CN106024392A - 一种柔性高光电转化石墨烯纤维光电极的制备方法 - Google Patents
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Abstract
本发明公开了一种柔性高光电转化石墨烯纤维光电极的制备方法。本发明制备的电极是以TiO2纳米颗粒/氧化石墨烯混合溶液为纺丝液，采用湿纺技术制备石墨烯/TiO2复合纤维，经过氧等离子刻蚀即得所述的石墨烯纤维光电极。本发明的制备方法包括：制备纺丝液；制备氧化石墨烯/TiO2复合纤维；制备石墨烯/TiO2复合纤维；最后将石墨烯/TiO2复合纤维放入氧等离子体处理器进行刻蚀，即得所述的石墨烯纤维光电极。本发明制备的石墨烯纤维光电极不仅使TiO2纳米颗粒嵌入在光电极表面，而且使得光电极表面嵌入的TiO2纳米颗粒部分裸露出来，提高了TiO2与光电极的结合牢固性和纤维光电极的光电转化性能；且具有柔韧性好、高光电转化性能等优点，在有机废水处理方面具有广阔的应用前景。
Description
技术领域
本发明属于石墨烯纤维光电极材料领域，尤其涉及一种柔性高光电转化石墨烯纤维光电极的制备方法。
背景技术
二氧化钛(TiO2)是目前研究最广泛的一种光催化材料，具有无毒、化学稳定性好、光催化活性高等优点，在气体净化、有机/无机废水处理、太阳能电池等领域得到了广泛应用。石墨烯是一种由六角形晶格组成的碳薄膜，以其优异的力学、光学、电学、热学性能和独特的二维结构成为材料领域的研究热点。近年来，石墨烯已与TiO2纳米粒复合制备光电极，并将其应用于染料敏化太阳能电池、有机物的光催化降解与光电转化以及光电化学传感器。虽然这些制备的TiO2纳米粒/石墨烯光电极具有较好的光化学与光电响应性能，然而在应用过程中仍然受到低光活性、电极刚性且小型化的影响，导致光电转化效率不理想、光电极构建成本高且难以放大化。石墨烯纤维由于其具有良好的力学强度、柔韧性、导电性和可编织性，为有效解决石墨烯基光电极存在的问题提供了可能。
发明内容
综上所述，本发明目的在于提供一种具有柔性和高光电转化性能的石墨烯/TiO2纤维光电极的制备方法。
一种柔性高光电转化石墨烯纤维光电极， 以TiO2纳米颗粒/氧化石墨烯混合溶液为纺丝液，采用湿纺技术制备石墨烯/TiO2复合纤维，经过氧等离子刻蚀即得所述的石墨烯纤维光电极。
一种柔性高光电转化石墨烯纤维光电极的制备方法，包括以下步骤：
步骤1、将氧化石墨烯配制成18mg/mL的去离子水分散液，按TiO2质量分数为0～60%的比例加入TiO2纳米颗粒，磁力搅拌得到分散均匀的纺丝液；
步骤2、采用注射泵及～0.9 mm的注射针头将纺丝液注入到凝固浴中，浸泡10～30min后，取出并自然干燥得到氧化石墨烯/TiO2复合纤维；
步骤3、将干燥的氧化氧化石墨烯/TiO2复合纤维在Ar气氛中于250～450℃下热处理3～5h，得到石墨烯/TiO2复合纤维；
步骤4、将石墨烯/TiO2复合纤维两端固定后，采用氧等离子体处理器对石墨烯/TiO2复合纤维进行刻蚀，即得所述的石墨烯纤维光电极。
进一步，所述的步骤1中的质量分数为：TiO2纳米颗粒占纺丝液固含量的质量分数。
进一步，所述的步骤2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4中的刻蚀条件为：氧气体流量400ml/min，工作功率为400W，刻蚀时间为1～7 min。
本发明的有益效果：
1. 本发明以氧化石墨烯/TiO2纳米颗粒为纺丝液，湿纺制备石墨烯纤维光电极，一方面，TiO2纳米颗粒在石墨烯片层表面分布均匀；另一方面，石墨烯纤维光电极中TiO2纳米颗粒的含量易于调控。
2. 本发明采用氧等离子刻蚀方法处理石墨烯纤维光电极，不仅使TiO2纳米颗粒嵌入在光电极表面，而且使得光电极表面嵌入的TiO2纳米颗粒部分裸露出来，提高了TiO2与光电极的结合牢固性和纤维光电极的光电转化性能。
3. 石墨烯纤维光电极制备方法简单，柔韧性好、可编织、易于放大化。
附图说明
图1a是石墨烯/TiO2(50%)纤维的SEM图；
图1b是石墨烯/TiO2(50%)纤维打结的SEM图；
图1c-f是石墨烯/TiO2(50%)纤维横截面的SEM图；
图2a-b是石墨烯/TiO2(50%)纤维在氧等离子体处理前后的SEM图；
图3是石墨烯、TiO2和石墨烯/TiO2纤维的拉曼图谱
图4是不同TiO2含量的石墨烯/TiO2纤维的强度；
图5是石墨烯/ TiO2(50%)纤维在不同氧等离子体处理时间下的光电流。
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
：
一种柔性高光电转化石墨烯纤维光电极的制备方法，包括如下步骤：
1）将氧化石墨烯配制成18mg/mL的去离子水分散液，按TiO2纳米颗粒占纺丝液固含量为50%的比例加入TiO2纳米颗粒，磁力搅拌得到分散均匀的纺丝液；
