石墨烯的宏量制备、可控组装及电化学性能研究
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摘要
石墨烯作为一种新型的二维碳质材料，具有独特的结构特征和优异的电学、力学、光学以及热学性质，在微电子器件、储能、催化、传感器以及功能型复合材料等领域具有广阔的应用前景。然而，目前石墨烯的制备、分散以及精细结构控制还存在很多瓶颈，限制了石墨烯的深入研究以及实用化进程。本论文针对石墨烯的制备以及电化学应用，在材料制备方面重点研究了石墨烯的宏量制备、粉体材料的分散、石墨烯基材料的组装，在应用探索方面重点考察了石墨烯的电化学传感以及电化学储能特性。
在制备方面，论文提出可实现石墨烯粉体材料宏量制备的低温负压化学解理方法。通过对氧化石墨热行为的分析，提出在含氧官能团集中分解的150~250℃区间创造负压环境，造就足够的内外压力差，实现氧化石墨烯片层的充分剥离以及还原。获得的石墨烯材料具有很好的结构完整性，并且以单层为主；石墨烯具有与高温化学解理法所获得石墨烯不同的表面化学，具有较高的电化学比电容。
在分散方面，论文提出使用单链DNA作为分散剂，实现了石墨烯片层的高浓度单分散。组装得到的石墨烯/DNA杂化物可以促进电化学反应中的直接电子转移，并且对双氧水具有良好的电化学响应。同时，使用DNA作为分散剂制备了石墨烯/NiO/DNA杂化物，其作为新型的无酶传感器实现了对葡萄糖的高灵敏度检测，具有检测限低、灵敏度高、稳定性好以及响应时间快等优点。
在二维结构组装方面，论文设计出具有良好离子和电子传输特性，并且具有良好稳定性的石墨烯基层状“三明治”结构。利用石墨烯片层的二维特征以及氧化物纳米颗粒的零维结构特征，通过多步自组装法构建出层状“三明治”结构杂化薄膜；功率以及循环性能测试证明该结构具有很好电化学应用前景。
本论文发现氧化石墨烯作为一种粘结组分，可以将表面活性剂分散的石墨烯片层连接起来，并且在气液界面组装得到了宏观的石墨烯薄膜材料。通过控制氧化石墨烯的含量可以实现对薄膜导电性的调节。
在三维结构组装方面，论文提出一步自组装法，化学还原的氧化石墨烯辅以KMnO_4，在温和条件下组装获得具有核壳复合结构的石墨烯宏观体，其壳由石墨烯薄膜组成，而核则为多孔结构。通过调节KMnO_4浓度，可实现对宏观体结构的调控，该材料表现出良好的电化学行为。在后续工作中，通过在组装过程中引入外力干扰，制备出了小尺寸的石墨烯组装体。
Graphene, as a novel carbon material which is characterized by uniquetwo-dimensional structure and fascinating electronic, thermal, mechanical and opticalproperties, shows great potential in many fields, such as nanoelectronics, energystorage and conversion, catalyst, ultrafast laser system, high sensitivite sensors,composites and so on. However, in-depth research and large scale application ofgraphene are still hindered by some key issues, such as large scale preparation,uniform dispersion of graphene nanosheets and precise structure control ofgraphene-based materials. With a purpose to promote the basic research and realapplication of graphene, this thesis focuses on mass-production and electrochemicalapplications, and the main work includes vacuum-promoted exfoliation from graphiteoxide, efficient dispersion in aqueous solution, controlled construction ofgraphene-based nanostructure and their applications in electrochemical sensors andenergy storage devices.
For the large scale preparation of powdered graphene, a vacuum-promotedexfoliation method at low temperature was for the first time proposed and theobtained graphenes are single-layer dominated and show high quality. Starting withthe investigation of the thermal properties of graphite oxide, we found that most offunctional groups attached to graphite oxide planes were decomposed in a verynarrow range of150~250℃. However, the graphite oxide cannot be fully exfoliatedat such low temperature since the internal force generated by the functional groupsdecomposition is not enough to push the layered strcuture exfoliated. Therefore, weintroduced an outward drawing force at such low temperature and realized fullexfoliation and reduction of graphite oxide layers by creating high vacuumenvironment. Furthermore, the low-temperature exfoliated graphenes show muchhigher capacitance than high-temperature exfoliated ones due to the different surfacechemistry.
