CN105723472A - 制造表面处理过的透明导电聚合物薄膜的方法以及使用其制造的透明电极 - Google Patents
制造表面处理过的透明导电聚合物薄膜的方法以及使用其制造的透明电极 Download PDFInfo
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Abstract
本发明涉及制造表面处理过的透明导电聚合物薄膜的方法,包括:1)制备PEDOT:PSS墨水组合物;2)使用该墨水组合物在基板上形成PEDOT:PSS薄膜;3)在该PEDOT:PSS薄膜上涂布对甲苯磺酸溶液并随后热处理该PEDOT:PSS薄膜;4)清洗该热处理过的PEDOT:PSS薄膜;和5)干燥该清洗过的PEDOT:PSS薄膜。
Description
技术领域
本发明涉及经由表面处理制造具有高电导率的透明导电聚合物薄膜的方法,并涉及使用该方法制造的透明电极。
背景技术
可以主要以水分散体形式提供聚(3,4-乙烯二氧噻吩)-聚(苯乙烯磺酸)(PEDOT:PSS)来形成聚合物薄膜,并且PEDOT:PSS的电导率低至0.1-1S/cm。因此,可以通过用二甲亚砜(DMSO)或二甲基甲酰胺(DMF)溶液或用多元醇如乙二醇作为第二掺杂剂添加该PEDOT:PSS溶液来提高PEDOT:PSS的电导率。
但是,添加此类材料会劣化长期储存PEDOT:PSS水分散体时的稳定性。此外,当用其涂覆玻璃或膜时,溶液的表面张力可能提高,在基板上的润湿性可能由此变差,使得难以形成均匀的膜。
为了解决这些问题,已经尝试对由PEDOT:PSS水分散体形成的聚合物薄膜施以表面处理以提高电导率。
具体而言,使用硫酸、六氟丙酮、甲醇或DMF对该PEDOT:PSS膜进行表面处理。特别地,使用硫酸会导致电导率的极大提高。但是,硫酸造成该PEDOT:PSS膜损失严重。此外,由于使用强酸,会出现工作者的安全问题。
发明内容
技术问题
因此,在牢记相关领域中遭遇的问题的情况下进行了本发明,本发明的一个目的是提供一种通过可以容易地操作的表面处理法制造具有与使用硫酸时同样高的电导率的透明导电聚合物薄膜的方法。
本发明的另一目的是通过使用该透明导电聚合物薄膜来提供具有高电导率的透明电极。
技术方案
为了实现上述目的,本发明提供制造表面处理过的透明导电聚合物薄膜的方法,包括:1)制备PEDOT:PSS墨水组合物;2)使用该墨水组合物在基板上形成PEDOT:PSS薄膜;3)用对甲苯磺酸溶液涂覆该PEDOT:PSS薄膜并随后热处理该PEDOT:PSS薄膜,得到热处理过的PEDOT:PSS薄膜;4)清洗该热处理过的PEDOT:PSS薄膜,得到清洗过的PEDOT:PSS薄膜;和5)干燥该清洗过的PEDOT:PSS薄膜。
有益效果
按照本发明,由于PEDOT:PSS水分散体可以在不添加其它材料的情况下形成薄膜,因此有可能形成均匀薄膜和具有高电导率的透明导电墨水膜。
按照本发明,透明导电聚合物薄膜具有高电导率,由此可以取代ITO电极使用,并可以用作有机太阳能电池的缓冲层(空穴传输层)或电极层。
附图说明
图1是显示在对比例2中制造的PEDOT:PSS薄膜的电子显微镜图像;和
图2是显示在实施例1中制造的PEDOT:PSS薄膜的电子显微镜图像。
具体实施方式
下面,将给出本发明的详细说明。
本发明涉及制造表面处理过的透明导电聚合物薄膜的方法,包括:1)制备PEDOT:PSS墨水组合物;2)使用该墨水组合物在基板上形成PEDOT:PSS薄膜;3)在该PEDOT:PSS薄膜上涂覆对甲苯磺酸溶液并随后热处理该PEDOT:PSS薄膜,得到热处理过的PEDOT:PSS薄膜;4)清洗该热处理过的PEDOT:PSS薄膜,得到清洗过的PEDOT:PSS薄膜;和5)干燥该清洗过的PEDOT:PSS薄膜。
