CN112185608B - 一种新型双层导电网络结构的柔性透明电极及其制备方法 - Google Patents
一种新型双层导电网络结构的柔性透明电极及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种新型双层导电网络结构的柔性透明电极及其制备方法,包括一种新型的双层网络导电结构,所述一种新型的双层网络导电结构由单宁酸功能化碳纳米管与银纳米线复合组成,底层的功能化碳纳米管导电网络为银纳米线提供导电路径,并且可作为导电粘合剂增加复合薄膜导电稳定性以及银纳米线和基底之间的黏附力,将聚对苯二甲酸乙二醇酯(PET)基底薄膜用蒸馏水和乙醇超声清洗然后烘干,将配好的单宁酸改性碳纳米管溶液(TCNT)。该新型双层导电网络结构的柔性透明电极及其制备方法通过机械按压和喷涂聚3,4‑乙烯二氧噻吩(PEDOT)溶液对导电薄膜进行后处理,得到了黏附力好、表面粗糙度低、导电性高的透明电极。
Description
技术领域
本发明涉及电极制备技术领域,具体为一种新型双层导电网络结构的柔性透明电极及其制备方法。
背景技术
电子器件是指在真空、气体或固体中,利用和控制电子运动规律而制成的器件。分为电真空器件、充气管器件和固态电子器件。在模拟电路中作整流、放大、调制、振荡、变频、锁相、控制、相关等作用;在数字电路中作采样、限幅、逻辑、存储、计数、延迟等用,充气管器件主要作整流、稳压和显示之用。固态电子器件如集成电路在过去几年中,光电器件包括有机发光二极管(OLED)、有机太阳能电池(OSC)和场效应晶体管(FET)得到了充分的发展,对透明导电薄膜(TCFs)的需求变得越来越迫切,现有的透明柔性电极表面粗糙度低,黏附力低,导电性能差。
发明内容
本发明的目的在于提供一种新型双层导电网络结构的柔性透明电极及其制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种新型双层导电网络结构的柔性透明电极,包括一种新型的双层网络导电结构,所述一种新型的双层网络导电结构由单宁酸功能化碳纳米管与银纳米线复合组成,底层的功能化碳纳米管导电网络为银纳米线提供导电路径,并且可作为导电粘合剂增加复合薄膜导电稳定性以及银纳米线和基底之间的黏附力,将聚对苯二甲酸乙二醇酯(PET)基底薄膜用蒸馏水和乙醇超声清洗然后烘干,将配好的单宁酸改性碳纳米管溶液(TCNT)、银纳米线(AgNW)分别采用喷涂法与旋涂法逐层涂布在PET薄膜基底上,得到双层导电网络结构的柔性透明电极,后采用机械按压和喷涂聚3,4-乙烯二氧噻吩(PEDOT)溶液对导电薄膜进行后处理,用单宁酸(TA)功能化的单壁碳纳米管(TCNT)作为银纳米线与基底的结合层,构建了TCNT/AgNW双层导电网络结构。富含酚羟基的TA分子通过π-π相互作用吸附在碳纳米管壁上,使功能化碳纳米管(TCNT)表现出亲水性,并有效地提高了与AgNWs的粘附性。此外,细密的导电碳纳米管网络填充了AgNW网络的开口,增加了载流子的传输路径,有效地提高了杂化膜的导电性和电稳定性。机械按压以及喷涂PEDOT:PSS的后处理工艺使薄膜的粗糙度大幅度降低,同时进一步提升了薄膜的导电性,机械性能,以及耐腐蚀性能,在透光率为80%~90%时,面电阻为10~100Ω/sq,表面粗糙度<10nm。
优选的,所采用的原料为银纳米线溶液,其长度为40~60μm,直径为40~70nm,单壁碳纳米管,其纯度>95wt.%,外径1~2nm,长度为5~30μm,单宁酸粉末,AR级,聚3,4-乙烯二氧噻吩溶液为PH1000,固含量为1~1.3%。
优选的,采用超声波分散机制备TCNT分散液的条件,功率100-200W,时间30-80min,分散剂为十二烷基苯磺酸钠,制得的碳纳米管溶液浓度为0.1~0.5mg/ml。
优选的,配置银纳米线水溶液浓度为0.8~1.2mg/ml。
优选的,聚3,4-乙烯二氧噻吩溶液稀释5~20倍然后加入5wt.%二甲基亚砜,搅拌20min以上。
优选的,得到透明导电薄膜的透光度为80%以上,面电阻可以达到50Ω/sq.以下,表面粗糙度在10nm以下。
该发明还提供一种新型双层导电网络结构的柔性透明电极的制备方法:
采用单宁酸功能化碳纳米管(TCNT)溶液的制备如下,将SWCNT与单宁酸以1:1~4的比例分散在去离子水中,然后在60℃水浴加热条件下搅拌24h,之后通过离心,过滤,冷冻干燥收集TCNT粉末,随后,使用SDBS作为分散剂,将一定量的TCNT分散于蒸馏水中,水浴超声30min,然后将溶液放入120W探针超声中继续超声分散40min,随后将混合液在8000rmp下离心20min,并收集90%的上清液,以获得相应浓度的TCNT悬浊液,采用喷涂法将配好的不同量的单宁酸改性碳纳米管(TCNT)溶液喷涂在PET基底上,硝酸浸泡处理20分钟后干燥,随后在TCNT层上以2000转每分的转速旋涂不同浓度的银纳米线溶液,并充分干燥,得到双层导电网络结构的薄膜,最后处理工艺为机械按压以及表面喷涂PEDOT:PSS溶液,将制得的双层导电网络薄膜放置在压片机上,在25MPa压力下按压10min,以使银纳米线相互焊接,随后将3ml的聚3,4-乙烯二氧噻吩(PEDOT)溶液喷涂到按压处理后的薄膜上。
与现有技术相比,本发明的有益效果是:
一、通过机械按压和喷涂聚3,4-乙烯二氧噻吩(PEDOT)溶液对导电薄膜进行后处理,得到了黏附力好、表面粗糙度低、导电性高的透明电极。
二、该透明电极的制备工艺简单、周期短,其双层导电网络结构使得薄膜的结构稳定、黏附力强,经过高效的后处理电极的导电性有了极大的提高,而且粗糙度急剧下降。
三、该高性能透明电极可广泛应用于OLED有机发光器件、显示器、触摸屏、薄膜晶体管以及光伏器件等方面。
四、通过聚3,4-乙烯二氧噻吩(PEDOT)溶液喷涂到按压处理后的薄膜,干燥得到黏附力好、粗糙度低、导电性高的透明电极。
附图说明
图1为本发明单宁酸改性碳纳米管/银纳米线/聚3,4-乙烯二氧噻吩(TCNT/AgNW/PEDOT)透明导电薄膜的示意图;
图2为本发明的单宁酸改性碳纳米管/银纳米线(TCNT/AgNW)薄膜扫描电子显微镜图;
图3为本发明单宁酸改性碳纳米管/银纳米线/聚3,4-乙烯二氧噻吩(TCNT/AgNW/PEDOT)透明导电薄膜扫描电子显微镜图;
图4为本发明单宁酸改性碳纳米管/银纳米线/聚3,4-乙烯二氧噻吩(TCNT/AgNW/PEDOT)透明导电薄膜的面电阻和透光率显示图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
在本发明的描述中,需要说明的是,术语“上”、“下”、“内”、“外”“前端”、“后端”、“两端”、“一端”、“另一端”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性。
在本发明的描述中,需要说明的是,除非另有明确的规定和限定,术语“安装”、“设置有”、“连接”等,应做广义理解,例如“连接”,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以具体情况理解上述术语在本发明中的具体含义。
请参阅图1-4,本发明提供的一种实施例:一种新型双层导电网络结构的柔性透明电极,包括一种新型的双层网络导电结构,其特征在于:所述一种新型的双层网络导电结构由单宁酸功能化碳纳米管与银纳米线复合组成,底层的功能化碳纳米管导电网络为银纳米线提供导电路径,并且可作为导电粘合剂增加复合薄膜导电稳定性以及银纳米线和基底之间的黏附力,将聚对苯二甲酸乙二醇酯(PET)基底薄膜用蒸馏水和乙醇超声清洗然后烘干,将配好的单宁酸改性碳纳米管溶液(TCNT)、银纳米线(AgNW)分别采用喷涂法与旋涂法逐层涂布在PET薄膜基底上,得到双层导电网络结构的柔性透明电极,后采用机械按压和喷涂聚3,4-乙烯二氧噻吩(PEDOT)溶液对导电薄膜进行后处理。
进一步,所采用的原料为银纳米线溶液,其长度为40~60μm,直径为40~70nm,单壁碳纳米管,其纯度>95wt.%,外径1~2nm,长度为5~30μm,单宁酸粉末,AR级,聚3,4-乙烯二氧噻吩溶液为PH1000,固含量为1~1.3%。
进一步,采用超声波分散机制备TCNT分散液的条件,功率100-200W,时间30-80min,分散剂为十二烷基苯磺酸钠,制得的碳纳米管溶液浓度为0.1~0.5mg/ml。
进一步,配置银纳米线水溶液浓度为0.8~1.2mg/ml。
进一步,聚3,4-乙烯二氧噻吩溶液稀释5~20倍然后加入5wt.%二甲基亚砜,搅拌20min以上。
进一步,得到透明导电薄膜的透光度为80%以上,面电阻可以达到50Ω/sq.以下,表面粗糙度在10nm以下。
该发明还提供一种新型双层导电网络结构的柔性透明电极的制备方法:
采用单宁酸功能化碳纳米管(TCNT)溶液的制备如下,将SWCNT与单宁酸以1:1~4的比例分散在去离子水中,然后在60℃水浴加热条件下搅拌24h,之后通过离心,过滤,冷冻干燥收集TCNT粉末,随后,使用SDBS作为分散剂,将一定量的TCNT分散于蒸馏水中,水浴超声30min,然后将溶液放入120W探针超声中继续超声分散40min,随后将混合液在8000rmp下离心20min,并收集90%的上清液,以获得相应浓度的TCNT悬浊液,采用喷涂法将配好的不同量的单宁酸改性碳纳米管(TCNT)溶液喷涂在PET基底上,硝酸浸泡处理20分钟后干燥,随后在TCNT层上以2000转每分的转速旋涂不同浓度的银纳米线溶液,并充分干燥,得到双层导电网络结构的薄膜,最后处理工艺为机械按压以及表面喷涂PEDOT:PSS溶液,将制得的双层导电网络薄膜放置在压片机上,在25MPa压力下按压10min,以使银纳米线相互焊接,随后将3ml的聚3,4-乙烯二氧噻吩(PEDOT)溶液喷涂到按压处理后的薄膜上。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何附图标记视为限制所涉及的权利要求。
Claims (7)
1.一种新型双层导电网络结构的柔性透明电极,包括一种新型的双层网络导电结构,其特征在于:所述一种新型的双层网络导电结构由单宁酸功能化碳纳米管与银纳米线复合组成,底层的功能化碳纳米管导电网络为银纳米线提供导电路径,并且可作为导电粘合剂增加复合薄膜导电稳定性以及银纳米线和基底之间的黏附力,将聚对苯二甲酸乙二醇酯(PET)基底薄膜用蒸馏水和乙醇超声清洗然后烘干,将配好的单宁酸改性碳纳米管溶液(TCNT)、银纳米线(AgNW)分别采用喷涂法与旋涂法逐层涂布在PET薄膜基底上,得到双层导电网络结构的柔性透明电极,后采用机械按压和喷涂聚3,4-乙烯二氧噻吩(PEDOT)溶液对导电薄膜进行后处理。
2.根据权利要求1所述的一种新型双层导电网络结构的柔性透明电极,其特征在于:所采用的原料为银纳米线溶液,其长度为40~60μm,直径为40~70nm,单壁碳纳米管,其纯度>95wt.%,外径1~2nm,长度为5~30μm,单宁酸粉末,AR级,聚3,4-乙烯二氧噻吩溶液为PH1000,固含量为1~1.3%。
3.根据权利要求1所述的一种新型双层导电网络结构的柔性透明电极,其特征在于:采用超声波分散机制备TCNT分散液的条件,功率100-200W,时间30-80min,分散剂为十二烷基苯磺酸钠,制得的碳纳米管溶液浓度为0.1~0.5mg/ml。
4.根据权利要求1所述的一种新型双层导电网络结构的柔性透明电极,其特征在于:配置银纳米线水溶液浓度为0.8~1.2mg/ml。
5.根据权利要求1所述的一种新型双层导电网络结构的柔性透明电极,其特征在于:聚3,4-乙烯二氧噻吩溶液稀释5~20倍然后加入5wt.%二甲基亚砜,搅拌20min以上。
6.根据权利要求1所述的一种新型双层导电网络结构的柔性透明电极,其特征在于:得到透明导电薄膜的透光度为80%以上,面电阻可以达到50Ω/sq.以下,表面粗糙度在10nm以下。
7.根据权利要求1所述的一种新型双层导电网络结构的柔性透明电极,还包括一种制备方法,其操作步骤如下:
采用单宁酸功能化碳纳米管(TCNT)溶液的制备如下,将SWCNT与单宁酸以1:1~4的比例分散在去离子水中,然后在60℃水浴加热条件下搅拌24h,之后通过离心,过滤,冷冻干燥收集TCNT粉末,随后,使用SDBS作为分散剂,将一定量的TCNT分散于蒸馏水中,水浴超声30min,然后将溶液放入120W探针超声中继续超声分散40min,随后将混合液在8000rmp下离心20min,并收集90%的上清液,以获得相应浓度的TCNT悬浊液,采用喷涂法将配好的不同量的单宁酸改性碳纳米管(TCNT)溶液喷涂在PET基底上,硝酸浸泡处理20分钟后干燥,随后在TCNT层上以2000转每分的转速旋涂不同浓度的银纳米线溶液,并充分干燥,得到双层导电网络结构的薄膜,最后处理工艺为机械按压以及表面喷涂PEDOT:PSS溶液,将制得的双层导电网络薄膜放置在压片机上,在25MPa压力下按压10min,以使银纳米线相互焊接,随后将3ml的聚3,4-乙烯二氧噻吩(PEDOT)溶液喷涂到按压处理后的薄膜上。
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