石墨烯材料的化学调控、组装及其性能研究
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摘要
氧化石墨烯(GO)为大规模制备石墨烯基材料提供了可能,还原GO制备还原石墨烯(rGO)是一个重要而充满挑战的课题。在本论文的第二章中,我们以DMAc/H2O混合溶剂分散GO,研究了其溶剂热还原的效果,常规的油浴加热以及微波加热作为热源分别进行了研究。反应温度不超过160°C。采用FT-IR,XRD,AFM,XPS, Raman和TGA测试表明在该温度下,GO已经发生脱氧,生产了热还原石墨烯。以微波为加热源条件下,反应可以在10min内完成。制备的石墨烯材料可以再经过超声分散到DMAc溶剂中形成稳定的分散液。抽滤获得热还原石墨烯纸的电导率达～200S/m,比原料GO纸要高104倍。该工作为在加热条件下使用氧化石墨烯材料的小组提供很好的参考价值。
为了能进一步提高GO的还原效果,我们采用化学还原剂还原。在第三章中,采用了一系列含硫化合物诸如NaHSO3, SOC12和S02替代水合肼用于还原GO制备还原石墨烯。FT-IR,TGA和XPS等测试表明经过95℃下化学还原生产了石墨烯,并且NaHSO3的还原能力与水合肼相当。我们提出了NaHSO3还原过程可能存在的还原机理。NaHSO3还原石墨烯,经抽滤制备的石墨烯纸电导率达到6500S/m,而相同条件下水合肼还原的样品为5100S/m。因而NaHSO3有可能替代水合肼作为还原GO的还原剂。
在GO还原过程中,如果处在强还原条件下有可能会在GO上发生氢化现象,生产C-H结构。在第四章中,我们发现了一种制备氢化石墨烯的新方法。将GO溶液置于60Co产生的γ射线下,在室温下经过辐照就可以生成氢化的还原石墨烯。该过程中GO被水合电子(eaq-)以及H自由基还原并加氢。制得的氢化还原石墨烯中最大氢化程度达到5.27wt.%,即H/C=0.76。该过程可以大规模制备出氢化的还原石墨烯。制备的氢化石墨烯作为离子电池负极材料使用,性能表现良好。
如何将微米级别的石墨烯片拼接组装成宏观尺度上的结构体,这对于开发石墨烯材料的应用非常重要。其中的一个发展方向便是应用范围广泛的三维石墨烯材料。在第五章中,我们在95℃常压下,原位还原自组装制备出了3D石墨烯材料-石墨烯水凝胶。该过程无需另加化学或者物理交联剂。制备的石墨烯水凝胶经过冷冻干燥处理获得石墨烯气凝胶,通过控制反应器形状可以达到控制3D石墨烯形状的目的。石墨烯水凝胶可应用于超级电容器,测试表明比电容高达160F/g。而石墨烯气凝胶具有质量轻、强度高、热稳定性好以及导电率高等优点。3D结构的石墨烯在超级电容器、油吸附材料以及催化剂载体等方面有巨大潜在用途。
3D石墨烯结构的独特性来自于基本组成单元——2D结构的石墨烯片,赋予该材料巨大的表面积可以与其他材料复合。以GO溶液为原料,可以方便地制备出3D石墨烯复合结构体。在第六章中,采用一步还原自组装的方法,以化学还原中收缩的石墨烯片层网络富集Fe304纳米颗粒,制得了石墨烯/Fe304复合气凝胶,该过程像撒网捕鱼一般。获得的材料具有多孔、质量轻和超顺磁性的特点。将石墨烯/Fe304复合材料用于锂离子电池负极,表现出了优异的电化学性能,在经过50次充放电循环后比容量依然高达1100mAh g-1。该方法也适用于其他3D石墨烯复合材料的制备。
通过控制石墨烯气凝胶的多孔结构我们可以获得不同的石墨烯结构体。在第七章中,我们采用冰模板的方法,制备了柔性大孔结构的3D石墨烯海绵。通过控制结冰的速率,可以达到控制3D石墨烯孔径结构的目的。在低结冰速率下,石墨烯水凝胶中的片层进行了再组装,形成多层次结构,冷冻干燥后获得多大孔结构海绵。制备的石墨烯海绵具有良好弹性能从50%形变中复原。将该石墨烯海绵应用于微生物燃料电池阳极,最大输出能量密度达427Wm-3,表现超过了相同条件下的碳毡。
如何将微米基本的GO片组装成宏观的膜结构材料一直是石墨烯加工领域所面临的挑战。从材料的角度来看泡泡膜,它们其实是很好的超薄膜模板。在第八章中,我们发展了一种制备自支撑GO超薄膜的新方法,维持GO泡泡膜稳定下干燥获得。制备的GO膜可以方便地转移到需要基底上。在经过化学还原和高温还原后,所制备rGO膜表现出了良好的电导率(920Ω□-1),该材料有望用于替代ITO和FTO,此外化学还原rGO膜可以用于柔性导电透明材料。该方法也望用于其他类石墨烯二维材料自支撑超薄膜的制备。
通常GO的还原在加热条件下进行,需要输入能量。事实上,溶液中GO的还原是一个消耗电子和质子脱氧的过程,GO扮演了去极化剂的作用。那么我们能否再还原GO的过程中导出能量呢?在第九章中,以锌片为负极,GO为正极,构建了Zn-GO的原电池。在还原GO的过程中可以同时导出电子对外做功。测得的电池容量与GO的氧化程度相关,在平均电压超过0.6V时,电容量在216到642mAh g-1之间。阻抗谱测试表明,放电过程中Zn/GO电池电阻在减小。GO膜的放电过程中存在着类似多米诺效应的现象。组装的原电池可以点亮LED灯,表明其有实际应用的可能。
受GO膜还原中的多米诺效应启发,在第十章中我们发现可以采用电化学方法来对GO结构体的进行还原。在此过程中,由于存在移动的三相界线,点或者线接触都可以触发GO结构体的整体还原,通常认为的面面接触并不是必要条件。我们制备了从1D石墨烯复合线,2D石墨烯复合纸与石墨烯透明导电膜(64%透光率,1.8KΩ□-1),3D石墨烯复合海绵,都展现了良好的导电性。测得还原后的石墨烯膜电导率为28200S/m,媲美HI和高温热还原。
