石墨烯基复合材料的制备与性能研究
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摘要
石墨烯是目前已知材料中厚度最薄、强度最大的材料，完美的石墨烯是由单层碳原子组成的六边形晶格结构二维碳质材料，展示出电子在内部的优异流动性以及优良的导热性能及刚度。由于石墨烯具有特殊的物理、化学性质以及优异的结构特性，已经在全世界范围内引起了一股新的研究热潮。基于石墨烯的材料已在催化、光学、电子学、磁学、传感器、储能等诸多领域显示出了巨大的应用潜能。本论文中将在分析石墨烯近期的研究和应用成果基础之上，开展新型的石墨烯及石墨烯基复合材料的构筑，深入研究石墨烯及石墨烯基复合材料的光、电催化以及抑菌性能，揭示材料的特殊结构与优异性能之间的关系，并对材料的光、电催化以及抑菌机理进行较为深入的研究。
采用淬火技术同步剥离与还原膨胀石墨制备高质量、高产率的石墨烯。XPS、Raman等测试结果表明通过水合肼或浓氨水辅助的淬火过程能够有效减少石墨烯表面的含氧基团，导电原子力分析表明石墨烯具有优异的导电性能。膨胀石墨层间存在大量插层化合物，通过淬火应力能够剥离膨胀石墨形成石墨烯片，高质量的石墨烯可以作为良好的载体材料构筑石墨烯基复合体。设计一种简单的浓氨水辅助水热合成法制备氮掺杂石墨烯。在还原氧化石墨的同时实现石墨烯的氮掺杂，氮掺杂石墨烯显示出较高的氮掺杂量（7.2%）以及较好的稳定性，同时氮掺杂石墨烯也显示出比石墨烯更优异的电容特性，比电容的最高值为144.6F/g。通过此种方法可以合成出具有广泛应用前景的高品质氮掺杂石墨烯，也为改善和提高超级电容器的电容特性以及稳定性提供了一种新的选择。
通过合适初级纳米粒子在膨胀石墨层间原位生长，利用初级纳米粒子生长力剥离膨胀石墨的同时与石墨烯复合构筑石墨烯基复合材料，石墨烯片的引入明显提高锐钛型TiO_2纳米晶的热稳定性，同时TiO_2自身的光生载流子分离效率提高，光催化性能研究表明复合材料不论在可见光还是紫外光下均比P25的催化活性要优异，在可见光下苯酚的降解率为62%，而在紫外光下苯酚的降解率为81%。为合成高性能的石墨烯基光催化剂提供了新颖的实验方法。采用HF和甲醇的溶剂热体系，一步合成新颖的石墨烯/暴露{001}高能面TiO_2复合体，利用复合体进一步深入探究TiO_2和C之间的电子转移行为，揭示二者之间的电子转移过程对进一步理解光催化机制具有指导意义。XPS结果表明TiO_2与石墨烯之间存在较强的相互作用以及电子转移行为。XANES进一步说明复合体中电子转移的途径与方向，这种电子转移行为能够对载流子分离效率的提高具有积极作用，利于光催化性能的提高。通过光催化性能评价发现石墨烯/暴露{001}高能面TiO_2复合体显示出比P25优异的紫外光催化活性。
通过简单的原位化学还原方法制备Ag/石墨烯复合结构，实验结果表明大约8～10μm的石墨片表面均匀生长着直径约为45nm的银纳米粒子。并在此基础上以大肠杆菌为受试菌株，用抑菌圈法测试Ag/石墨烯复合体的抑菌效果，实验结果表明Ag/石墨烯复合体对大肠杆菌具有优异的抑菌性能，可能归因于高质量石墨烯的引入使得Ag纳米颗粒的分散性提高，同时也提高了Ag纳米颗粒的光照稳定性，Ag纳米粒子与石墨烯片协同效应共同促进抑菌性能的明显提高。
通过几种新颖的方法制备了新型的石墨烯及石墨烯基复合材料，研究复合材料各组分之间的相互作用机理，探索复合材料结构与性能之间关系，丰富石墨烯及石墨烯基复合材料相关领域的基础理论，从而为实现相关材料的实际应用奠定坚实基础。
Graphene has attracted increasing attention because its unique nanostructure holds greatpromise for potential applications in different fields such as photocatalysis, sensors, batteriesand supercapacitors. Graphene sheets, one-atom-thick two-dimensional layers of sp2-bondedcarbon, are predicted to have a range of unusual properties. Their thermal conductivity andmechanical stiffness may rival the remarkable in-plane values for graphite; theirfracturestrength should be comparable to that of carbon nanotubes for similar types of defects;and recent studies have shown that individual graphene sheets have extraordinary electronictransport properties. One possible route to harnessing these propertiesfor applications wouldbe to incorporate graphene sheets in acomposite material. The manufacturing of suchcomposites requires not only that graphene sheets be produced on a sufficient scale but thatthey also be incorporated, and homogeneously distributed, into various matrices. The mainresearch contents of thesis are shown as follows:
Recently, single-or few-layer graphene sheets had been prepared by several methods.However, the low productivity of the micromechanical exfoliation makes it unsuitable forlarge-scale use. The functionalization of GO disrupts the electronic structure of graphene.Thus, facile and efficient strategy to produce high quality and large yield graphene is urgentlyrequired. Quenching technology is an important operation in the final fabrication process ofany engineering component. We can make full use of quenching stress to exfoliate graphitelayers for the production of graphene. In the first part, we presented a high-efficient hydrazinehydrate or concentrated ammonia-assisted quenching route to prepare the high qualitygraphenes. The success process was attributed to the strong quenching and presence ofhydrazine hydrate or concentrated ammonia. The strategy is promising due to its facileoperation, rapid production and low-cost starting materials.
