CN115989141A - 有机导电膜的制造方法、有机导电膜以及层叠体 - Google Patents
有机导电膜的制造方法、有机导电膜以及层叠体 Download PDFInfo
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- CN115989141A CN115989141A CN202180052174.0A CN202180052174A CN115989141A CN 115989141 A CN115989141 A CN 115989141A CN 202180052174 A CN202180052174 A CN 202180052174A CN 115989141 A CN115989141 A CN 115989141A
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Abstract
一种有机导电膜的制造方法,包括:制备包含酸系有机导电性高分子、碱中和剂以及液体介质且在25℃的pH为4.0~6.5的涂液的工序;将涂液涂布在基材层上的工序;以及从所涂布的涂液中除去液体介质的工序。
Description
技术领域
本公开涉及有机导电膜的制造方法、有机导电膜以及层叠体。
背景技术
近年来,液晶显示装置、电致发光显示器、太阳能电池、触摸面板等广泛普及,在这些当中,作为透明电极,使用在膜上层叠ITO(氧化铟锡)而成的电极。然而,作为ITO的材料的铟存在世界性资源枯竭和安全性的担忧,正在研究作为替代的有机系材料。作为这样的有机系材料,可以列举出π共轭系导电性高分子,具体而言,可以列举出聚噻吩系导电性高分子。
关于形成π共轭系导电性高分子膜的技术,已知使用包含π共轭系导电性高分子的导电性高分子溶液(例如,参照专利文献1)。
现有技术文献
专利文献
专利文献1:日本特开平7-105718号公报
发明内容
本发明所要解决的课题
然而,在根据专利文献1制备溶液的情况下,包含酸系有机导电性高分子的溶液因其组成而有时表现出强酸性。在这种情况下,从安全性确保和加工装置的腐蚀抑制等观点来看,考虑使用中和剂等来将溶液的pH调节至中性附近。然而,根据本发明人的见解,使用这样调节了pH的溶液形成的导电性的高分子层的耐光性不充分。
本公开是鉴于上述情况而完成的,目的在于提供耐光性优异的有机导电膜的制造方法。本公开的另一个目的在于提供耐光性优异的有机导电膜。
用于解决课题的手段
本发明人经过深入研究,结果表明:残留在由包含酸系有机导电性高分子的溶液形成的导电层中的来自碱中和剂的成分的量对耐光性产生影响。在这一见解下,本发明人最终完成了本发明。
本公开的一个方面涉及的有机导电膜的制造方法包括:制备包含酸系有机导电性高分子、碱中和剂以及液体介质且在25℃的pH为4.0~6.5的涂液的工序;将涂液涂布在基材层上的工序;以及从所涂布的涂液中除去液体介质的工序。通过使用这样调节了pH的涂液,如后所述可以适当控制酸系有机导电性高分子层中的来自碱中和剂的阳离子含量,结果能够制造耐光性优异的有机导电膜。根据本发明人的研究可知:这样,除了pH不会过高、即来自碱中和剂的阳离子含量没有过多以外,pH不会过低、即来自碱中和剂的阳离子含量不会过少也是重要的。
在制造方法的一个方式中,酸系有机导电性高分子可以包含聚噻吩系导电性高分子。
在制造方法的一个方式中,碱中和剂可以包含氨水。
本公开的一个方面涉及的有机导电膜具备基材层和基材层上的酸系有机导电性高分子层,酸系有机导电性高分子层中的来自碱中和剂的阳离子含量为0.5~5.0mg/cm3。通过将酸系有机导电性高分子层中的来自碱中和剂的阳离子含量设在0.5~5.0mg/cm3的范围内,可以得到耐光性优异的有机导电膜。