Graphene oxide (GO) provides possible to prepare graphene based materials in large scale. Reduction of graphene oxide to reduced graphene oxide (rGO) is one important and challenging topic. In Chapter II, we studied the solvent thermal reduction of graphene oxide in mixture DMAc/H2O solvent under atmosphere press, both bath heating and microwave heating were employed, respectively. The reaction temperature is below160℃. FT-IR, XRD, AFM, XPS, Raman, and TGA measurements reveal that deoxygenation of GO occurs under the mild thermal conditions, yielding rGO. For micarowave as heating source, the reduction time is within10minutes, and the as-prepared rGO can be well dispersed in DMAc to form a stable suspension. The conductivity of reduced graphene paper was measured about200S/m,104times higher than that of GO paper.
For a more high extent of reduction for graphene oxide, chemical reducing agents are used. In Chapter III, instead of hydrazine, sulfur-containing compounds such as NaHSO3, SOCl2and SO2et al. were used to reduce graphene oxide to chemical reduced graphene oxide. FT-IR, TGA, XPS et al. measurements confirmed the formation of rGO under chemical reduction at95℃. The results reveal that the reducing ability of NaHSO3is comparable to that of hydrazine. A possible mechanism of the reduction has been suggested. The electrical conductivity of the rGO paper prepared using a NaHSO3reducing agent is found to be6500Sm-1while it is observed to be5100Sm-1for hydrazine reduced graphene paper. These studies confirm that NaHSO3can be a good candidate as a reducing agent to compete with hydrazine
Hydrogenation of GO also may occur during its reduction at strong reducing conditions, forming C-H group in GO plane. In Chapter IV, we found a novel method to prepare hydrogenated graphene (HG) via a direct synchronal reduction and hydrogenation of graphene oxide (GO) in aqueous suspension under60Co gamma rays irradiation at room temperature. GO can be reduced by the aqueous electron (eaq-) while the hydrogenation takes place by the hydrogen radicals formed in-situ under irradiation. The maximum hydrogen content of the as-prepared highly hydrogenated graphene (HHG) is found to be5.27wt%with H/C=0.76. The yield of the target product is in gram scale and is promising for large scale prepartion. The as prepared HHG also shows high performance as anode materials for lithium ion batteries.
