石墨烯及石墨烯基材料的控制制备与超级电容器应用研究
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摘要
1.报道了利用化学氧化还原法来实现石墨烯尺寸和层数的控制制备,并进一步通过实验和理论计算研究了石墨烯的尺寸和层数对其比表面积的影响,以及它们对基于石墨烯的透明电极器件的导电性影响。首先,我们通过增加氧化剂与原料的比例实现了氧化石墨烯尺寸的不断减小。原子力显微镜的表征结果显示,随着氧化剂与原料比例的增加,产物中氧化石墨烯的片层面积从20000nm~2逐渐减小到550nm~2。其次,我们通过减少氧化剂与原料的比例实现了寡层氧化石墨烯的制备。原子力显微镜的表征结果显示,制备得到的寡层氧化石墨烯的厚度大多为2-3纳米,对应的片层数为2-4层；并且寡层氧化石墨烯的平均尺寸约为1微米,远大于单层氧化石墨烯的尺寸。此外,我们通过溶液旋涂和不同的还原方法分别制备得到了基于单层石墨烯和寡层石墨烯的透明导电电极,并测试了它们的导电性。测试结果表明,基于寡层石墨烯的透明导电电极的导电性为480S／cmm,比基于单层石墨烯的透明导电电极的导电性要高一个数量级(38S／cm),说明石墨烯的尺寸和层数对透明电极器件的导电性有较大的影响；同时我们建立一系列石墨烯模型,并计算了它们的理论比表面积,结果显示,石墨烯材料的比表面积与边缘碳原子数的比例以及片层堆叠情况是密切相关的,其中边缘碳原子数的比例决定于石墨烯片层的尺寸大小和片层上缺陷的数量。即：石墨烯片层的尺寸越小、片层上的缺陷数量越多或石墨烯片层之间的堆叠越少,其对应的石墨烯宏观材料的比表面积就越高。这与实验得到的结果是一致的,即单层氧化石墨烯的比表面积(60m~2/g)明显高于寡层氧化石墨烯(4m~2／g)。
2.目前很少有一种宏观sp2碳材料能够同时展现出优异的导电性和比表面积。因此,我们借鉴了制备复合材料的思路,通过结合石墨烯优异的导电性以及活性碳较高的比表面积得到了兼具优良导电性和比表面积的宏观sp2碳材料。我们发现该sp2碳材料的导电性和比表面积可以通过调节石墨烯前体与活性碳前体的比例来控制。在导电性方面,石墨烯前体的比例越高,·该产物的导电性就越高；而在比表面积方面,产物的比表面积则是与原料的结构疏松度密切相关的。即在反应过程中,原料的结构越疏松,它就越容易与活化剂氢氧化钾进行均匀的混合和反应,因此其产物的比表面积也比较高。为了进一步验证这一现象,我们以具有疏松多孔结构的花粉以及具有致密结构的酚醛树脂作为两种原料,对它们进行相同的活化反应并比较了产物的比表面积。结果显示由花粉制备得到的产物的比表面积要远高于由酚醛树脂制备得到的产物的比表面积,证明产物的比表面积确实与原料的结构疏松度确实有很大的关系。此外我们还对系列sp2碳材料的结构进行了详细的表征和计算模拟,结果显示：1,这些sp2碳材料主要是由很多高度扭曲的石墨烯碎片无序搭接而成的；2,对于具有不同比表面积的sp2碳材料产物,其包含的石墨烯碎片的尺寸大小和层数以及堆叠情况是不同的；3,sp2碳材料的比表面积能够超过石墨烯的理论值是因为其边缘碳原子的比例比较高。而在sp2碳材料的六元环共轭结构中引入五元环和七元环以后,sp2碳材料的比表面积不但没有增加,反而会减小。这些结果同样可以适用于其他具有高比表面积的复杂sp2碳材料,如活性碳,因此这不仅对活性碳的结构摸索和研究开辟了新思路,更从根本上解释了sp2碳材料超高比表面积的来源,具有很重要的意义。
3.我们通过调控sp2碳材料制备过程中的反应参数以及改变原料的种类和形貌,制备得到了一系列具有不同比表面积和孔径分布的sp2碳材料,并测试了这些sp2碳材料在两种离子液中的实验比电容值。其中最好的比电容值为220F/g,其基于活性材料的能量密度能达到90Wh/kg以上。同时我们系统地研究了sp2碳材料的比表面积和孔径分布对其超级电容器性能的影响。结果显示各sp2碳材料的实验比电容值与系列sp2碳材料的有效比表面积呈现较好的线性关系,其线性关系的斜率为0.142,线性相关系数为0.96,这说明比表面积和孔径分布对sp2碳材料电容性能都有重要的影响。此外,我们还建立了一种基于sp2碳材料以及离子液电解液的结构模型,并通过几何建模和数学计算分别得到了系列sp2碳材料在两种离子液中的理论比电容值。我们发现系列sp2碳材料的实验比电容值和理论比电容值具有很好的一致性,这说明在衡量sp2碳材料的电容性能时,可以通过这种理论计算模型简单快速地得出其比电容值,而不用组装实际的超级电容器器件。这对快速有效的衡量和筛选适用于超级电容器的高性能sp2碳材料提供了新的途径,具有很重要的意义。
4.我们以氧化石墨烯、硝酸钴和柠檬酸作为原料,利用溶胶凝胶法和“自燃烧”的方法制备得到了石墨烯/钴金属纳米颗粒的复合材料。该复合材料同时具有较好的导电性和铁磁性,在电磁屏蔽和吸波等领域具有很广泛的应用前景。此外,这种通过干凝胶自燃烧制备石墨烯/钴纳米粒子复合材料的方法具有着独特的优点,它不仅操作简单、反应条件温和,而且还具有很强的普适性,可以广泛的适用于其他石墨烯基金属纳米复合材料的制备(比如镍、银或铜等金属纳米粒子),因此具有很重要的意义。
1. Large scale synthesis of graphene with controlled size and layer numbers has been realized by chemical exfoliation method. The impact of graphene size and layer numbers on the electrical conductivity of transparent conductive film electrodes and their specific surface area (SSA) has also been well studied. It is found with increasing amount of oxidants, the size of graphene oxide (GO) is dramatically decreased from20000to550nm2. And if we decrease the amount of oxidants, we can get few layered graphene oxide (FGO) which exhibits both larger size (～1μm) and number of layers (2-4) than single layered GO. Transparent conductive film electrodes based on reduced GO and FGO have been fabricated by spin coating process and chemical or thermal reduction. It is demonstrated that transparent conductive film electrodes based on reduced FGO exhibit much higher electrical conductivity of～480S/m than those based on reduced GO (-38S/m), which indicates that the size and number of layers of graphene have played important roles on the electrical conductivities of transparent conductive film electrodes. Furthermore, based on the results from theoretical calculation and experimental characterizations, we also find out that the size and number of layers in graphene materials have great influence on their SSA. That is, the SSA of graphene materials will highly decrease with increasing size and number of layers, as an example shown in FGO (60m2/g) and GO (4m2/g).