Supercapacitors have attracted increasing attention as alternative energy-storage systems.Up to now, carbon nanomaterials such as porous carbon materials and carbon nanotubes havebeen used as supercapacitors electrodes due to their large surface areas and highconductivities. The capacitive behavior of carbon materials can be further improved by thepresence of active species that contribute to the total specific capacitance by the pseudocapacitive effect. In this work, we developed a concentrate ammonia-assistedhydrothermal method to obtain N-doped graphene sheets by simultaneous N-doping andreduction of graphene oxide (GO) sheets. The effects of hydrothermal temperature on surfacechemistry and structure of the N-doped graphene sheets were also investigated. N bindingconfigurations of sample consist of pyridine N, quaternary N, and pyridine-N oxides. Thesample exhibits excellent thermal stability. Electrical measurements demonstrate that productsshow higher capacitive performance than that of pure graphene that ascribe thepseudocapacitive effect from the N-doping. The samples also show excellent long-term cyclestability of capacitive performance.
We present a facile route to prepare TiO_2-graphene composites by in situ growth of TiO_2ininterlayer of low-cost expanded graphite (EG) under solvothermal. The vacuum-assistanttechnology associated with the use of surfactant (cetyltrimethylammonium bromides) plays akey role in the fabrication of such composites. Firstly, the vacuum environment promotes theinitial solution containing Ti(OBu)4, and the surfactant fully infusing into the interlayer of EG;subsequently, numerous nanoparticles of TiO_2in situ uniformly grow in interlayer with thehelp of surfactant, facilitates the EG exfoliation; in the mean time, EG by the aid of theethanol solvothermal, eventually forming the TiO_2-graphene composites. The as-preparedsamples have been characterized by Raman, SEM, TEM, AFM, FT-IR, and thermogravimeticanalysis. It is shown that a large number of TiO_2nanoparticles homogeneously cover thesurface of high-quality graphene sheets. The graphene exhibits multi-layered structure(five~seven layers). Noticeably, the synthesized TiO_2-graphene by post thermal treatment athigh temperature under nitrogen show high photocatalytic activity to degrade phenol undervisible and UV light in comparison with bare P25. The enhanced photocatalytic performanceis attributed to the increased charge separation, the strengthened light absorbance and lightabsorption width, and the fine adsorptivity for pollutants.
A simply and feasible strategy to synthesize the novel anatase TiO_2/graphene compositeswith exposed TiO_2{001} high-energy facets by the hydrofluoric acid-and methanol-jointassisted solvothermal reactions. During the synthesis process, graphene were uniformlycovered with a large number anatase TiO_2nanoparticles, exposing the {001} facets. TheX-ray photoelectron spectroscopy (XPS) and X-ray absorption (XAS) measurements show the presence of electron transfer between TiO_2and graphene. Furthermore, transient photovoltage(TPV) spectra of the composite also exhibits prolonged mean lifetime of electron-hole pairscompared with pure TiO_2. The electron transfer between Ti and C will greatly retard therecombination of photoinduced charge carriers and prolong electron lifetime, whichcontributing to the enhancement of photocatalytic performance. During the photocatalysismeasurement, the TiO_2/graphene composites have high photocatalytic activity compared withthe P25under UV light, likely due to the effective separation of photoinduced charge andexposure of high reactive {001} facets.
A novel Ag/graphene composite antibacterial agent was synthesized through a facilechemical reduction method. The high quality graphene was selected as the carbon substratefor supporting Ag particles. The composite had been characterized by high-resolutiontransmission electron microscopy and scanning electron microscopy. The results show thatabout45~50nm Ag nanoparticles are uniformly dispersed on the surface of the graphene. Theantibacterial activity of composite is investigated using the agar well diffusion method. Theresults reveal that excellent and stable antibacterial activity of composite against E. coli due tofavorable dispersibility of Ag nanoparticles and introduction of high quality graphene.