We proposed a facile method to realize the single-layer dispersion of graphenepowder in aqueous solution. By using single-stranded DNA as a high efficientdispersing agent, graphene was well dispersed in aqueous solution in highconcentration while graphene/DNA hybrid was obtained by self-assembly simultaneously. This hybrid promotes the electron transfer in the electrocatalysisprocess and shows good response to H2O2. Graphene/NiO/DNA hybrid, which can beused as a nonenzymatic sensor, was also prepared by self-assembly and showssensitive response to glucose. The above two hybrids demonstrate good sensingability, such as large detection ranges, short response periods, low detection limit andhigh sensitivity and stability.
For the two-dimensional graphene-based macrostructure fabrication, we designedand fabricated a membrane-like hybrid with layered sandwich structure conbiningtwo-dimensional graphene layers with zero-dimensional nanoparticles. A muti-stepstrategy that was conducted under ‘‘homogenous’’ and ‘‘mild’’ conditions wasdeveloped to fabricate this hybrid membrane. This structure possesses goodconductivity and open ion transportation channel and is an ideal structure forelectrochemical energy storage with excellent cycling and power performance.
Besides, we found that graphene oxide can be used as a sticking component to linkgraphene sheets together. By introducing graphene oxide in the water dispersedgraphene aided by the surfactant, a macroscopic graphene-based membrane wasfabricated at the liquid-air interface upon heating. The conductivity of suchgraphene-based membrane can be finely tuned by changing the graphene oxidefraction.
For the construction of three-dimensional graphene-based structure, we proposed aone-pot self-assembly process under mild condition and obtained a novelthree-dimensional graphene-based macroassembly with core–shell hybrid structure.Such a hybrid structure is characterized by a porous core and layered membrane shell,and its macro-morphology and infrastructure can be easily tuned by changing theKMnO_4fraction. The prepared assembly shows good electrochemical performanceand improved Coulombic efficiency than powdered graphene. Furthermore, byintroducing the external turbulent force in the assembly process, the macroassemblywith smaller size is obtained.
在制备方面，论文提出可实现石墨烯粉体材料宏量制备的低温负压化学解理方法。通过对氧化石墨热行为的分析，提出在含氧官能团集中分解的150~250℃区间创造负压环境，造就足够的内外压力差，实现氧化石墨烯片层的充分剥离以及还原。获得的石墨烯材料具有很好的结构完整性，并且以单层为主；石墨烯具有与高温化学解理法所获得石墨烯不同的表面化学，具有较高的电化学比电容。
在分散方面，论文提出使用单链DNA作为分散剂，实现了石墨烯片层的高浓度单分散。组装得到的石墨烯/DNA杂化物可以促进电化学反应中的直接电子转移，并且对双氧水具有良好的电化学响应。同时，使用DNA作为分散剂制备了石墨烯/NiO/DNA杂化物，其作为新型的无酶传感器实现了对葡萄糖的高灵敏度检测，具有检测限低、灵敏度高、稳定性好以及响应时间快等优点。
在二维结构组装方面，论文设计出具有良好离子和电子传输特性，并且具有良好稳定性的石墨烯基层状“三明治”结构。利用石墨烯片层的二维特征以及氧化物纳米颗粒的零维结构特征，通过多步自组装法构建出层状“三明治”结构杂化薄膜；功率以及循环性能测试证明该结构具有很好电化学应用前景。
本论文发现氧化石墨烯作为一种粘结组分，可以将表面活性剂分散的石墨烯片层连接起来，并且在气液界面组装得到了宏观的石墨烯薄膜材料。通过控制氧化石墨烯的含量可以实现对薄膜导电性的调节。
在三维结构组装方面，论文提出一步自组装法，化学还原的氧化石墨烯辅以KMnO_4，在温和条件下组装获得具有核壳复合结构的石墨烯宏观体，其壳由石墨烯薄膜组成，而核则为多孔结构。通过调节KMnO_4浓度，可实现对宏观体结构的调控，该材料表现出良好的电化学行为。在后续工作中，通过在组装过程中引入外力干扰，制备出了小尺寸的石墨烯组装体。
Graphene, as a novel carbon material which is characterized by uniquetwo-dimensional structure and fascinating electronic, thermal, mechanical and opticalproperties, shows great potential in many fields, such as nanoelectronics, energystorage and conversion, catalyst, ultrafast laser system, high sensitivite sensors,composites and so on. However, in-depth research and large scale application ofgraphene are still hindered by some key issues, such as large scale preparation,uniform dispersion of graphene nanosheets and precise structure control ofgraphene-based materials. With a purpose to promote the basic research and realapplication of graphene, this thesis focuses on mass-production and electrochemicalapplications, and the main work includes vacuum-promoted exfoliation from graphiteoxide, efficient dispersion in aqueous solution, controlled construction ofgraphene-based nanostructure and their applications in electrochemical sensors andenergy storage devices.