2. Until now, few sp2carbon materials simultaneously exhibit superior performance for SSA and electrical conductivity at bulk state. Thus, by combining the good conductivity of graphene and high SSA of activated carbon, we prepare a series of graphene-based sp2carbon materials at the bulk scale, which exhibit ultrahigh SSA and excellent bulk conductivity. It is found that both the SSA and conductivity of the products can be controlled by varying the proportion between the graphene and activated carbon in the products. The conductivity of the products is increased with increasing amount of graphene. But the SSA of the products is firstly increased but then decreased with increasing amount of graphene. Thorough characterizations have suggested that the structure and morphology of carbon precursors played important roles on the SSA of the products. This is further identified by using porous pollens and firm solid phenolic resin as carbon precursors of activated carbons. And activated carbons based on porous pollens have exhibited much higher SSA than phenolic resin based activated carbons. Furthermore, comprehensive study and structural characterization have been performed for exploring the structure of graphene-based sp2carbon materials and explaining the origin of its ultrahigh specific surface (even higher than the theoretical SSA of graphene,2680m2/g). We conclude that these graphene-based sp2carbon materials consist of mainly defected/wrinkled single layer graphene sheets in the dimensional size of a few nanometers. And the ultrahigh SSA cannot be due to the existence of pentagon and/or heptagon in the graphene-based sp2carbon materials but should mainly come from the edge (or defects) of the graphene sheets with dimensional size of a few nanometers. We believe this should be also applicable to other sp2carbon materials with high SSA, such as activated carbon, thus has important implication for the structural and property study of activated carbon.
3. A series of sp2carbon materials with different SSA and controlled pore size distribution (PSD) were prepared at large scale through a facile and low-cost method. The SSA and PSD of these carbon materials were controlled by adjusting preparation methods and using different carbon sources. Experimental capacitance performance has been tested for all the sp carbon materials and the highest specific capacitance in ionic liquid is220F/g, with an ultrahigh energy density up to90Wh/kg. The impacts of SSA and PSD on their capacitance performance were thoroughly investigated, which demonstrated that both SSA and PSD played the most important role on their effective SSA (E-SSA) and capacitance performance. And a linear relationship has been observed between the E-SSA and experimental specific capacitance, with a coefficient of determination of0.96. Furthermore, a general theoretical model using the slit/cylindrical NL-DFT approach is proposed for the estimation of the specific capacitance of sp2carbon materials, which is in good agreement with the experimental specific capacitance. These results offer a simple but reliable method to predict the capacitance performance of these materials, thus speeding up the designing and screening the materials for high performance supercapacitor and other surface area related devices.