2） 采用注射泵及的注射针头将纺丝液注入到有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/TiO2复合纤维；
3）将干燥的复合纤维在Ar气氛中于450℃下热处理3h，得到石墨烯/TiO2复合纤维；
4）将石墨烯/TiO2复合纤维两端固定后，采用氧等离子体处理器在氧气体流量400ml/min、工作功率为400W的条件下刻蚀石墨烯/TiO2复合纤维5 min，即得所述的石墨烯纤维光电极。
将石墨烯纤维光电极编织成5×5cm网作为工作电极，饱和甘汞电极作为参比电极，铂丝作为辅助电极，KCl溶液（0.1 mol/L）作为电解液，测试2 ×105mol/L罗丹明B的光电转化，氙灯光照90min后，光电转化率为97%。
实施例
2
：
一种柔性高光电转化石墨烯纤维光电极的制备方法，包括如下步骤：
1）将氧化石墨烯配制成18mg/mL的去离子水分散液，按TiO2纳米颗粒占纺丝液固含量为30%的比例加入TiO2纳米颗粒，磁力搅拌得到分散均匀的纺丝液；
2） 采用注射泵及的注射针头将纺丝液注入到有4wt% CaCl2的乙醇/水(1:1 v/v)凝固浴中，浸泡25min后，取出并自然干燥得到氧化石墨烯/TiO2复合纤维；
3）将干燥的复合纤维在Ar气氛中于350℃下热处理4h，得到石墨烯/TiO2复合纤维；
4）将石墨烯/TiO2复合纤维两端固定后，采用氧等离子体处理器在氧气体流量400ml/min、工作功率为400W的条件下刻蚀石墨烯/TiO2复合纤维3 min，即得所述的石墨烯纤维光电极。
将石墨烯纤维光电极编织成5×5cm网作为工作电极，饱和甘汞电极作为参比电极，铂丝作为辅助电极，KCl溶液（0.1mol/L）作为电解液，测试2 ×105mol/L罗丹明B的光电转化，氙灯光照90min后，光电转化率为91%。
实施例
3
：
一种柔性高光电转化石墨烯纤维光电极的制备方法，包括如下步骤：
1）将氧化石墨烯配制成18mg/mL的去离子水分散液，按TiO2纳米颗粒占纺丝液固含量为40%的比例加入TiO2纳米颗粒，磁力搅拌得到分散均匀的纺丝液；
2） 采用注射泵及的注射针头将纺丝液注入到有5wt% CaCl2的乙醇/水(1:1 v/v)凝固浴中，浸泡15min后，取出并自然干燥得到氧化石墨烯/TiO2复合纤维；
3）将干燥的复合纤维在Ar气氛中于250℃下热处理5h，得到石墨烯/TiO2复合纤维；
4）将石墨烯/TiO2复合纤维两端固定后，采用氧等离子体处理器在氧气体流量400ml/min、工作功率为400W的条件下刻蚀石墨烯/TiO2复合纤维7 min，即得所述的石墨烯纤维光电极。
将石墨烯纤维光电极编织成5×5cm网作为工作电极，饱和甘汞电极作为参比电极，铂丝作为辅助电极，KCl溶液（0.1 mol/L）作为电解液，测试2 ×105mol/L罗丹明B的光电转化，氙灯光照90min后，光电转化率为94%。
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 (5)
1.一种柔性高光电转化石墨烯纤维光电极，其特征在于：以TiO2纳米颗粒/氧化石墨烯混合溶液为纺丝液，采用湿纺技术制备石墨烯/TiO2复合纤维，经过氧等离子刻蚀即得所述的石墨烯纤维光电极。
2.一种柔性高光电转化石墨烯纤维光电极的制备方法，其特征在于，包括以下步骤：
步骤1、将氧化石墨烯配制成18mg/mL的去离子水分散液，按TiO2质量分数为0～60%的比例加入TiO2纳米颗粒，磁力搅拌得到分散均匀的纺丝液；
步骤2、采用注射泵及Ø0.5～0.9 mm的注射针头将纺丝液注入到凝固浴中，浸泡10～30min后，取出并自然干燥得到氧化石墨烯/TiO2复合纤维；
步骤3、将干燥的氧化氧化石墨烯/TiO2复合纤维在Ar气氛中于250～450℃下热处理3～5h，得到石墨烯/TiO2复合纤维；
步骤4、将石墨烯/TiO2复合纤维两端固定后，采用氧等离子体处理器对石墨烯/TiO2复合纤维进行刻蚀，即得所述的石墨烯纤维光电极。
3.根据权利要求2所述的一种柔性高光电转化石墨烯纤维光电极的制备方法，其特征在于，所述的步骤1中的质量分数为：TiO2纳米颗粒占纺丝液固含量的质量分数。
4.根据权利要求2所述的一种柔性高光电转化石墨烯纤维光电极的制备方法，其特征在于，所述的步骤2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。
5.根据权利要求2所述的一种柔性高光电转化石墨烯纤维光电极的制备方法，其特征在于，所述的步骤4中的刻蚀条件为：氧气体流量400ml/min，工作功率为400W，刻蚀时间为1～7 min。
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