在有机导电膜的一个方式中,酸系有机导电性高分子可以包含聚噻吩系导电性高分子。
在有机导电膜的一个方式中,来自碱中和剂的阳离子可以包含铵离子。
在有机导电膜的一个方式中,基材层可以包含树脂基材或玻璃基材。
在一个方式中,有机导电膜可以用作电磁波抑制片的电阻覆膜或电子器件中的电路材料。
本发明的效果
根据本公开,可以提供耐光性优异的有机导电膜的制造方法。另外,根据本公开,可以提供耐光性优异的有机导电膜。这样的有机导电膜可以通过上述的制造方法得到。
附图说明
[图1]图1是一个实施方式涉及的有机导电膜的示意性剖面图。
具体实施方式
以下,对本发明的实施方式进行详细地说明。但是,本发明不限于以下的实施方式。
<有机导电膜>
图1是一个实施方式涉及的有机导电膜的示意性剖面图。有机导电膜10具备基材层1和基材层1上的酸系有机导电性高分子层2。
(基材层)
基材层作为有机导电膜的基材而发挥功能。作为基材层的材料,可以列举出树脂和玻璃。即,基材层可以包含树脂基材或玻璃基材,也可以为树脂基材或玻璃基材。
作为树脂,没有特别地限定,例如可以列举出:聚对苯二甲酸乙二醇酯(PET)、聚对苯二甲酸丁二醇酯(PBT)、聚萘二甲酸乙二醇酯、改性聚酯等聚酯树脂;聚乙烯(PE)树脂、聚丙烯(PP)树脂、环状烯烃树脂等聚烯烃树脂;聚氯乙烯、聚偏二氯乙烯等乙烯基系树脂;聚乙烯醇缩丁醛(PVB)等聚乙烯醇缩醛树脂;聚醚醚酮(PEEK)树脂;聚砜(PSF)树脂;聚醚砜(PES)树脂;聚碳酸酯(PC)树脂;聚酰胺树脂;聚酰亚胺树脂;聚苯乙烯树脂;丙烯酸树脂;三醋酸纤维素(TAC)树脂等。从易得性、价格等观点来看,树脂可以为PET、PBT等聚酯树脂或PP等聚烯烃树脂。
作为玻璃,没有特别地限定,可以列举出:钠钙玻璃、铅玻璃、硼硅酸盐玻璃、石英玻璃等。从易得性、价格等观点来看,玻璃可以为钠钙玻璃。
基材层可以包含一层由这些材料形成的层,也可以包含多层。在基材层由多层构成(为层叠体)的情况下,可以将树脂基材彼此组合使用,也可以组合使用树脂基材和玻璃基材。作为树脂基材彼此的组合,例如可以列举出PP层/PET层构成、PP层/PBT层构成。
对基材层的厚度没有特别地限定,但是从根据用途的透明性和强度的观点来看,例如可以设为10~200μm、也可以为25~75μm。另外,从涂液的涂布性、与高分子层的密合性等观点来看,也可以根据需要对基材层的表面实施电晕处理或易粘接处理。
基材层对于可见光区域中的波长的电磁波可以是透过性的、也可以是不透过性的,根据有机导电膜的规格进行适当选择。例如,在对有机导电膜要求对于可见光区域中的波长的电磁波的透过性的情况下,可以选择透过性的基材层。另外,在对基材要求图案或木纹风格的设计的情况下,可以对基材层实施印刷或在基材层的表面形成凹凸。
(酸系有机导电性高分子层)
酸系有机导电性高分子层具有导电性,包含酸系有机导电性高分子。在本说明书中,酸系有机导电性高分子是指包含π共轭系导电性高分子、和相对于π共轭系导电性高分子的多阴离子掺杂剂的导电性复合体。作为π共轭系导电性高分子,没有特别地限定,可以列举出:聚噻吩、聚吡咯、聚苯胺、聚乙炔、聚亚苯基亚乙烯(polyphenylene vinylene)、聚萘以及它们的衍生物等。这些当中,从透明性、导电性、稳定性等观点来看,π共轭系导电性高分子特别可以为聚噻吩系导电性高分子。