该PEDOT:PSS墨水组合物可以包含PEDOT:PSS水分散体、溶剂和表面活性剂。
该PEDOT:PSS水分散体使所述墨水组合物具有电导率。
该PEDOT:PSS水分散体的量可以为所述墨水组合物总重量的10-70重量%。如果其量小于10重量%,由于PEDOT:PSS的量过低,难以确保足够的电导率。相反,如果其量超过70重量%,铺展性会变差,由此使得难以形成均匀的薄膜,并在喷墨时劣化喷射性质。
在本发明的优选实施方案中,该PEDOT:PSS水分散体包括例如可获自Heraeus的PH-1000。
由于具有高粘度的PEDOT:PSS水分散体不能单独喷射,其以包含溶剂和表面活性剂的墨水组合物形式配制以便喷射。
所述溶剂可以包含去离子水(DI水)、二乙二醇丁醚或二乙二醇乙醚、和丙二醇。
去离子水用于分散PEDOT:PSS水分散体,其量可以为所述溶剂总重量的40-80重量%,并可以是所述墨水组合物总重量的10-40重量%。如果去离子水的量超过所述墨水组合物总重量的40重量%,所得墨水具有高表面张力,由此可能无法铺展在基板上并难以喷射。相反,如果其量小于10重量%,所得墨水因高粘度而不适用于喷墨。
二乙二醇丁醚或二乙二醇乙醚用于降低墨水的挥发性和提高喷射能力。
二乙二醇丁醚或二乙二醇乙醚的量可以为所述溶剂总重量的5-40重量%,并且可以是所述墨水组合物总重量的2-15重量%。如果二乙二醇丁醚或二乙二醇乙醚的量超过溶剂总重量的40重量%,所得墨水可能具有降低的电导率。相反,如果其量小于5重量%,铺展性和喷射性质会变差。
丙二醇起到保持墨水组合物的分散性和电导率。其量可以为所述溶剂总重量的5-40重量%,并可以是所述墨水组合物总重量的5-20重量%。如果其量落在上述范围之外,该墨水的电导率可能降低。
含有包含表面活性剂是为了提高所述墨水组合物的铺展性,并且其量为所述墨水组合物总重量的0.01-5重量%。如果其量小于0.01重量%,可能不能按需获得铺展性。相反,如果其量超过5重量%,该墨水的电导率可能降低。
该表面活性剂可以包括非离子表面活性剂,尤其是氟类表面活性剂。
在另一实施方案中,所述PEDOT:PSS墨水组合物可以进一步包含DMSO或DMF。
因此,可以添加DMSO或DMF以提高所述墨水组合物的电导率,其量可以为该墨水组合物总重量的1-5重量%。如果其量小于1重量%,在电导率方面没有改进。相反,如果其量超过5重量%,该墨水的电导率可能降低,并且可能导致差的稳定性。
在进一步的实施方案中,该PEDOT:PSS墨水组合物可以进一步包括DMSO或DMF,以及多元醇化合物。
该多元醇化合物可以包括但不必须限于甘油、二乙二醇、乙二醇和山梨糖醇。
添加该多元醇化合物是为了提高所述墨水组合物的电导率,其量可以为所述墨水组合物总重量的0.5-8重量%。如果其量超过8重量%,电导率可能降低。相反,如果其量小于0.5重量%,在电导率方面没有改进。
由于由此形成的墨水组合物表现出优异的喷射性质,其可以使用喷墨印刷法图案化,并由此适用于喷墨印刷。
在本发明中,进行2)使用如上所述的墨水组合物在基板上形成PEDOT:PSS薄膜。
该PEDOT:PSS薄膜通常使用棒涂、旋涂、喷墨印刷或喷涂来形成。特别有用的是喷墨印刷,因为可以使用少量材料在所需位置处实现直接图案化。
所述基板可以包括玻璃、薄膜等等,但是并非特别限于此。
用于膜基板的材料没有特殊限制,并可以包括例如PET、PC/PMMA或聚酰亚胺。
步骤3)是在所述PEDOT:PSS薄膜上涂覆对甲苯磺酸溶液并随后热处理该PEDOT:PSS薄膜的过程。
该对甲苯磺酸溶液可以是水溶液,或者是使用甲醇或乙醇作为溶剂的溶液。
在本发明中,对甲苯磺酸(PTSA)用于PEDOT:PSS薄膜的表面处理。由于PTSA是固体,其与硫酸相比易于操作,并用于提供与使用硫酸时同样高的电导率。此外,由于PTSA容易被甲醇,可以形成不具有表面污渍的清洁薄膜。在薄膜表面上形成水渍的情况下,薄膜的雾度可能不合意地提高。
