氧化石墨的表面功能化及其应用
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摘要
石墨烯具有单原子厚度的二维蜂窝状结构，由于其具有优异的电传导性、热传导性和力学性能，可以广泛应用在传感器、纳米电子学、聚合物增强材料和超级电容器等领域。常用的制备方法有机械剥离、化学气相沉积、外延生长等方法。然而，这些方法都不能大量制备石墨烯。氧化石墨被认为是宏量制备石墨烯最优异的前驱体材料，可以通过将氧化石墨超声剥离后再经化学还原来制备石墨烯。本论文采用葡萄糖、乙二胺和对苯二胺作为还原剂将氧化石墨还原和表面功能化修饰。主要工作如下：
（1）以葡萄糖还原的石墨烯（G-graphene）和聚乙烯醇（PVA）为原料，通过水溶液共混的方法制备出机械性能增强的聚乙烯醇纳米复合材料。选择共价型表面活性剂聚乙烯吡咯烷酮（PVP）作为G-graphene的表面修饰剂来改善G-graphene与聚乙烯醇的相容性。当PVP修饰的石墨烯（G-P-graphene）的含量为0.7wt%时，聚乙烯醇纳米复合材料的拉伸强度由聚乙烯醇的105MPa增加到154MPa；杨氏模量由聚乙烯醇的3.3GPa增加到4.9GPa。力学性能的增加是因为G-P-graphene在聚乙烯醇基体中良好的分散，以及G-P-graphene与聚乙烯醇之间存在的强烈的氢键作用共同作用的结果。
（2）采用乙二胺作为还原剂，通过简单水回流的方法制备出乙二胺还原修饰的石墨烯（ED-RGO）。反应原理是乙二胺上的胺基与氧化石墨表面的环氧基发生了亲核取代反应。ED-RGO作为Cr(VI)离子吸附剂，与其他传统吸附剂相比，具有更优异的移除效率，而且吸附后的吸附剂很容易分离。在低pH的条件下，高毒性的Cr(VI)可以被ED-RGO还原为低毒性的Cr(III)，还原过程采用一种间接的还原机制。还原过程中所需要的电子来自ED-RGO六元环上的π电子。ED-RGO作为一种新型吸附剂，在含Cr(VI)废水治理领域具有很好的应用前景。
（3）用对苯二胺作为还原修饰剂，通过简单水回流的方法得到对苯二胺还原修饰的石墨烯（GO-PPD）。反应原理同样是对苯二胺上的胺基与氧化石墨表面的环氧基发生了亲核取代反应。还原后得到的GO-PPD膜的电导率高达2.1×10~2S m~(-1)，是氧化石墨膜的近9倍。此外，将GO-PPD与聚苯乙烯复合制备得到的纳米复合材料的导电逾渗阈值低达～0.34vol%，复合材料的热稳定性也提高了～8°C，这是由于GO-PPD可以在聚苯乙烯基体中具有良好的分散。
（4）采用溶液共混的方法，将GO-PPD和热膨胀的石墨烯分别和聚碳酸酯（PC）基体复合，得到聚碳酸酯基导电复合材料。采用间歇式超临界CO_2发泡技术制备聚碳酸酯/石墨烯导电复合泡沫材料；同时研究了发泡条件（发泡时间、饱和压力和饱和温度）对泡孔尺寸和泡孔密度的影响，选择出最佳的发泡条件。在此条件下制备出的纯聚碳酸酯发泡样品的泡孔尺寸为28.2μm，泡孔密度为7.85×107cells cm~(-3)。扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线衍射（XRD）、热失重分析（TGA）和流变表征分析的结果表明GO-PPD在聚碳酸酯基体中具有良好的分散。复合材料的发泡结果证明填料在基体中良好的分散有利于在发泡过程中泡孔尺寸的降低和泡孔密度的增加。制备的PC/GO-PPD复合材料的泡孔直径为0.76μm，泡孔密度为5.69×1011cells cm~(-3)。此外，PC/GO-PPD的发泡材料和块状材料比起来，在较低的填料含量时就发生了由绝缘体向导体的转变，这是因为微米级的泡孔尺寸没有够破坏材料的导电网络。
Graphene, which consists of atom-thick sheets of carbon packed in atwo-dimensional honeycomb lattice, has been used in sensors,nanoelectronics, composite reinforcement and capacitors because of itshigh electrical conductivity, high thermal conductivity and superiormechanical properties. Several methods, such as the mechanicalexfoliation, chemical vapor deposition, epitaxial growth on electricallyinsulating surface have been employed in preparing graphene nanosheets.However, scaling up is a major hurdle with these methods. It has beenwell demonstrated that graphene oxide (GO) is an excellent precursor toprepare graphene by ultrasonic exfoliation and chemical reduction. In thiswork, GO was reduced and functionalized with glucose, ethylenediamineand p-phenylene diamine, respectively. And the main work of this thesisincludes:
(1) Poly(vinyl alcohol)(PVA) nanocomposite films with enhancedmechanical properties were prepared by solution blending ofglucose-reduced graphene oxide (G-graphene) with aqueous solution of PVA. Poly(N-vinyl-2-pyrrolidone)(PVP) was selected as the surfactant toimprove the stability of the aqueous suspension of G-graphene. With0.7wt%of PVP-stabilized G-graphene (G-P-graphene), the tensile strengthof PVA increases from105MPa to154MPa and the Young’s modulusincreases from3.3GPa to4.9GPa. These substantial improvements wereattributed to the good dispersion of G-P-graphene nanosheets in PVAmatrix and the strong hydrogen-bonding interaction betweenG-P-graphene nanosheets and PVA macromolecular chains.