It is important to assembly the micrometers size graphene sheets into macroscopic architechures for more applications. Three-dimensional (3D) architecture of graphene is significant important. In Chapter V, a mild method for preparation of3D architectures of graphene is developed via an in situ self-assembly of rGO nanosheets that were in-situ formed by a mild chemical reduction at95℃under atmosphere pressure without stirring. No chemical or physical cross-linkers and high press are required. Graphene aerogels can be prepared by freeze-drying of graphene hydrogels, and the shapes of the3D architectures can be controlled by changing the types of the reactors. The graphene hydrogel shows high specific capacitance(～160F/g) in supercapacitor. Graphene aerogels are in low density, high mechanical properties, thermal stability and high electrical conductivity.3D graphene architectures are good candidates for potential application in supercapacitors, oil sorbents and catalysts supports.
The unique structure of3D graphene architectures comes from the building units-2D graphene sheets, providing extremely large area for combination with other components. Hybrid3D graphene architectures can be easily prepared during self-assembly in aqueous from the well dispersed GO sheets. In Chapter VI, electrical conductive magnetic graphene/Fe3O4aerogel has been successfully prepared by the one-step reduction and self-assembly of the mixture of GO in the present of Fe3O4nanoparticles, and the assembly process looks like the fishing process. The obtained gel is superparamagnetic, porous and light weight. Graphene/Fe3O4composite can be used as anode materials for LIBs, and it shows good electrochemical performance,1100mAh g-1after50cycles of charging/discharging. This study is a base for developing new3D graphene/nanoparticles for wide applications in near future.
More different graphene architectures can be prepared if we control the porous structure of graphene aerogels. A simple and effective method for the fabrication of flexible macroporous3D graphene sponge using ice template is developed in Chapter Ⅶ. It is found that the porous structures of the3D graphene architecture depended on the rate of ice crystal formation. At a low cooling rate, the inner walls of the graphene hydrogel are re-assembled into hierarchical macroporous structure by the as-formed ice crystals, resulting in the formation of macroporous graphene sponge after freeze-drying. The as-prepared graphene sponge is flexible and can recover from a50%deformation. As the graphene sponge is used as the anode of a microbial fuel cell (MFC), the maximum power density reaches427.0W m-3, which is higher than that of the MFC fabricated using carbon felt as the anode material.
Assembling micrometers size graphene oxide sheets into macroscopic film is another challenge for graphene fabrication. Foam film acts as template for ultrathin film fabrication if it is seen in a material view. In Chapter Ⅷ, we developed a novel method for the fabrication of macroscopic free-standing ultrathin films of GO through the route of the preparation dried foam films. The prepared GO thin film can be easily transferred to any substrates. After chemical or thermal reduction, the relative rGO film with highly electrical conductivity (920Ω□-1) was prepared, which has potential application as electrode materials to replace of ITO or FTO in flexible photoelectric devices. This method is also suitable for2D graphene-like material free-standing ultrathin films fabrication.
Generally, the reduction of graphene oxide is conducted in heating condition, where energy is put-in. In fact, the reduction of GO in aqueous is a deoxygenation process with cost of electron and proton, during which GO plays the role of depolarizer. Can we out-put the energy during the reduction of GO? In Chapter IX, a primary battery has been fabricated, where Zn plate as anode and graphene oxide (GO) as cathode, and the electron-output has been achieved while a reduced graphene oxided (rGO) film was obtained synchronously. The output capacities of the batteries depend on the oxygenated degree and the amount of GO, and their specific capacity ranged from216to642mAh g-1while the average voltage is up0.6V. Electrochemical impedance spectroscopy (EIS) measurements reveal the decreasing resistance of Zn/GO cell during discharging process. And a domino-like process was observed during the discharging of GO film. A LED lamp can be ignited by the battery, indicating its potential for practical application.