作为聚噻吩系导电性高分子,例如可以列举出:聚噻吩、聚(3-甲基噻吩)、聚(3-乙基噻吩)、聚(3-丙基噻吩)、聚(3-丁基噻吩)、聚(3-己基噻吩)、聚(3-庚基噻吩)、聚(3-辛基噻吩)、聚(3-癸基噻吩)、聚(3-十二烷基噻吩)、聚(3-十八烷基噻吩)、聚(3-溴噻吩)、聚(3-氯噻吩)、聚(3-碘噻吩)、聚(3-氰基噻吩)、聚(3-苯基噻吩)、聚(3,4-二甲基噻吩)、聚(3,4-二丁基噻吩)、聚(3-羟基噻吩)、聚(3-甲氧基噻吩)、聚(3-乙氧基噻吩)、聚(3-丁氧基噻吩)、聚(3-己氧基噻吩)、聚(3-庚氧基噻吩)、聚(3-辛氧基噻吩)、聚(3-癸氧基噻吩)、聚(3-十二烷氧基噻吩)、聚(3-十八烷氧基噻吩)、聚(3,4-二羟基噻吩)、聚(3,4-二甲氧基噻吩)、聚(3,4-二乙氧基噻吩)、聚(3,4-二丙氧基噻吩)、聚(3,4-二丁氧基噻吩)、聚(3,4-二己氧基噻吩)、聚(3,4-二庚氧基噻吩)、聚(3,4-二辛氧基噻吩)、聚(3,4-二癸氧基噻吩)、聚(3,4-二十二烷氧基噻吩)、聚(3,4-亚乙二氧基噻吩)、聚(3,4-亚丙二氧基噻吩)、聚(3,4-亚丁二氧基噻吩)、聚(3-甲基-4-甲氧基噻吩)、聚(3-甲基-4-乙氧基噻吩)、聚(3-羧基噻吩)、聚(3-甲基-4-羧基噻吩)、聚(3-甲基-4-羧基乙基噻吩)、聚(3-甲基-4-羧基丁基噻吩)。从导电性、化学稳定性、生产性等观点来看,聚噻吩系导电性高分子可以为聚(3,4-亚乙二氧基噻吩)。
聚噻吩系导电性高分子可以单独使用1种或2种以上组合使用。
酸系有机导电性高分子层包含相对于π共轭系导电性高分子的多阴离子掺杂剂。由此,可以提高酸系有机导电性高分子层的导电性。作为多阴离子掺杂剂,例如可以列举出:链烷磺酸、聚苯乙烯磺酸、聚乙烯硫酸、聚乙烯磺酸、聚芳基磺酸、聚丙烯磺酸、聚甲基丙烯磺酸、聚(2-丙烯酰胺-2-甲基丙磺酸)、聚异戊二烯磺酸、聚甲基丙烯酸磺乙酯、聚(4-甲基丙烯酸磺丁酯)、聚甲基丙烯酰氧基苯磺酸等具有磺基的高分子酸;对甲苯磺酸、十二烷基苯磺酸等具有磺基的有机酸等。从化学稳定性和导电性的观点来看,多阴离子掺杂剂可以为聚苯乙烯磺酸。
多阴离子掺杂剂可以单独使用1种或2种以上组合使用。
至少一部分的聚噻吩系导电性高分子与至少一部分的多阴离子掺杂剂在层内形成导电性复合体。从透明性、导电性等观点来看,导电性复合体可以为聚(3,4-亚乙二氧基噻吩)(PEDOT)与聚苯乙烯磺酸(PSS)的复合体,即聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)(PEDOT-PSS)。
只要不显著地损害预期效果,则酸系有机导电性高分子层也可以包含除聚噻吩系导电性高分子和多阴离子掺杂剂以外的其他成分(例如粘结剂等)。在这种情况下,酸系有机导电性高分子层中的聚噻吩系导电性高分子和多阴离子掺杂剂的合计量可以设为50质量%以上、可以为80质量%以上、可以为90质量%以上。
对酸系有机导电性高分子层的厚度没有特别地限定,例如可以设为10nm~1μm、也可以为200~600nm。
如后所述,酸系有机导电性高分子层的形成可以通过将包含酸系有机导电性高分子和碱中和剂且在25℃的pH为4.0~6.5的涂液涂布在基材层上来进行。从保持优异的耐光性的观点来看,酸系有机导电性高分子层中的来自碱中和剂的阳离子含量为0.5~5.0mg/cm3、可以为3.0~5.0mg/cm3、可以为4.5~5.0mg/cm3。据推测,酸系有机导电性高分子层包含一定量以上的阳离子的原因是,由于与酸系有机导电性高分子之间产生氢键等而使阳离子被捕获,在除去液体介质之后也残留在层中。
阳离子含量可以通过离子色谱法进行测定。具体而言,将有机导电膜放入萃取溶剂(超纯水)中,在25℃环境下静置24小时。将静置后的萃取溶剂用超纯水稀释50倍后,通过离子色谱法进行阳离子的定量。根据定量结果,可以算出残留在酸系有机导电性高分子层中的阳离子的含量。
来自碱中和剂的阳离子可以包含铵离子。在这种情况下,在利用离子色谱法的测定中,存在于酸系有机导电性高分子层中的铵离子量可以设为0.5~5.0mg/cm3、可以为3.0~5.0mg/cm3、可以为4.5~5.0mg/cm3。
