CN106098154B - 一种芯鞘型石墨烯纤维复合光电极及其制备方法 - Google Patents

一种芯鞘型石墨烯纤维复合光电极及其制备方法 Download PDF

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CN106098154B
CN106098154B CN201610354940.XA CN201610354940A CN106098154B CN 106098154 B CN106098154 B CN 106098154B CN 201610354940 A CN201610354940 A CN 201610354940A CN 106098154 B CN106098154 B CN 106098154B
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杨政鹏
张春静
张雪峰
张春雷
赵威
牛宇涛
管学茂
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Abstract

本发明公开了一种芯鞘型石墨烯纤维复合光电极及其制备方法，本发明以浸涂聚合物凝胶电解质的石墨烯纤维为内电极，将石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在内电极上，构建所述的芯鞘型石墨烯纤维复合光电极。本发明的制备方法包括：制备氧化石墨烯纤维；还原制备石墨烯纤维；制备石墨烯/氢化TiO2纳米棒纤维；最后将石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在纤维电极上，即构建成所述的芯鞘型石墨烯纤维复合光电极。本发明制备的光电极具有制备简单、导电性好、可见光活性高、柔性好、可编织等优点。本发明可用于太阳能转化及有机废气光催化降解，在光电转化领域具有广泛的应用前景。