Inspired by the domino-like process during the chemical reduction of dried GO foam film in Zn-GO primary cell, we found electrochemical reduction method can be a general route for highly reduction of GO architectures in Chapter X. Point or line contacting can lead to the overall reduction of GO architectures for the moving three phase lines (3PIs), where face contact is not necessary. We fabricated1D graphene/cellulose line,2D graphene film/paper composite and3D graphene/sponge composite, and all showed excellent conductivity. The reduced graphene film gains conductivity of28200S/m, comparable with reduced by HI or thermal annealing, while this method is mild and green. We also prepared flexible graphene film on PET of large area, showing64%transparency with low resistance of1.8KΩ□-1.
为了能进一步提高GO的还原效果,我们采用化学还原剂还原。在第三章中,采用了一系列含硫化合物诸如NaHSO3, SOC12和S02替代水合肼用于还原GO制备还原石墨烯。FT-IR,TGA和XPS等测试表明经过95℃下化学还原生产了石墨烯,并且NaHSO3的还原能力与水合肼相当。我们提出了NaHSO3还原过程可能存在的还原机理。NaHSO3还原石墨烯,经抽滤制备的石墨烯纸电导率达到6500S/m,而相同条件下水合肼还原的样品为5100S/m。因而NaHSO3有可能替代水合肼作为还原GO的还原剂。
在GO还原过程中,如果处在强还原条件下有可能会在GO上发生氢化现象,生产C-H结构。在第四章中,我们发现了一种制备氢化石墨烯的新方法。将GO溶液置于60Co产生的γ射线下,在室温下经过辐照就可以生成氢化的还原石墨烯。该过程中GO被水合电子(eaq-)以及H自由基还原并加氢。制得的氢化还原石墨烯中最大氢化程度达到5.27wt.%,即H/C=0.76。该过程可以大规模制备出氢化的还原石墨烯。制备的氢化石墨烯作为离子电池负极材料使用,性能表现良好。
如何将微米级别的石墨烯片拼接组装成宏观尺度上的结构体,这对于开发石墨烯材料的应用非常重要。其中的一个发展方向便是应用范围广泛的三维石墨烯材料。在第五章中,我们在95℃常压下,原位还原自组装制备出了3D石墨烯材料-石墨烯水凝胶。该过程无需另加化学或者物理交联剂。制备的石墨烯水凝胶经过冷冻干燥处理获得石墨烯气凝胶,通过控制反应器形状可以达到控制3D石墨烯形状的目的。石墨烯水凝胶可应用于超级电容器,测试表明比电容高达160F/g。而石墨烯气凝胶具有质量轻、强度高、热稳定性好以及导电率高等优点。3D结构的石墨烯在超级电容器、油吸附材料以及催化剂载体等方面有巨大潜在用途。
3D石墨烯结构的独特性来自于基本组成单元——2D结构的石墨烯片,赋予该材料巨大的表面积可以与其他材料复合。以GO溶液为原料,可以方便地制备出3D石墨烯复合结构体。在第六章中,采用一步还原自组装的方法,以化学还原中收缩的石墨烯片层网络富集Fe304纳米颗粒,制得了石墨烯/Fe304复合气凝胶,该过程像撒网捕鱼一般。获得的材料具有多孔、质量轻和超顺磁性的特点。将石墨烯/Fe304复合材料用于锂离子电池负极,表现出了优异的电化学性能,在经过50次充放电循环后比容量依然高达1100mAh g-1。该方法也适用于其他3D石墨烯复合材料的制备。
通过控制石墨烯气凝胶的多孔结构我们可以获得不同的石墨烯结构体。在第七章中,我们采用冰模板的方法,制备了柔性大孔结构的3D石墨烯海绵。通过控制结冰的速率,可以达到控制3D石墨烯孔径结构的目的。在低结冰速率下,石墨烯水凝胶中的片层进行了再组装,形成多层次结构,冷冻干燥后获得多大孔结构海绵。制备的石墨烯海绵具有良好弹性能从50%形变中复原。将该石墨烯海绵应用于微生物燃料电池阳极,最大输出能量密度达427Wm-3,表现超过了相同条件下的碳毡。
如何将微米基本的GO片组装成宏观的膜结构材料一直是石墨烯加工领域所面临的挑战。从材料的角度来看泡泡膜,它们其实是很好的超薄膜模板。在第八章中,我们发展了一种制备自支撑GO超薄膜的新方法,维持GO泡泡膜稳定下干燥获得。制备的GO膜可以方便地转移到需要基底上。在经过化学还原和高温还原后,所制备rGO膜表现出了良好的电导率(920Ω□-1),该材料有望用于替代ITO和FTO,此外化学还原rGO膜可以用于柔性导电透明材料。该方法也望用于其他类石墨烯二维材料自支撑超薄膜的制备。
通常GO的还原在加热条件下进行,需要输入能量。事实上,溶液中GO的还原是一个消耗电子和质子脱氧的过程,GO扮演了去极化剂的作用。那么我们能否再还原GO的过程中导出能量呢?在第九章中,以锌片为负极,GO为正极,构建了Zn-GO的原电池。在还原GO的过程中可以同时导出电子对外做功。测得的电池容量与GO的氧化程度相关,在平均电压超过0.6V时,电容量在216到642mAh g-1之间。阻抗谱测试表明,放电过程中Zn/GO电池电阻在减小。GO膜的放电过程中存在着类似多米诺效应的现象。组装的原电池可以点亮LED灯,表明其有实际应用的可能。