4. A versatile new strategy for producing graphene/cobalt magnetic nanocomposites by combining the sol-gel method and autocombustion is presented. GO, cobalt nitrate and citric acid are used as starting materials and a dry gel of the mixture is prepared through a routine sol-gel approach. The autocombustion reaction was activated at300℃in a tube furnace under an argon atmosphere, which produces lots of reducing agents such as H2and CH4and then in situ reduce GO and cobalt oxide to get graphene/cobalt magnetic nanocomposites. It is demonstrated that the cobalt nanoparticles (but not cobalt oxide) with size of～10nm are homogeneously loaded on graphene sheets. Further more, other metal nanoparticles such as Ni, Cu, Ag and Bi can also be loaded on graphene using the same method, which have great potential for the application on the electromagnetic shield and microwave absorption.
2.目前很少有一种宏观sp2碳材料能够同时展现出优异的导电性和比表面积。因此,我们借鉴了制备复合材料的思路,通过结合石墨烯优异的导电性以及活性碳较高的比表面积得到了兼具优良导电性和比表面积的宏观sp2碳材料。我们发现该sp2碳材料的导电性和比表面积可以通过调节石墨烯前体与活性碳前体的比例来控制。在导电性方面,石墨烯前体的比例越高,·该产物的导电性就越高；而在比表面积方面,产物的比表面积则是与原料的结构疏松度密切相关的。即在反应过程中,原料的结构越疏松,它就越容易与活化剂氢氧化钾进行均匀的混合和反应,因此其产物的比表面积也比较高。为了进一步验证这一现象,我们以具有疏松多孔结构的花粉以及具有致密结构的酚醛树脂作为两种原料,对它们进行相同的活化反应并比较了产物的比表面积。结果显示由花粉制备得到的产物的比表面积要远高于由酚醛树脂制备得到的产物的比表面积,证明产物的比表面积确实与原料的结构疏松度确实有很大的关系。此外我们还对系列sp2碳材料的结构进行了详细的表征和计算模拟,结果显示：1,这些sp2碳材料主要是由很多高度扭曲的石墨烯碎片无序搭接而成的；2,对于具有不同比表面积的sp2碳材料产物,其包含的石墨烯碎片的尺寸大小和层数以及堆叠情况是不同的；3,sp2碳材料的比表面积能够超过石墨烯的理论值是因为其边缘碳原子的比例比较高。而在sp2碳材料的六元环共轭结构中引入五元环和七元环以后,sp2碳材料的比表面积不但没有增加,反而会减小。这些结果同样可以适用于其他具有高比表面积的复杂sp2碳材料,如活性碳,因此这不仅对活性碳的结构摸索和研究开辟了新思路,更从根本上解释了sp2碳材料超高比表面积的来源,具有很重要的意义。
3.我们通过调控sp2碳材料制备过程中的反应参数以及改变原料的种类和形貌,制备得到了一系列具有不同比表面积和孔径分布的sp2碳材料,并测试了这些sp2碳材料在两种离子液中的实验比电容值。其中最好的比电容值为220F/g,其基于活性材料的能量密度能达到90Wh/kg以上。同时我们系统地研究了sp2碳材料的比表面积和孔径分布对其超级电容器性能的影响。结果显示各sp2碳材料的实验比电容值与系列sp2碳材料的有效比表面积呈现较好的线性关系,其线性关系的斜率为0.142,线性相关系数为0.96,这说明比表面积和孔径分布对sp2碳材料电容性能都有重要的影响。此外,我们还建立了一种基于sp2碳材料以及离子液电解液的结构模型,并通过几何建模和数学计算分别得到了系列sp2碳材料在两种离子液中的理论比电容值。我们发现系列sp2碳材料的实验比电容值和理论比电容值具有很好的一致性,这说明在衡量sp2碳材料的电容性能时,可以通过这种理论计算模型简单快速地得出其比电容值,而不用组装实际的超级电容器器件。这对快速有效的衡量和筛选适用于超级电容器的高性能sp2碳材料提供了新的途径,具有很重要的意义。
4.我们以氧化石墨烯、硝酸钴和柠檬酸作为原料,利用溶胶凝胶法和“自燃烧”的方法制备得到了石墨烯/钴金属纳米颗粒的复合材料。该复合材料同时具有较好的导电性和铁磁性,在电磁屏蔽和吸波等领域具有很广泛的应用前景。此外,这种通过干凝胶自燃烧制备石墨烯/钴纳米粒子复合材料的方法具有着独特的优点,它不仅操作简单、反应条件温和,而且还具有很强的普适性,可以广泛的适用于其他石墨烯基金属纳米复合材料的制备(比如镍、银或铜等金属纳米粒子),因此具有很重要的意义。
1. Large scale synthesis of graphene with controlled size and layer numbers has been realized by chemical exfoliation method. The impact of graphene size and layer numbers on the electrical conductivity of transparent conductive film electrodes and their specific surface area (SSA) has also been well studied. It is found with increasing amount of oxidants, the size of graphene oxide (GO) is dramatically decreased from20000to550nm2. And if we decrease the amount of oxidants, we can get few layered graphene oxide (FGO) which exhibits both larger size (～1μm) and number of layers (2-4) than single layered GO. Transparent conductive film electrodes based on reduced GO and FGO have been fabricated by spin coating process and chemical or thermal reduction. It is demonstrated that transparent conductive film electrodes based on reduced FGO exhibit much higher electrical conductivity of～480S/m than those based on reduced GO (-38S/m), which indicates that the size and number of layers of graphene have played important roles on the electrical conductivities of transparent conductive film electrodes. Furthermore, based on the results from theoretical calculation and experimental characterizations, we also find out that the size and number of layers in graphene materials have great influence on their SSA. That is, the SSA of graphene materials will highly decrease with increasing size and number of layers, as an example shown in FGO (60m2/g) and GO (4m2/g).
