CN108682565A - 一种层-层石墨烯/二硫化钼复合电极材料及其制备方法 - Google Patents
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Abstract
本发明属于新能源纳米功能材料技术领域，具体为一种层‑层石墨烯/二硫化钼复合电极材料及其制备方法。本发明通过静电吸附自组装得到具有单层或少层石墨烯与单层二硫化钼的层‑层结构的电极材料。本发明制备的电极材料可充分利用石墨烯的优异的导电性和二硫化钼的高催化性，可根据对导电性和催化性的不同需求调整氧化石墨烯与二硫化钼的比例。本发明制备的材料制备操作简便，工艺简单，条件要求低。将该层‑层组装的电极材料应用到染料敏化太阳能电池对电极制备进行电池组装获得高效光电转化效率。
Description
技术领域
本发明属于纳米功能化材料制备技术领域，具体的说，涉及一种层-层石墨烯/二硫化钼复合电极材料及其制备方法。
背景技术
随着能源危机和环境污染不断加剧，探索开发新型环保高效的能源是人类社会可持续发展的必然选择。太阳能取之不尽用之不竭，近几十年来对太阳能的开发利用得到了较大的提高，基于以硅晶体为主的第一代太阳能电池和以碲化镉和铜铟镓硒薄膜为主的第二代太阳能电池都有较好的光电转换效率，但因工艺复杂、成本高、环境污染严重等缺点制约了两种技术的普及。1991年瑞士的Gratzel等报道的染料敏化太阳能电池(Dye-Sensitized Solar Cells，DSSCs)作为第三代太阳能电池，因其成本低、易组装、PCE高等诸多优点，具有非常广阔的发展前景。
DSSCs主要由吸附染料的纳米晶TiO2光阳极、含有氧化还原电对的电解液和对电极组成。对电极的主要作用是收集外电路的电子，并将其高效快速地传递给电解质，同时催化还原I3 -。传统铂(Pt)电极因稳定性好、导电性和催化性能高等优点而得到广大发展，但因其价格高和稀有性等因素限制了Pt电极的商业应用。目前碳材料因价格低廉、方便易得、导电性好优点而成为应用较多的Pt替代材料，如碳纳米管、石墨烯、富勒烯等，而碳材料在染料敏化太阳能电池中表现出较弱的催化性，所以研究人员常常将碳材料与具有高催化性的材料复合制备兼备导电与催化性能的对电极。
二硫化钼(MoS2)作为一种典型的过渡金属化合物因具有与Pt类似的电子结构表现出优异的催化性能。不同于石墨烯的零带隙，MoS2具有独特带隙结构，块状MoS2半导体简介能带为1.2eV，电子跃迁方式为非垂直跃迁。而当MoS2片层为单层时，因量子限域效应，能隙不断扩大，单层MoS2能隙达到1.8eV，且电子为直接跃迁。因而，相比于块状MoS2，二维单层MoS2表现出优异的催化特性。
发明内容
为了解决现有技术的缺点和不足，本发明的目的是提供一种层-层石墨烯/二硫化钼复合电极材料及其制备方法。本发明利用石墨烯与二硫化钼在一定的pH下具有相反的zeta 电位，通过静电吸附自组装成具有层-层结构的电极材料，制备操作简便，工艺简单，条件要求低；本发明可通过调整石墨烯与二硫化钼，调整材料的电化学性能和催化性能。
本发明可以通过以下技术方案来实现。
本发明提供一种层-层石墨烯/二硫化钼复合电极材料的制备方法，包括以下步骤：
(1)将50～200mg的氧化石墨加入到40-60mL去离子水中，并超声2～6h，得到分散均匀的氧化石墨烯溶液，即溶液A；
(2)取10-50mL的1-3mg·mL-1单层MoS2分散液，超声使其分散均匀，得到溶液B；
(3)用pH计分别调节溶液A、B的pH值在2.5-6.5之间；
(4)在搅拌的情况下，滴加溶液B至溶液A中，得到混合溶液C，滴加完毕后，继续搅拌10-15h；
(5)将步骤(4)中得到的混合溶液C离心，得到黑色固体；
(6)将步骤(5)中的黑色固体用去离子水洗涤后真空干燥，再将真空干燥后产物在管式炉中惰性氛围下，750-850℃的温度下退火处理1-3h，得到层-层组装的石墨烯/二硫化钼。
本发明中，步骤(4)中，滴加速度为10-30滴/分钟。
本发明中，步骤(5)中，离心转速为11000-13000r·min-1，离心时间为8-15min。
本发明制备的层-层G/MoS2电极材料，可用作光催化材料以及锂离子电池、太阳能电池、电容器等新型能源的理想电极材料。
和现有技术相比，本发明的有益效果在于：
(1)本发明通过调整材料的pH使两种材料在同一pH下拥有相反zeta电位来静电吸附的方式制备电极，操作简便，工艺简单，速度快，条件要求低，成本低。
(2)本发明制备的电极材料可同时具有良好的导电性和催化性，可根据对导电性和催化性的不同需求调整氧化石墨烯与二硫化钼的比例。通过循环伏安与交流阻抗测试得知，石墨烯的含量越高，复合材料的导电性越好，反之催化性越好。
(3)本发明中，氧化石墨通过超声处理得到氧化石墨烯纳米片层，与带有相反zeta电位的单层MoS2纳米片发生静电吸附，得到具有单层或少层石墨烯与单层MoS2的层-层组装的电极材料。
附图说明
图1是石墨烯与MoS2在不同pH下的zeta电位图示。
图2是实施例1所获得的G/MoS2电极材料中高倍透射电子显微镜图片。