受GO膜还原中的多米诺效应启发,在第十章中我们发现可以采用电化学方法来对GO结构体的进行还原。在此过程中,由于存在移动的三相界线,点或者线接触都可以触发GO结构体的整体还原,通常认为的面面接触并不是必要条件。我们制备了从1D石墨烯复合线,2D石墨烯复合纸与石墨烯透明导电膜(64%透光率,1.8KΩ□-1),3D石墨烯复合海绵,都展现了良好的导电性。测得还原后的石墨烯膜电导率为28200S/m,媲美HI和高温热还原。
Graphene oxide (GO) provides possible to prepare graphene based materials in large scale. Reduction of graphene oxide to reduced graphene oxide (rGO) is one important and challenging topic. In Chapter II, we studied the solvent thermal reduction of graphene oxide in mixture DMAc/H2O solvent under atmosphere press, both bath heating and microwave heating were employed, respectively. The reaction temperature is below160℃. FT-IR, XRD, AFM, XPS, Raman, and TGA measurements reveal that deoxygenation of GO occurs under the mild thermal conditions, yielding rGO. For micarowave as heating source, the reduction time is within10minutes, and the as-prepared rGO can be well dispersed in DMAc to form a stable suspension. The conductivity of reduced graphene paper was measured about200S/m,104times higher than that of GO paper.
For a more high extent of reduction for graphene oxide, chemical reducing agents are used. In Chapter III, instead of hydrazine, sulfur-containing compounds such as NaHSO3, SOCl2and SO2et al. were used to reduce graphene oxide to chemical reduced graphene oxide. FT-IR, TGA, XPS et al. measurements confirmed the formation of rGO under chemical reduction at95℃. The results reveal that the reducing ability of NaHSO3is comparable to that of hydrazine. A possible mechanism of the reduction has been suggested. The electrical conductivity of the rGO paper prepared using a NaHSO3reducing agent is found to be6500Sm-1while it is observed to be5100Sm-1for hydrazine reduced graphene paper. These studies confirm that NaHSO3can be a good candidate as a reducing agent to compete with hydrazine
Hydrogenation of GO also may occur during its reduction at strong reducing conditions, forming C-H group in GO plane. In Chapter IV, we found a novel method to prepare hydrogenated graphene (HG) via a direct synchronal reduction and hydrogenation of graphene oxide (GO) in aqueous suspension under60Co gamma rays irradiation at room temperature. GO can be reduced by the aqueous electron (eaq-) while the hydrogenation takes place by the hydrogen radicals formed in-situ under irradiation. The maximum hydrogen content of the as-prepared highly hydrogenated graphene (HHG) is found to be5.27wt%with H/C=0.76. The yield of the target product is in gram scale and is promising for large scale prepartion. The as prepared HHG also shows high performance as anode materials for lithium ion batteries.