该对甲苯磺酸溶液的浓度可以为0.01-0.2M。如果其浓度超过该上限,不能进一步提高电导率。
该对甲苯磺酸溶液可以使用通常的涂覆工艺施加在该PEDOT:PSS薄膜上。例如,漆刷、喷涂、刮涂、浸绘(dip-drawing)、旋涂、喷墨印刷或狭缝式模具涂布是有用的。
所述热处理温度设定为80-170℃,优选100-160℃。此外,热处理进行1-30分钟,优选3-15分钟。
步骤4)是在溶剂如甲醇、乙醇或IPA中浸没热处理过的PEDOT:PSS薄膜以去除残留在该薄膜表面上的PTSA的过程。由此,该浸没过程在室温下进行30秒至10分钟,优选3-8分钟。此类浸没条件可以根据样品的尺寸而变化。
在本发明的方法中,在用PTSA对薄膜进行表面处理后,残留在该薄膜表面上的PTSA可以用甲醇容易地清洗,由此最小化对薄膜表面的污染。
步骤5)是干燥PEDOT:PSS薄膜的过程,将其从溶剂中取出,以便除去残留在其上的溶剂。
通过上述方法制造的包含PEDOT:PSS的透明导电聚合物薄膜经由表面处理极大地提高了电导率。
本发明涉及包括通过上述方法制造的透明导电聚合物薄膜的透明电极。
此外,本发明涉及包括该透明导电聚合物薄膜作为缓冲层或电极层的有机太阳能电池。
下面是经由以下实施例对本发明进行的描述。
<实施例1>
对PH-1000(获自Heraeus)施以1000rpm下的旋涂30秒,由此形成膜,其随后在热板上在120℃下干燥15分钟,获得PEDOT:PSS薄膜。随后,将对甲苯磺酸(PTSA)(0.16M)溶液滴加到该PEDOT:PSS薄膜上,随后在热板上在160℃下热处理该PEDOT:PSS薄膜5分钟,在室温下冷却,随后浸没在MeOH中5分钟。随后,该PEDOT:PSS薄膜在热板上在160℃下干燥5分钟。
<实施例2>
以与实施例1相同的方式形成PEDOT:PSS薄膜,除了使用PTSA(0.1M)溶液。
<实施例3>
以与实施例1相同的方式形成PEDOT:PSS薄膜,除了其上滴加有PTSA(0.16M)溶液的PEDOT:PSS薄膜在140℃下热处理10分钟,并在140℃下干燥5分钟。
<实施例4>
以与实施例1相同的方式形成PEDOT:PSS薄膜,除了其上滴加有PTSA(0.16M)溶液的PEDOT:PSS薄膜在100℃下热处理15分钟,用MeOH清洗并在100℃下干燥5分钟。
<对比例1>
通过在1000rpm/30秒的条件下对PH-1000溶液施以旋涂来形成PEDOT:PSS薄膜。因此,没有进行表面处理。
<对比例2>
以与实施例1相同的方式形成PEDOT:PSS薄膜,除了使用0.16M的硫酸水溶液取代PTSA溶液,并用水进行清洗。
<对比例3>
以与实施例1相同的方式形成PEDOT:PSS薄膜,除了使用甲醇取代PTSA溶液。
<对比例4>
以与实施例1相同的方式形成PEDOT:PSS薄膜,除了使用0.16M硫酸水溶液,并在100℃下热处理15分钟和在100℃下干燥5分钟。
为了评价薄膜的性质,测量实施例1至4和对比例1至4的PEDOT:PSS薄膜的薄层电阻、透光率和雾度。
<薄膜性质的评价>
使用4点探针测量薄膜的薄层电阻。此外,测量透光率和雾度。
[表1]
<膜损伤的评价>
为了评价膜是否被损伤,使用电子显微镜观察实施例1和对比例2的PEDOT:PSS薄膜。
如图1中所示,对比例2的PEDOT:PSS薄膜被严重损伤。因此,使用硫酸水溶液的表面处理可能产生过度的膜损失。但是,如图2中所示,没有观察到对实施例1的PEDOT:PSS薄膜的损伤。因此,在用PTSA表面处理时不存在膜损伤。
基于该评价结果,按照本发明可以形成均匀的薄膜,并且还可以形成具有高电导率的透明导电墨水膜。
Claims (15)
1.制造表面处理过的透明导电聚合物薄膜的方法,包括:
1)制备PEDOT:PSS(聚(3,4-乙烯二氧噻吩)-聚(苯乙烯磺酸))墨水组合物;
2)使用所述墨水组合物在基板上形成PEDOT:PSS薄膜;
3)在所述PEDOT:PSS薄膜上涂布对甲苯磺酸溶液并随后热处理所述PEDOT:PSS薄膜,得到热处理过的PEDOT:PSS薄膜;
4)清洗所述热处理过的PEDOT:PSS薄膜,得到清洗过的PEDOT:PSS薄膜;和
5)干燥所述清洗过的PEDOT:PSS薄膜。
2.权利要求1的方法,其中所述PEDOT:PSS墨水组合物包含PEDOT:PSS水分散体、溶剂和表面活性剂。
3.权利要求2的方法,其中基于所述墨水组合物的总重量,所述PEDOT:PSS水分散体的用量为10-70重量%。
4.权利要求2的方法,其中所述溶剂包含去离子水、二乙二醇丁醚或二乙二醇乙醚、和丙二醇。
5.权利要求4的方法,其中基于所述溶剂的总重量,所述去离子水的含量为40-80重量%。
6.权利要求4的方法,其中基于所述溶剂的总重量,所述二乙二醇丁醚或二乙二醇乙醚的含量为5-40重量%。
7.权利要求4的方法,其中基于所述溶剂的总重量,所述丙二醇的含量为5-40重量%。
8.权利要求2的方法,其中基于所述墨水组合物的总重量,所述表面活性剂的用量为0.01-5重量%。
9.权利要求2的方法,其中所述PEDOT:PSS墨水组合物进一步包含DMSO(二甲亚砜)或DMF(二甲基甲酰胺)。
10.权利要求9的方法,其中基于所述墨水组合物的总重量,所述DMSO或DMF的用量为1-5重量%。
11.权利要求9的方法,其中所述PEDOT:PSS墨水组合物进一步包含多元醇化合物。
12.权利要求11的方法,其中基于所述墨水组合物的总重量,所述多元醇化合物的用量为0.5-8重量%。
13.权利要求1的方法,其中所述对甲苯磺酸溶液具有0.01-0.2M的浓度。
14.透明电极,包含通过权利要求1的方法制造的透明导电聚合物薄膜。
15.有机太阳能电池,包含通过权利要求1的方法制造的透明导电聚合物薄膜作为缓冲层或电极层。
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CN112126095A (zh) * | 2020-09-30 | 2020-12-25 | 华中科技大学 | 一种pedot:pss薄膜及其制备方法与应用 |
CN112126095B (zh) * | 2020-09-30 | 2021-12-03 | 华中科技大学 | 一种pedot:pss薄膜及其制备方法与应用 |
CN112735832A (zh) * | 2020-12-24 | 2021-04-30 | 湖南艾华集团股份有限公司 | 一种中高压固态铝电解电容器及其制备方法 |
CN112735832B (zh) * | 2020-12-24 | 2022-06-10 | 湖南艾华集团股份有限公司 | 一种中高压固态铝电解电容器及其制备方法 |
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CN105723472B (zh) | 2017-07-28 |
WO2015071794A1 (ko) | 2015-05-21 |
JP2016533003A (ja) | 2016-10-20 |
JP6101869B2 (ja) | 2017-03-22 |
KR101669574B1 (ko) | 2016-10-26 |
KR20150041971A (ko) | 2015-04-20 |
US9653217B2 (en) | 2017-05-16 |
US20160268056A1 (en) | 2016-09-15 |
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