Description

一种芯鞘型石墨烯纤维复合光电极及其制备方法
技术领域
本发明属于柔性光电转化器件材料领域，具体涉及一种芯鞘型石墨烯纤维复合光电极及其制备方法。
背景技术
石墨烯是从石墨材料中剥离出来、由碳原子组成的只有一层原子厚度的二维晶体，因其具有优异的力学、光学、电学、热学性能以及独特的二维结构，引起了世界各国学者的广泛关注。为了推动石墨烯材料的实际应用，需将其制成一维的纤维、二维的薄膜以及三维的气凝胶等宏观组装结构。其中，石墨烯纤维以其良好的力学强度、柔韧性、导电性和可编织性，迅速成为石墨烯领域的研究热点之一。目前，石墨烯纤维已在光伏电池、超级电容器、柔性纤维状驱动器、固相微萃取、催化等方面显示出潜在的应用价值，如中国专利CN103390507 B公布了一种石墨烯/铂纳米粒子复合纤维电极材料及其制备方法，以它为对电极的纤维状染料敏化太阳能电池达到了8.45%的光电转化效率，是迄今为止所报导的线状太阳能电池最高效率；中国专利CN 104916453 A公布了一种同轴石墨烯纤维超级电容器及其制备方法，该电容器比电容高、循环性良好、有很好的韧性；中国专利CN 104949609 A公开了一种石墨烯柔性传感器及其制造方法，该传感器具有优良形变能力和较高电阻应变灵敏系数。这些基于石墨烯纤维的器件呈现出良好的柔韧性和可编织性，在可穿戴电子器件领域具有广阔的应用前景。
发明内容
本发明的目的在于提供一种芯鞘型石墨烯纤维复合光电极及其制备方法。
为达到上述目的，本发明采用以下技术方案：
一种芯鞘型石墨烯纤维复合光电极，其内电极为表面浸涂聚合物凝胶电解质的石墨烯纤维，外电极为石墨烯/氢化TiO2纳米棒纤维，由所述外电极顺序紧密缠绕在内电极上构建。
一种芯鞘型石墨烯纤维复合光电极的制备方法，包括如下步骤：
步骤1、将氧化石墨烯配制成10~20mg/ml的去离子水分散液，采用注射泵及Ø0.5~0.9mm的注射针头将分散液注入到凝固浴中，浸泡10~30min后，取出并自然干燥得到氧化石墨烯纤维，备用；
步骤2、将步骤1制得的氧化石墨烯纤维置于还原氛围中，60~90℃下还原6~12h，得到石墨烯纤维；
步骤3、将步骤2制得的石墨烯纤维浸涂聚合物凝胶电解质，得到凝胶电解质包裹的石墨烯纤维状电极，备用；
步骤4、将步骤1制得的氧化石墨烯纤维置于钛酸丁酯-去离子水-盐酸混合溶液中，密闭于反应釜中，经过水热反应在石墨烯纤维表面修饰TiO2纳米棒，清洗干燥后在H2/Ar气氛中热处理即得石墨烯/氢化TiO2纳米棒纤维；
步骤5、将步骤4制得的石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在步骤3制得的纤维电极上，即构建成所述的芯鞘型石墨烯纤维复合光电极。
进一步，所述的步骤1中的凝固浴为：含有1~5 wt% CaCl2的乙醇/水溶液，其中乙醇/水溶液为按1:1的体积比将乙醇和水均匀混合制得。
进一步，所述的步骤2中的还原氛围为35~45% HI溶液。
进一步，所述的步骤3中的聚合物凝胶电解质为聚乙烯醇/磷酸凝胶电解质，其包含1份的聚乙烯醇，9份水和1份磷酸。
进一步，所述的步骤4中的钛酸丁酯-去离子水-盐酸混合溶液各组分的体积比为1:8~12:8~12。
进一步，所述的步骤4中的水热反应温度为120~180℃，水热反应时间为8~12 h。
进一步，所述的步骤4中的H2/Ar气氛中热处理方法为：H2(5~20%)/Ar气氛中250~450℃下加热3~6h。
本发明的有益效果：
1、本发明在石墨烯纤维表面负载氢化TiO2纳米棒，一方面，TiO2纳米棒降低了光生电子-正穴的再结合几率；另一方面，氢化TiO2具有较高的可见光活性及导电性；致使石墨烯/氢化TiO2纳米棒纤维具有高光电转化性能。
2、石墨烯纤维复合光电极的芯鞘型结构具有较高接触面积，有利于电子的快速传递和转移，进而提高复合光电极的光电转化性能。
3、石墨烯对有机废弃物吸附能力强，有利于石墨烯纤维复合光电极对有机污染物的光催化降解及光电转化。
4、石墨烯纤维复合光电极柔韧性好，可编织，易于放大化。
附图说明
图1是芯鞘型石墨烯纤维复合光电极制备流程示意图
图2是石墨烯纤维复合光电极的光学图片
具体实施方式
为了更好地理解本发明，以下结合实施例对本发明作进一步说明：
实施例1：
一种芯鞘型石墨烯纤维复合光电极的制备方法，包括如下步骤：
步骤1、将氧化石墨烯配制成15mg/mL的去离子水分散液，采用注射泵及Ø0.7mm的注射针头将分散液注入到含3wt% CaCl2的乙醇/水(1:1 v/v)凝固浴中，浸泡20min后，取出并自然干燥得到氧化石墨烯纤维，备用；
步骤2、将步骤1制得的氧化石墨烯纤维置于40%HI溶液中，80℃下还原10h，得到石墨烯纤维；
步骤3、将步骤2制得的石墨烯纤维浸涂聚乙烯醇/磷酸凝胶电解质，得到凝胶电解质包裹的纤维状电极，备用；
步骤4、将步骤1制得的氧化石墨烯纤维置于体积比为1:10:10的钛酸丁酯-去离子水-盐酸混合溶液中，密闭于反应釜中，在150℃温度下水热反应10 h，清洗干燥后在H2(10%)/Ar气氛中250℃下加热5h即得石墨烯/氢化TiO2纳米棒纤维；
步骤5、将步骤4制得的石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在步骤3制得的纤维电极上，即构建成所述的芯鞘型石墨烯纤维复合光电极。
实施例2：
一种芯鞘型石墨烯纤维复合光电极的制备方法，包括如下步骤：
步骤1、将氧化石墨烯配制成10mg/mL的去离子水分散液，采用注射泵及Ø0.5mm的注射针头将分散液注入到含5wt% CaCl2的乙醇/水(1:1 v/v)凝固浴，浸泡15min后，取出并自然干燥得到氧化石墨烯纤维，备用；
步骤2、将步骤1制得的氧化石墨烯纤维置于35%HI溶液中，60℃下还原12h，得到石墨烯纤维；
步骤3、将步骤2制得的石墨烯纤维浸涂聚乙烯醇/磷酸凝胶电解质，得到凝胶电解质包裹的纤维状电极，备用；
步骤4、将步骤1制得的氧化石墨烯纤维置于体积比为1:8:8的钛酸丁酯-去离子水-盐酸混合溶液中，密闭于反应釜中，在120℃温度下水热反应18 h，清洗干燥后在H2(15%)/Ar气氛中250℃下加热6h即得石墨烯/氢化TiO2纳米棒纤维；
步骤5、将步骤4制得的石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在步骤3制得的纤维电极上，即构建成所述的芯鞘型石墨烯纤维复合光电极。
实施例3：
一种芯鞘型石墨烯纤维复合光电极的制备方法，包括如下步骤：
步骤1、将氧化石墨烯配制成20mg/mL的去离子水分散液，采用注射泵及Ø0.9mm的注射针头将分散液注入到含2wt% CaCl2的乙醇/水(1:1 v/v)凝固浴中，浸泡30min后，取出并自然干燥得到氧化石墨烯纤维，备用；
步骤2、将步骤1制得的氧化石墨烯纤维置于45%HI溶液中， 90℃下还原6h，得到石墨烯纤维；
步骤3、将步骤2制得的石墨烯纤维浸涂聚乙烯醇/磷酸凝胶电解质，得到凝胶电解质包裹的纤维状电极，备用；
步骤4、将步骤1制得的氧化石墨烯纤维置于体积比为1:12:12的钛酸丁酯-去离子水-盐酸混合溶液中，密闭于反应釜中，在180℃温度下水热反应10 h，清洗干燥后在H2(15%)/Ar气氛中450℃下加热3h即得石墨烯/氢化TiO2纳米棒纤维；
步骤5、将步骤4制得的石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在步骤3制得的纤维电极上，即构建成所述的芯鞘型石墨烯纤维复合光电极。
虽然，上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (7)