(2) Ethylenediamine-reduced graphene oxide (ED-RGO) sheets wereprepared by simple refluxing of GO solution with ethylenediamine (ED).This was possible by the nucleophilic substitution reaction of epoxidegroups of GO with amine groups of ED. Compared with otherconventional adsorbents, ED-RGO exhibits relatively a high removal rateand can be easily separated from the solution after adsorption. Moreimportantly, Cr(VI) can be effectively reduced to low toxic Cr(III) speciesat low pH, which follows an indirect reduction mechanism with the aid ofπ electrons on the carbocyclic six-membered ring of ED-RGO. It isexpected that ED-RGO can be applied as a novel adsorbent for Cr(VI)removal from wastewater.
(3) A facile and efficient approach was developed to simultaneouslyfunctionalize and reduce GO with p-phenylene diamine (PPD) by simplerefluxing. This was also possible by the nucleophilic substitution reaction of epoxide groups of GO with amine groups of PPD. As a consequence,electrical conductivity of GO-PPD increased to2.1×10~2S/m, which wasnearly9orders of magnitude higher than that of GO. Additionally, afterthe incorporation of GO-PPD in polystyrene (PS), the compositesexhibited a sharp transition from electrically insulating to conductingbehavior with a low percolation threshold of～0.34vol%, which wasattributed to the improved dispersion and the reduction of GO-PPD.Thermal stability of the PS/GO-PPD composite was also～8°C higherthan that of PS.
(4) Electrically conductive polycarbonate (PC) nanocomposites wereprepared by solution blending of PC matrix with thermal expansiongraphene or GO-PPD, respectively. PC microcellular electricallyconductive foams were obtained by two-step foaming with subcriticalCO2as an environmentally benign foaming agent. The influences offoaming time, saturated pressure and saturated temperature on the cellsize and cell density were investigated. The foaming conditions were alsooptimized. The average cell diameter and cell density of pure PC matrixwere28.2μm and7.85×10~7cells cm~3, respectively. Compared to thermalexpansion graphene, GO-PPD exhibited an improved dispersion in PCmatrix, which was confirmed by SEM, TEM, XRD, TGA and rheologicalmeasurement. The good dispersion of GO-PPD in PC matrix could inhibitthe cell expansion and had high nucleation efficiency during foaming. The average cell diameter and cell density of PC/GO-PPD were0.76μmand5.69×1011cells cm~3, respectively.Compared to that of the bulknanocomposites, the insulator to semiconductor transition of the foamsshifted to lower GO-PPD content because the conductive network wasnot destroyed by the micron-sized cells.
（1）以葡萄糖还原的石墨烯（G-graphene）和聚乙烯醇（PVA）为原料，通过水溶液共混的方法制备出机械性能增强的聚乙烯醇纳米复合材料。选择共价型表面活性剂聚乙烯吡咯烷酮（PVP）作为G-graphene的表面修饰剂来改善G-graphene与聚乙烯醇的相容性。当PVP修饰的石墨烯（G-P-graphene）的含量为0.7wt%时，聚乙烯醇纳米复合材料的拉伸强度由聚乙烯醇的105MPa增加到154MPa；杨氏模量由聚乙烯醇的3.3GPa增加到4.9GPa。力学性能的增加是因为G-P-graphene在聚乙烯醇基体中良好的分散，以及G-P-graphene与聚乙烯醇之间存在的强烈的氢键作用共同作用的结果。
（2）采用乙二胺作为还原剂，通过简单水回流的方法制备出乙二胺还原修饰的石墨烯（ED-RGO）。反应原理是乙二胺上的胺基与氧化石墨表面的环氧基发生了亲核取代反应。ED-RGO作为Cr(VI)离子吸附剂，与其他传统吸附剂相比，具有更优异的移除效率，而且吸附后的吸附剂很容易分离。在低pH的条件下，高毒性的Cr(VI)可以被ED-RGO还原为低毒性的Cr(III)，还原过程采用一种间接的还原机制。还原过程中所需要的电子来自ED-RGO六元环上的π电子。ED-RGO作为一种新型吸附剂，在含Cr(VI)废水治理领域具有很好的应用前景。
（3）用对苯二胺作为还原修饰剂，通过简单水回流的方法得到对苯二胺还原修饰的石墨烯（GO-PPD）。反应原理同样是对苯二胺上的胺基与氧化石墨表面的环氧基发生了亲核取代反应。还原后得到的GO-PPD膜的电导率高达2.1×10~2S m~(-1)，是氧化石墨膜的近9倍。此外，将GO-PPD与聚苯乙烯复合制备得到的纳米复合材料的导电逾渗阈值低达～0.34vol%，复合材料的热稳定性也提高了～8°C，这是由于GO-PPD可以在聚苯乙烯基体中具有良好的分散。
（4）采用溶液共混的方法，将GO-PPD和热膨胀的石墨烯分别和聚碳酸酯（PC）基体复合，得到聚碳酸酯基导电复合材料。采用间歇式超临界CO_2发泡技术制备聚碳酸酯/石墨烯导电复合泡沫材料；同时研究了发泡条件（发泡时间、饱和压力和饱和温度）对泡孔尺寸和泡孔密度的影响，选择出最佳的发泡条件。在此条件下制备出的纯聚碳酸酯发泡样品的泡孔尺寸为28.2μm，泡孔密度为7.85×107cells cm~(-3)。扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线衍射（XRD）、热失重分析（TGA）和流变表征分析的结果表明GO-PPD在聚碳酸酯基体中具有良好的分散。复合材料的发泡结果证明填料在基体中良好的分散有利于在发泡过程中泡孔尺寸的降低和泡孔密度的增加。制备的PC/GO-PPD复合材料的泡孔直径为0.76μm，泡孔密度为5.69×1011cells cm~(-3)。此外，PC/GO-PPD的发泡材料和块状材料比起来，在较低的填料含量时就发生了由绝缘体向导体的转变，这是因为微米级的泡孔尺寸没有够破坏材料的导电网络。