图3是实施例1所获得的G/MoS2电极材料边缘层-层结构的透射电子显微镜图片。
图4是实施例中三个G/MoS2电极材料制备电极后以I-/I3 -电解液在20mV·s-1扫描速度下所测得的循环伏安(CV)曲线。
图5是实施例中三个G/MoS2电极材料各自组装虚拟电池的交流阻抗(EIS)测试图谱。
具体实施方式
为了使本技术领域的研究人员更好地理解本发明的技术方案，下面结合实施例对本发明产品作进一步详细的说明，但本发明的实施方式不限于此。
图1是石墨烯与MoS2在不同pH下的zeta电位图示；实施例中，带有相反zeta电位的单层MoS2纳米片和氧化石墨烯发生静电吸附，得到具有单层或少层石墨烯与单层MoS2的层-层组装的电极材料。
实施例1
(1)称取50mg的氧化石墨至50mL去离子水中，超声4h得到分散均匀的氧化石墨烯溶液；
(2)取10mL的2mg·mL-1单层MoS2分散液，超声使其分散均匀；
(3)用pH计分别调节溶液(1)、(2)的pH到3.0；
(4)在搅拌的情况下，以每分钟20滴的速率滴加单层MoS2溶液至氧化石墨烯溶液中，得到混合溶液，滴加完毕后将混合溶液以800r·min-1搅拌12h；
(5)将步骤(4)中得到的混合溶液以12000r·min-1的速率离心10min，得到黑色固体；
(6)将步骤(5)中的黑色固体用去离子水洗涤三次后真空干燥48h，并将产物在管式炉中氩气氛围下做800℃退火处理2h，最后得到层-层组装的石墨烯/二硫化钼，记作 G/MoS2-1。图2是实施例1所获得的G/MoS2电极材料中高倍透射电子显微镜图片，图中可以看到许多块状MoS2堆积在大片的石墨烯表面。图3是实施例1所获得的G/MoS2电极材料边缘层-层结构的透射电子显微镜图片，由图可知石墨烯与MoS2是层-层状复合。
实施例2
将实施例1中单层MoS2分散液改取20mL，其余均同实施例1，最终所获得杂化材料标记为G/MoS2-2。
实施例3
实施例3，将实施例1中单层MoS2分散液改取25mL，其余均同实施例1，最终所获得杂化材料标记为G/MoS2-3。
图4是实施例中三个G/MoS2电极材料制备电极后以I-/I3 -电解液在20mV·s-1扫描速度下所测得的循环伏安(CV)曲线。CV曲线左侧负电位的一对峰(氧化峰(ii)和还原峰(ii))的峰电位差△Ep和对应的氧化峰(ii)电流密度Jp是考察电极催化性能的两个重要参数，其中△Ep越小，Jp值越大表明材料对I3 -离子的还原性越好，即催化性能越好。对各电极CV曲线分析得，G/MoS2-1，G/MoS2-2，G/MoS2-3电极各自的峰电位差△Ep分别为 174，250和170mV，而G/MoS2-1，G/MoS2-2，G/MoS2-3电极各自Jp值分别为3.61，3.08 和3.62mA·cm-2，其中G/MoS2-3具有最小的△Ep与最高的Jp值，由此表明高的MoS2负载量可以提高复合电极材料的催化性能。
图5是实施例中三个G/MoS2电极材料各自组装虚拟电池的交流阻抗(EIS)测试图谱。制备电极过程中，电极表面负载同等质量的电极材料，即电极表面薄膜厚度可认为相同，因此忽略电极的薄膜电阻(Rsh)对电池性能影响的讨论；而G/MoS2-1，G/MoS2-2，G/MoS2-3电极的电荷转移电阻(Rct)分别为0.35，0.49和2.03Ω·cm-2。其中G/MoS2-1具有最小的Rct，即G/MoS2-1具有更高的导电性；G/MoS2-3负载过多的MoS2负载，而MoS2本身导电性差，这也影响了杂化材料的整体导电性。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其它的任何未背离本发明的精神实质和原则之内的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种层-层石墨烯/二硫化钼复合电极材料的制备方法，其特征在于，包括以下步骤：
(1)将50～200mg的氧化石墨加入到40-60mL去离子水中，并超声2～6h，得到分散均匀的氧化石墨烯溶液，即溶液A；
(2)取10-50mL的1-3mg·mL-1单层MoS2分散液，超声使其分散均匀，得到溶液B；
(3)用pH计分别调节溶液A、B的pH值在2.5-6.5之间；
(4)在搅拌的情况下，滴加溶液B至溶液A中，得到混合溶液C，滴加完毕后，继续搅拌10-15h；
(5)将步骤(4)中得到的混合溶液C离心，得到黑色固体；
(6)将步骤(5)中的黑色固体用去离子水洗涤后真空干燥，再将真空干燥后产物在管式炉中惰性氛围下，750-850℃的温度下退火处理1-3h，得到层-层组装的石墨烯/二硫化钼。
2.根据权利要求1所述的制备方法，其特征在于，步骤(4)中，滴加速度为10-30滴/分钟。
3.根据权利要求1所述的制备方法，其特征在于，步骤(5)中，离心转速为11000-13000r·min-1，离心时间为8-15min。
4.一种根据权利要求1-3之一所述的制备方法制得的层-层石墨烯/二硫化钼复合电极材料。
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