For the large scale preparation of powdered graphene, a vacuum-promotedexfoliation method at low temperature was for the first time proposed and theobtained graphenes are single-layer dominated and show high quality. Starting withthe investigation of the thermal properties of graphite oxide, we found that most offunctional groups attached to graphite oxide planes were decomposed in a verynarrow range of150~250℃. However, the graphite oxide cannot be fully exfoliatedat such low temperature since the internal force generated by the functional groupsdecomposition is not enough to push the layered strcuture exfoliated. Therefore, weintroduced an outward drawing force at such low temperature and realized fullexfoliation and reduction of graphite oxide layers by creating high vacuumenvironment. Furthermore, the low-temperature exfoliated graphenes show muchhigher capacitance than high-temperature exfoliated ones due to the different surfacechemistry.
We proposed a facile method to realize the single-layer dispersion of graphenepowder in aqueous solution. By using single-stranded DNA as a high efficientdispersing agent, graphene was well dispersed in aqueous solution in highconcentration while graphene/DNA hybrid was obtained by self-assembly simultaneously. This hybrid promotes the electron transfer in the electrocatalysisprocess and shows good response to H2O2. Graphene/NiO/DNA hybrid, which can beused as a nonenzymatic sensor, was also prepared by self-assembly and showssensitive response to glucose. The above two hybrids demonstrate good sensingability, such as large detection ranges, short response periods, low detection limit andhigh sensitivity and stability.
For the two-dimensional graphene-based macrostructure fabrication, we designedand fabricated a membrane-like hybrid with layered sandwich structure conbiningtwo-dimensional graphene layers with zero-dimensional nanoparticles. A muti-stepstrategy that was conducted under ‘‘homogenous’’ and ‘‘mild’’ conditions wasdeveloped to fabricate this hybrid membrane. This structure possesses goodconductivity and open ion transportation channel and is an ideal structure forelectrochemical energy storage with excellent cycling and power performance.
Besides, we found that graphene oxide can be used as a sticking component to linkgraphene sheets together. By introducing graphene oxide in the water dispersedgraphene aided by the surfactant, a macroscopic graphene-based membrane wasfabricated at the liquid-air interface upon heating. The conductivity of suchgraphene-based membrane can be finely tuned by changing the graphene oxidefraction.
For the construction of three-dimensional graphene-based structure, we proposed aone-pot self-assembly process under mild condition and obtained a novelthree-dimensional graphene-based macroassembly with core–shell hybrid structure.Such a hybrid structure is characterized by a porous core and layered membrane shell,and its macro-morphology and infrastructure can be easily tuned by changing theKMnO_4fraction. The prepared assembly shows good electrochemical performanceand improved Coulombic efficiency than powdered graphene. Furthermore, byintroducing the external turbulent force in the assembly process, the macroassemblywith smaller size is obtained.
引文
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