1.一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于：所述的电极其内电极为表面浸涂聚合物凝胶电解质的石墨烯纤维，外电极为石墨烯/氢化TiO2纳米棒纤维，所述外电极顺序紧密缠绕在内电极上构建；
所述芯鞘型石墨烯纤维复合光电极的制备方法，包括以下步骤：
步骤1、将氧化石墨烯配制成10～20mg/ml的去离子水分散液，采用注射泵及Ø0.5～0.9mm的注射针头将分散液注入到凝固浴中，浸泡10～30min后，取出并自然干燥得到氧化石墨烯纤维，备用；
步骤2、将步骤1制得的氧化石墨烯纤维置于还原氛围中，60～90℃下还原6~12h，得到石墨烯纤维；
步骤3、将步骤2制得的石墨烯纤维浸涂聚合物凝胶电解质，得到凝胶电解质包裹的石墨烯纤维状电极，备用；
步骤4、将步骤1制得的氧化石墨烯纤维置于钛酸丁酯-去离子水-盐酸混合溶液中，密闭于反应釜中，经过水热反应在石墨烯纤维表面修饰TiO2纳米棒，清洗干燥后在H2/Ar气氛中热处理即得石墨烯/氢化TiO2纳米棒纤维；
步骤5、将步骤4制得的石墨烯/氢化TiO2纳米棒纤维顺序紧密缠绕在步骤3制得的纤维电极上，即构建成所述的芯鞘型石墨烯纤维复合光电极。
2.根据权利要求1所述的一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于，所述的步骤1中的凝固浴为：含有1～5wt% CaCl2的乙醇/水溶液，其中乙醇/水溶液为按1:1的体积比将乙醇和水均匀混合制得。
3.根据权利要求1所述的一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于：所述的步骤2中的还原氛围为35~45% HI溶液。
4.根据权利要求1所述的一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于，所述的步骤3中的聚合物凝胶电解质为聚乙烯醇/磷酸凝胶电解质，其包含1份的聚乙烯醇，9份水和1份磷酸。
5.根据权利要求1所述的一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于，所述的步骤4中的钛酸丁酯-去离子水-盐酸混合溶液各组分的体积比为1:8～12:8～12。
6.根据权利要求1所述的一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于，所述的步骤4中的水热反应温度为120～180℃，水热反应时间为8～12h。
7.根据权利要求1所述的一种芯鞘型石墨烯纤维复合光电极的制备方法，其特征在于，所述的步骤4中的H2/Ar气氛中热处理方法为：H2(5～20%)/Ar气氛中250～450℃下加热3～6h。
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