐵(III)錯合物。比較例2及比較例3中未發現溶液的顏色變化,確認了硫酸鐵的鐵離子與鄰苯二甲酸或苯甲酸未進行錯合形成。
將該溶液於0℃~5℃的溫度環境下攪拌並放置一晚。於放置一晚後,進行超濾,藉由噴射混合進行分散處理。於分散處理後,進一步進行超濾,以成為導電性高分子的濃度為約2 wt%的分散液的方式調整溶媒的量。
(光吸收光譜的獲取)
利用水稀釋實施例1及實施例2以及比較例1至比較例3中製作的分散液,以使分散液內的固體成分濃度成為0.04 wt%,利用UV-vis測定照射光的波長與吸光度的關係。再者,作為分散介質的水的光吸收光譜亦作為空白藉由UV-vis進行了測定。
(導電度的測定)
以實施例1及實施例2以及比較例1至比較例3中製作的分散液(A)與乙二醇(B)的體積比成為A:B=70:30的方式,於分散液中混合乙二醇,向玻璃板滴加100 μl的混合液,並使其乾燥,藉此於玻璃板上使導電性高分子成膜。利用四探針法測定該導電性高分子的膜的導電度。再者,相同的玻璃板的導電度亦作為空白利用四探針法進行測定。
(測定結果)
下表2中示出實施例1及實施例2以及比較例1至比較例3中獲得的光吸收光譜中的585 nm的吸光度、800 nm的吸光度及1200 nm的吸光度。進而將由該些吸光度計算出的指標D示於表2中。另外,將藉由四探針法獲得的導電度示於表2中。
(表2)
585 nm的吸光度A | 800 nm的吸光度B | 1200 nm的吸光度C | 指標D(D=(B+C)/A) | 導電度/Scm -1 | |
實施例1 | 1.47 | 2.38 | 4.11 | 4.41 | 1.2×10 1 |
實施例2 | 1.30 | 2.0 | 3.50 | 4.23 | 6.1×10 -1 |
比較例1 | 1.11 | 1.80 | 2.40 | 3.78 | 2.1×10 -2 |
比較例2 | 1.13 | 1.68 | 1.93 | 3.19 | <1×10 -7 |
比較例3 | 1.10 | 1.59 | 2.22 | 3.46 | 8.5×10 -5 |
如表2所示,確認了實施例1及實施例2的分散液中所含的導電性高分子的光吸收光譜的指標D為4以上。另一方面,比較例1至比較例3的分散液中所含的導電性高分子的指標D小於4。而且,確認了指標D為4以上的實施例1及實施例2與比較例1至比較例3相比,導電度大幅提高,指標D為4以上的光譜的導電性高分子顯示出高導電度。
藉由實施例1及實施例2的分散液呈紫紅色,確認了於實施例1及實施例2的分散液中生成了水楊酸鐵(III)。另一方面,由於比較例1至比較例3的分散液無顏色變化,因此確認了比較例1至比較例3的分散液中不含水楊酸鐵(III)或其他錯合物。若結合該事實與指標D的結果及導電度,則可得出結論:水楊酸鐵(III)作為氧化促進劑發揮作用,指標D為4以上的實施例1及實施例2與比較例1至比較例3相比,導電度大幅提高。
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Claims (11)
- 一種固體電解電容器,其特徵在於包括: 電容器元件,是使陽極箔與陰極箔相向而成;以及 導電性高分子,附著於所述電容器元件內, 基於所述導電性高分子的光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由以下式子導出的指標D為4以上, (式) D=(B+C)/A。
- 如請求項1所述的固體電解電容器,其中所述導電性高分子為摻雜有聚苯乙烯磺酸的聚乙烯二氧噻吩。
- 一種固體電解質,其特徵在於包含基於光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由以下式子導出的指標D為4以上的導電性高分子, (式) D=(B+C)/A。
- 一種導電性高分子分散液,是導電性高分子的分散液,其特徵在於, 基於所述導電性高分子的光吸收光譜的585 nm的吸光度A、800 nm的吸光度B及1200 nm的吸光度C而由以下式子導出的指標D為4以上, (式) D=(B+C)/A。
- 如請求項4所述的導電性高分子分散液,其中所述導電性高分子為摻雜有聚苯乙烯磺酸的聚乙烯二氧噻吩。
- 一種氧化促進劑,是生成導電性高分子的化學氧化聚合反應的氧化促進劑,其特徵在於, 包含水楊酸鐵(III)錯合物。
- 一種固體電解電容器的製造方法,其特徵在於包括: 製作使一對電極體相向的電容器元件的步驟;以及 高分子附著步驟,使導電性高分子附著於所述電容器元件內, 於所述高分子附著步驟中,包括聚合步驟,所述聚合步驟是在包含水楊酸鐵(III)錯合物與構成共軛系高分子的單體的溶液內進行化學氧化聚合,而生成導電性高分子。
- 如請求項7所述的固體電解電容器的製造方法,其中於所述高分子附著步驟中,使藉由所述聚合步驟獲得的分散液含浸於所述電容器元件中。
- 如請求項7或請求項8所述的固體電解電容器的製造方法,其中所述聚合步驟包括氧化促進劑生成步驟,所述氧化促進劑生成步驟是將硼合二水楊酸鹽或水楊酸鹽與鐵(III)化合物添加至所述溶液中,於所述溶液內生成所述水楊酸鐵(III)錯合物。
- 一種導電性高分子分散液的製造方法,是導電性高分子的分散液的製造方法,其特徵在於, 在包含水楊酸鐵(III)錯合物與構成共軛系高分子的單體的溶液內進行化學氧化聚合。
- 如請求項10所述的導電性高分子分散液的製造方法,包括氧化促進劑生成步驟,所述氧化促進劑生成步驟是將硼合二水楊酸鹽或水楊酸鹽與鐵(III)化合物添加至所述溶液中,於所述溶液內生成所述水楊酸鐵(III)錯合物。
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