The novel graphene and graphene-based composite materials are prepared by severalmethods. We futher study the mechanism of interaction between the various components ofthe composite. Meanwhile, we understand the relationship between structure and properties ofcomposite materials. We hope our work can improve the development of related theory.
采用淬火技术同步剥离与还原膨胀石墨制备高质量、高产率的石墨烯。XPS、Raman等测试结果表明通过水合肼或浓氨水辅助的淬火过程能够有效减少石墨烯表面的含氧基团，导电原子力分析表明石墨烯具有优异的导电性能。膨胀石墨层间存在大量插层化合物，通过淬火应力能够剥离膨胀石墨形成石墨烯片，高质量的石墨烯可以作为良好的载体材料构筑石墨烯基复合体。设计一种简单的浓氨水辅助水热合成法制备氮掺杂石墨烯。在还原氧化石墨的同时实现石墨烯的氮掺杂，氮掺杂石墨烯显示出较高的氮掺杂量（7.2%）以及较好的稳定性，同时氮掺杂石墨烯也显示出比石墨烯更优异的电容特性，比电容的最高值为144.6F/g。通过此种方法可以合成出具有广泛应用前景的高品质氮掺杂石墨烯，也为改善和提高超级电容器的电容特性以及稳定性提供了一种新的选择。
通过合适初级纳米粒子在膨胀石墨层间原位生长，利用初级纳米粒子生长力剥离膨胀石墨的同时与石墨烯复合构筑石墨烯基复合材料，石墨烯片的引入明显提高锐钛型TiO_2纳米晶的热稳定性，同时TiO_2自身的光生载流子分离效率提高，光催化性能研究表明复合材料不论在可见光还是紫外光下均比P25的催化活性要优异，在可见光下苯酚的降解率为62%，而在紫外光下苯酚的降解率为81%。为合成高性能的石墨烯基光催化剂提供了新颖的实验方法。采用HF和甲醇的溶剂热体系，一步合成新颖的石墨烯/暴露{001}高能面TiO_2复合体，利用复合体进一步深入探究TiO_2和C之间的电子转移行为，揭示二者之间的电子转移过程对进一步理解光催化机制具有指导意义。XPS结果表明TiO_2与石墨烯之间存在较强的相互作用以及电子转移行为。XANES进一步说明复合体中电子转移的途径与方向，这种电子转移行为能够对载流子分离效率的提高具有积极作用，利于光催化性能的提高。通过光催化性能评价发现石墨烯/暴露{001}高能面TiO_2复合体显示出比P25优异的紫外光催化活性。
通过简单的原位化学还原方法制备Ag/石墨烯复合结构，实验结果表明大约8～10μm的石墨片表面均匀生长着直径约为45nm的银纳米粒子。并在此基础上以大肠杆菌为受试菌株，用抑菌圈法测试Ag/石墨烯复合体的抑菌效果，实验结果表明Ag/石墨烯复合体对大肠杆菌具有优异的抑菌性能，可能归因于高质量石墨烯的引入使得Ag纳米颗粒的分散性提高，同时也提高了Ag纳米颗粒的光照稳定性，Ag纳米粒子与石墨烯片协同效应共同促进抑菌性能的明显提高。
通过几种新颖的方法制备了新型的石墨烯及石墨烯基复合材料，研究复合材料各组分之间的相互作用机理，探索复合材料结构与性能之间关系，丰富石墨烯及石墨烯基复合材料相关领域的基础理论，从而为实现相关材料的实际应用奠定坚实基础。
Graphene has attracted increasing attention because its unique nanostructure holds greatpromise for potential applications in different fields such as photocatalysis, sensors, batteriesand supercapacitors. Graphene sheets, one-atom-thick two-dimensional layers of sp2-bondedcarbon, are predicted to have a range of unusual properties. Their thermal conductivity andmechanical stiffness may rival the remarkable in-plane values for graphite; theirfracturestrength should be comparable to that of carbon nanotubes for similar types of defects;and recent studies have shown that individual graphene sheets have extraordinary electronictransport properties. One possible route to harnessing these propertiesfor applications wouldbe to incorporate graphene sheets in acomposite material. The manufacturing of suchcomposites requires not only that graphene sheets be produced on a sufficient scale but thatthey also be incorporated, and homogeneously distributed, into various matrices. The mainresearch contents of thesis are shown as follows:
Recently, single-or few-layer graphene sheets had been prepared by several methods.However, the low productivity of the micromechanical exfoliation makes it unsuitable forlarge-scale use. The functionalization of GO disrupts the electronic structure of graphene.Thus, facile and efficient strategy to produce high quality and large yield graphene is urgentlyrequired. Quenching technology is an important operation in the final fabrication process ofany engineering component. We can make full use of quenching stress to exfoliate graphitelayers for the production of graphene. In the first part, we presented a high-efficient hydrazinehydrate or concentrated ammonia-assisted quenching route to prepare the high qualitygraphenes. The success process was attributed to the strong quenching and presence ofhydrazine hydrate or concentrated ammonia. The strategy is promising due to its facileoperation, rapid production and low-cost starting materials.