It is important to assembly the micrometers size graphene sheets into macroscopic architechures for more applications. Three-dimensional (3D) architecture of graphene is significant important. In Chapter V, a mild method for preparation of3D architectures of graphene is developed via an in situ self-assembly of rGO nanosheets that were in-situ formed by a mild chemical reduction at95℃under atmosphere pressure without stirring. No chemical or physical cross-linkers and high press are required. Graphene aerogels can be prepared by freeze-drying of graphene hydrogels, and the shapes of the3D architectures can be controlled by changing the types of the reactors. The graphene hydrogel shows high specific capacitance(～160F/g) in supercapacitor. Graphene aerogels are in low density, high mechanical properties, thermal stability and high electrical conductivity.3D graphene architectures are good candidates for potential application in supercapacitors, oil sorbents and catalysts supports.
The unique structure of3D graphene architectures comes from the building units-2D graphene sheets, providing extremely large area for combination with other components. Hybrid3D graphene architectures can be easily prepared during self-assembly in aqueous from the well dispersed GO sheets. In Chapter VI, electrical conductive magnetic graphene/Fe3O4aerogel has been successfully prepared by the one-step reduction and self-assembly of the mixture of GO in the present of Fe3O4nanoparticles, and the assembly process looks like the fishing process. The obtained gel is superparamagnetic, porous and light weight. Graphene/Fe3O4composite can be used as anode materials for LIBs, and it shows good electrochemical performance,1100mAh g-1after50cycles of charging/discharging. This study is a base for developing new3D graphene/nanoparticles for wide applications in near future.
More different graphene architectures can be prepared if we control the porous structure of graphene aerogels. A simple and effective method for the fabrication of flexible macroporous3D graphene sponge using ice template is developed in Chapter Ⅶ. It is found that the porous structures of the3D graphene architecture depended on the rate of ice crystal formation. At a low cooling rate, the inner walls of the graphene hydrogel are re-assembled into hierarchical macroporous structure by the as-formed ice crystals, resulting in the formation of macroporous graphene sponge after freeze-drying. The as-prepared graphene sponge is flexible and can recover from a50%deformation. As the graphene sponge is used as the anode of a microbial fuel cell (MFC), the maximum power density reaches427.0W m-3, which is higher than that of the MFC fabricated using carbon felt as the anode material.
Assembling micrometers size graphene oxide sheets into macroscopic film is another challenge for graphene fabrication. Foam film acts as template for ultrathin film fabrication if it is seen in a material view. In Chapter Ⅷ, we developed a novel method for the fabrication of macroscopic free-standing ultrathin films of GO through the route of the preparation dried foam films. The prepared GO thin film can be easily transferred to any substrates. After chemical or thermal reduction, the relative rGO film with highly electrical conductivity (920Ω□-1) was prepared, which has potential application as electrode materials to replace of ITO or FTO in flexible photoelectric devices. This method is also suitable for2D graphene-like material free-standing ultrathin films fabrication.
Generally, the reduction of graphene oxide is conducted in heating condition, where energy is put-in. In fact, the reduction of GO in aqueous is a deoxygenation process with cost of electron and proton, during which GO plays the role of depolarizer. Can we out-put the energy during the reduction of GO? In Chapter IX, a primary battery has been fabricated, where Zn plate as anode and graphene oxide (GO) as cathode, and the electron-output has been achieved while a reduced graphene oxided (rGO) film was obtained synchronously. The output capacities of the batteries depend on the oxygenated degree and the amount of GO, and their specific capacity ranged from216to642mAh g-1while the average voltage is up0.6V. Electrochemical impedance spectroscopy (EIS) measurements reveal the decreasing resistance of Zn/GO cell during discharging process. And a domino-like process was observed during the discharging of GO film. A LED lamp can be ignited by the battery, indicating its potential for practical application.
Inspired by the domino-like process during the chemical reduction of dried GO foam film in Zn-GO primary cell, we found electrochemical reduction method can be a general route for highly reduction of GO architectures in Chapter X. Point or line contacting can lead to the overall reduction of GO architectures for the moving three phase lines (3PIs), where face contact is not necessary. We fabricated1D graphene/cellulose line,2D graphene film/paper composite and3D graphene/sponge composite, and all showed excellent conductivity. The reduced graphene film gains conductivity of28200S/m, comparable with reduced by HI or thermal annealing, while this method is mild and green. We also prepared flexible graphene film on PET of large area, showing64%transparency with low resistance of1.8KΩ□-1.
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