酸系有机导电性高分子层的耐光性优异,这即意味着表面电阻难以随着时间而上升。在利用4端子法的测定中,由下式表示的酸系有机导电性高分子层的表面电阻变化可以为4.0×102以下、可以为3.0×102以下。
表面电阻变化=耐光性试验后的表面电阻值/耐光性试验前的表面电阻值
其中,耐光性试验是指氙型促进耐光性试验(条件:放射照度60W/m2、BPT温度63℃、槽内温度40℃、槽内湿度50%rh、试验时间500小时)。
有机导电膜可以用作电磁波抑制片的电阻覆膜或电子器件中的电路材料,但是不限于此。需要说明的是,作为电磁波抑制片,有机导电膜可以如日本专利第6523563号公报记载的电阻覆膜层那样使用。另外,作为电子器件,有机导电膜可以如日本特开2005-71929号公报记载的正孔输送层那样使用。
<电磁波抑制片>
电磁波抑制片可以认为是具备有机导电膜、介电层、以及电磁波遮蔽层的层叠体。对电磁波抑制片的制造方法没有特别地限定,例如可以列举出以下的方法。
(1)将有机导电膜粘接在层叠有介电层和电磁波遮蔽层的层叠体上的方法。
(2)利用涂布法在层叠有介电层和电磁波遮蔽层的层叠体上形成酸系有机导电性高分子层、并在其上粘接基材层的方法。
(3)利用涂布法在层叠有介电层和电磁波遮蔽层的层叠体上形成酸系有机导电性高分子层、并在其上挤出基材层的方法
一个方面涉及的电磁波抑制片依次层叠均具有透光性的电阻覆膜、介电层、以及电磁波遮蔽层,电阻覆膜包含酸系有机导电性高分子层。但是,在电磁波抑制片的其他方式中,电阻覆膜的基材层对于可见光区域的电磁波也可以具有不透过性(可以为完全地不透过、也可以为不完全地不透过)。
在电磁波抑制片的一个方式中,将介电层设定为能够吸收30GHz至300GHz的毫米波带以上的高频带的电磁波的层厚,电磁波遮蔽层由导电性网状物构成,导电性网状物的开口率为35%以上85%以下,总光线透射率为30%以上,电磁波抑制片中的电磁波的衰减量为20dB以上。
在电磁波抑制片的一个方式中,电磁波遮蔽层的表面电阻值为0.3Ω/sq以下。
在电磁波抑制片的一个方式中,电阻覆膜的表面电阻值相对于真空的阻抗在-15%至+20%的范围内。
<有机导电膜的制造方法>
包括:制备包含酸系有机导电性高分子、碱中和剂以及液体介质的涂液的工序;将涂液涂布在基材层上的工序;以及从所涂布的涂液中除去液体介质的工序。
(碱中和剂)
除了酸系有机导电性高分子层中示例出的上述材料以外,涂液还可以含有碱中和剂。作为碱中和剂,只要是能够调节涂液的pH、且难以影响酸系有机导电性高分子的复合状态的物质即可,没有特别地限定,例如可以列举出:碱金属或碱土金属等的氢氧化物或碳酸盐、氨等铵化合物、胺类等。从易得性的观点来看,碱中和剂可以包含氨。
(液体介质)
作为液体溶剂,没有特别地限定,例如可以列举出:水、有机溶剂、水和有机溶剂的混合溶剂等。
涂液在25℃的pH为4.0~6.5。通过将pH调节在该范围内,可以对形成的酸系有机导电性高分子层赋予优异的耐光性。从该观点来看,涂液的pH可以为4.5~5.5。
作为将涂液涂布在基材层上的方法,没有特别地限定,例如可以列举出:凹版涂布法、逆转辊涂布法、模涂法、气刀涂布法、刮刀涂布法、刮棒涂布法(rod coating)、棒式涂布法(bar coating)、帘涂法、刀涂法、传送辊涂法、挤压涂布法、浸渍涂布法、吻涂法、喷涂法、压延涂布法、挤出涂布法等以往公知的涂布方法。
作为除去液体介质的方法,可以列举出:加热除去、减压除去、以及它们的组合。例如在利用加热除去液体介质的情况下,加热温度例如可以设为50~200℃、可以为90~150℃。加热时间取决于加热温度,例如可以设为30秒~15分钟、可以为1~5分钟。
实施例
通过以下的实施例对本发明进行更详细地说明,但是本发明不限于这些例子。
<涂液的制备>