Supercapacitors have attracted increasing attention as alternative energy-storage systems.Up to now, carbon nanomaterials such as porous carbon materials and carbon nanotubes havebeen used as supercapacitors electrodes due to their large surface areas and highconductivities. The capacitive behavior of carbon materials can be further improved by thepresence of active species that contribute to the total specific capacitance by the pseudocapacitive effect. In this work, we developed a concentrate ammonia-assistedhydrothermal method to obtain N-doped graphene sheets by simultaneous N-doping andreduction of graphene oxide (GO) sheets. The effects of hydrothermal temperature on surfacechemistry and structure of the N-doped graphene sheets were also investigated. N bindingconfigurations of sample consist of pyridine N, quaternary N, and pyridine-N oxides. Thesample exhibits excellent thermal stability. Electrical measurements demonstrate that productsshow higher capacitive performance than that of pure graphene that ascribe thepseudocapacitive effect from the N-doping. The samples also show excellent long-term cyclestability of capacitive performance.
We present a facile route to prepare TiO_2-graphene composites by in situ growth of TiO_2ininterlayer of low-cost expanded graphite (EG) under solvothermal. The vacuum-assistanttechnology associated with the use of surfactant (cetyltrimethylammonium bromides) plays akey role in the fabrication of such composites. Firstly, the vacuum environment promotes theinitial solution containing Ti(OBu)4, and the surfactant fully infusing into the interlayer of EG;subsequently, numerous nanoparticles of TiO_2in situ uniformly grow in interlayer with thehelp of surfactant, facilitates the EG exfoliation; in the mean time, EG by the aid of theethanol solvothermal, eventually forming the TiO_2-graphene composites. The as-preparedsamples have been characterized by Raman, SEM, TEM, AFM, FT-IR, and thermogravimeticanalysis. It is shown that a large number of TiO_2nanoparticles homogeneously cover thesurface of high-quality graphene sheets. The graphene exhibits multi-layered structure(five~seven layers). Noticeably, the synthesized TiO_2-graphene by post thermal treatment athigh temperature under nitrogen show high photocatalytic activity to degrade phenol undervisible and UV light in comparison with bare P25. The enhanced photocatalytic performanceis attributed to the increased charge separation, the strengthened light absorbance and lightabsorption width, and the fine adsorptivity for pollutants.
A simply and feasible strategy to synthesize the novel anatase TiO_2/graphene compositeswith exposed TiO_2{001} high-energy facets by the hydrofluoric acid-and methanol-jointassisted solvothermal reactions. During the synthesis process, graphene were uniformlycovered with a large number anatase TiO_2nanoparticles, exposing the {001} facets. TheX-ray photoelectron spectroscopy (XPS) and X-ray absorption (XAS) measurements show the presence of electron transfer between TiO_2and graphene. Furthermore, transient photovoltage(TPV) spectra of the composite also exhibits prolonged mean lifetime of electron-hole pairscompared with pure TiO_2. The electron transfer between Ti and C will greatly retard therecombination of photoinduced charge carriers and prolong electron lifetime, whichcontributing to the enhancement of photocatalytic performance. During the photocatalysismeasurement, the TiO_2/graphene composites have high photocatalytic activity compared withthe P25under UV light, likely due to the effective separation of photoinduced charge andexposure of high reactive {001} facets.
A novel Ag/graphene composite antibacterial agent was synthesized through a facilechemical reduction method. The high quality graphene was selected as the carbon substratefor supporting Ag particles. The composite had been characterized by high-resolutiontransmission electron microscopy and scanning electron microscopy. The results show thatabout45~50nm Ag nanoparticles are uniformly dispersed on the surface of the graphene. Theantibacterial activity of composite is investigated using the agar well diffusion method. Theresults reveal that excellent and stable antibacterial activity of composite against E. coli due tofavorable dispersibility of Ag nanoparticles and introduction of high quality graphene.
The novel graphene and graphene-based composite materials are prepared by severalmethods. We futher study the mechanism of interaction between the various components ofthe composite. Meanwhile, we understand the relationship between structure and properties ofcomposite materials. We hope our work can improve the development of related theory.
引文
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