2. Until now, few sp2carbon materials simultaneously exhibit superior performance for SSA and electrical conductivity at bulk state. Thus, by combining the good conductivity of graphene and high SSA of activated carbon, we prepare a series of graphene-based sp2carbon materials at the bulk scale, which exhibit ultrahigh SSA and excellent bulk conductivity. It is found that both the SSA and conductivity of the products can be controlled by varying the proportion between the graphene and activated carbon in the products. The conductivity of the products is increased with increasing amount of graphene. But the SSA of the products is firstly increased but then decreased with increasing amount of graphene. Thorough characterizations have suggested that the structure and morphology of carbon precursors played important roles on the SSA of the products. This is further identified by using porous pollens and firm solid phenolic resin as carbon precursors of activated carbons. And activated carbons based on porous pollens have exhibited much higher SSA than phenolic resin based activated carbons. Furthermore, comprehensive study and structural characterization have been performed for exploring the structure of graphene-based sp2carbon materials and explaining the origin of its ultrahigh specific surface (even higher than the theoretical SSA of graphene,2680m2/g). We conclude that these graphene-based sp2carbon materials consist of mainly defected/wrinkled single layer graphene sheets in the dimensional size of a few nanometers. And the ultrahigh SSA cannot be due to the existence of pentagon and/or heptagon in the graphene-based sp2carbon materials but should mainly come from the edge (or defects) of the graphene sheets with dimensional size of a few nanometers. We believe this should be also applicable to other sp2carbon materials with high SSA, such as activated carbon, thus has important implication for the structural and property study of activated carbon.
3. A series of sp2carbon materials with different SSA and controlled pore size distribution (PSD) were prepared at large scale through a facile and low-cost method. The SSA and PSD of these carbon materials were controlled by adjusting preparation methods and using different carbon sources. Experimental capacitance performance has been tested for all the sp carbon materials and the highest specific capacitance in ionic liquid is220F/g, with an ultrahigh energy density up to90Wh/kg. The impacts of SSA and PSD on their capacitance performance were thoroughly investigated, which demonstrated that both SSA and PSD played the most important role on their effective SSA (E-SSA) and capacitance performance. And a linear relationship has been observed between the E-SSA and experimental specific capacitance, with a coefficient of determination of0.96. Furthermore, a general theoretical model using the slit/cylindrical NL-DFT approach is proposed for the estimation of the specific capacitance of sp2carbon materials, which is in good agreement with the experimental specific capacitance. These results offer a simple but reliable method to predict the capacitance performance of these materials, thus speeding up the designing and screening the materials for high performance supercapacitor and other surface area related devices.
4. A versatile new strategy for producing graphene/cobalt magnetic nanocomposites by combining the sol-gel method and autocombustion is presented. GO, cobalt nitrate and citric acid are used as starting materials and a dry gel of the mixture is prepared through a routine sol-gel approach. The autocombustion reaction was activated at300℃in a tube furnace under an argon atmosphere, which produces lots of reducing agents such as H2and CH4and then in situ reduce GO and cobalt oxide to get graphene/cobalt magnetic nanocomposites. It is demonstrated that the cobalt nanoparticles (but not cobalt oxide) with size of～10nm are homogeneously loaded on graphene sheets. Further more, other metal nanoparticles such as Ni, Cu, Ag and Bi can also be loaded on graphene using the same method, which have great potential for the application on the electromagnetic shield and microwave absorption.
引文
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