作为聚(3,4-亚乙二氧基噻吩)-聚(苯乙烯磺酸)(PEDOT-PSS)分散液,准备了Heraeus株式会社制造的分散液Clevios PH1000(pH=3)。另外,作为包含碱中和剂的溶液,准备了关东化学株式会社制造的氨水(pH=12)。然后,按照表1准备了涂液1~3。涂液1是上述分散液本身,涂液2和3是通过在分散液PH1000中添加氨水以调节pH而成的溶液。25℃的涂液的pH通过株式会社堀场制作所制造的台式pH仪F-37来测定。
[表1]
涂液 | pH(25℃) |
1 | <3 |
2 | 5 |
3 | 7 |
<有机导电膜的制作>
使用棒涂机#18在聚对苯二甲酸乙二醇酯基材(PET、厚度50μm)上涂布各涂液,形成了涂膜。通过将所得的涂膜在120℃加热1分钟,从而在PET基材上形成了PEDOT-PSS层(厚度约300nm)。由此,制作了有机导电膜。
<有机导电膜的评价>
(PEDOT-PSS层中的阳离子含量)
使用Dionex株式会社制造的离子色谱DX-320定量了残留在PEDOT-PSS层中的铵离子。将各有机导电膜(样品尺寸:1cm2(1cm×1cm))放入萃取溶剂(超纯水100ml)中,在25℃环境下静置24小时。将静置后的萃取溶剂用超纯水稀释50倍后,通过离子色谱法进行了铵离子的定量。根据定量结果,算出了残留在PEDOT-PSS层中的铵离子的含量。结果如表2所示。
(表面电阻变化)
使用Mitsubishi Chemical Analytech Co.,Ltd.制造的Loresta-GP(MCP-T610、直列4探针(ASP)),在温度25℃测定PEDOT-PSS层的耐光性试验前后的表面电阻值。将各有机导电膜(样品尺寸:25cm2(5cm×5cm))的样品数设为3个、对各样品的测定次数设为5次、对共计15点测定表面电阻值并求取平均值,将其作为各PEDOT-PSS层的表面电阻值。然后,根据下式算出了表面电阻变化。结果如表2所示。
表面电阻变化=耐光性试验后的表面电阻值/耐光性试验前的表面电阻值
(其中,耐光性试验通过使用Suga试验机株式会社制造的Xenon Weather MeterX75,在放射照度60W/m2、BPT温度63℃、槽内温度40℃、槽内湿度50%rh、试验时间~500小时的条件下实施。)
[表2]
在比较例2中,在经过500小时后,观察到比实施例1大一个量级的表面电阻变化。
另一方面,在实施例1中,即使经过500小时表面电阻变化也被抑制地很低,具体而言,表面电阻值的变化控制在300。该值小于比较例1。
符号的说明
1…基材层、2…酸系有机导电性高分子层、10…有机导电膜。
Claims (9)
1.一种有机导电膜的制造方法,包括:
制备包含酸系有机导电性高分子、碱中和剂以及液体介质且在25℃的pH为4.0~6.5的涂液的工序;
将所述涂液涂布在基材层上的工序;以及
从所涂布的所述涂液中除去所述液体介质的工序。
2.根据权利要求1所述的制造方法,其中,
所述酸系有机导电性高分子包含聚噻吩系导电性高分子。
3.根据权利要求1或2所述的制造方法,其中,
所述碱中和剂包含氨。
4.一种有机导电膜,具备基材层和基材层上的酸系有机导电性高分子层,所述酸系有机导电性高分子层中的来自碱中和剂的阳离子含量为0.5~5.0mg/cm3。
5.根据权利要求4所述的膜,其中,
所述酸系有机导电性高分子包含聚噻吩系导电性高分子。
6.根据权利要求4或5所述的膜,其中,
来自所述碱中和剂的阳离子包含铵离子。
7.根据权利要求4至6中任一项所述的膜,其中,
所述基材层包含树脂基材或玻璃基材。
8.根据权利要求4至7中任一项所述的膜,用作电磁波抑制片的电阻覆膜或电子器件中的电路材料。
9.一种层叠体,具备:权利要求4至8中任一项所述的膜、介电层、以及电磁波遮蔽层。
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