Graphene, which consists of atom-thick sheets of carbon packed in atwo-dimensional honeycomb lattice, has been used in sensors,nanoelectronics, composite reinforcement and capacitors because of itshigh electrical conductivity, high thermal conductivity and superiormechanical properties. Several methods, such as the mechanicalexfoliation, chemical vapor deposition, epitaxial growth on electricallyinsulating surface have been employed in preparing graphene nanosheets.However, scaling up is a major hurdle with these methods. It has beenwell demonstrated that graphene oxide (GO) is an excellent precursor toprepare graphene by ultrasonic exfoliation and chemical reduction. In thiswork, GO was reduced and functionalized with glucose, ethylenediamineand p-phenylene diamine, respectively. And the main work of this thesisincludes:
(1) Poly(vinyl alcohol)(PVA) nanocomposite films with enhancedmechanical properties were prepared by solution blending ofglucose-reduced graphene oxide (G-graphene) with aqueous solution of PVA. Poly(N-vinyl-2-pyrrolidone)(PVP) was selected as the surfactant toimprove the stability of the aqueous suspension of G-graphene. With0.7wt%of PVP-stabilized G-graphene (G-P-graphene), the tensile strengthof PVA increases from105MPa to154MPa and the Young’s modulusincreases from3.3GPa to4.9GPa. These substantial improvements wereattributed to the good dispersion of G-P-graphene nanosheets in PVAmatrix and the strong hydrogen-bonding interaction betweenG-P-graphene nanosheets and PVA macromolecular chains.
(2) Ethylenediamine-reduced graphene oxide (ED-RGO) sheets wereprepared by simple refluxing of GO solution with ethylenediamine (ED).This was possible by the nucleophilic substitution reaction of epoxidegroups of GO with amine groups of ED. Compared with otherconventional adsorbents, ED-RGO exhibits relatively a high removal rateand can be easily separated from the solution after adsorption. Moreimportantly, Cr(VI) can be effectively reduced to low toxic Cr(III) speciesat low pH, which follows an indirect reduction mechanism with the aid ofπ electrons on the carbocyclic six-membered ring of ED-RGO. It isexpected that ED-RGO can be applied as a novel adsorbent for Cr(VI)removal from wastewater.
(3) A facile and efficient approach was developed to simultaneouslyfunctionalize and reduce GO with p-phenylene diamine (PPD) by simplerefluxing. This was also possible by the nucleophilic substitution reaction of epoxide groups of GO with amine groups of PPD. As a consequence,electrical conductivity of GO-PPD increased to2.1×10~2S/m, which wasnearly9orders of magnitude higher than that of GO. Additionally, afterthe incorporation of GO-PPD in polystyrene (PS), the compositesexhibited a sharp transition from electrically insulating to conductingbehavior with a low percolation threshold of～0.34vol%, which wasattributed to the improved dispersion and the reduction of GO-PPD.Thermal stability of the PS/GO-PPD composite was also～8°C higherthan that of PS.
(4) Electrically conductive polycarbonate (PC) nanocomposites wereprepared by solution blending of PC matrix with thermal expansiongraphene or GO-PPD, respectively. PC microcellular electricallyconductive foams were obtained by two-step foaming with subcriticalCO2as an environmentally benign foaming agent. The influences offoaming time, saturated pressure and saturated temperature on the cellsize and cell density were investigated. The foaming conditions were alsooptimized. The average cell diameter and cell density of pure PC matrixwere28.2μm and7.85×10~7cells cm~3, respectively. Compared to thermalexpansion graphene, GO-PPD exhibited an improved dispersion in PCmatrix, which was confirmed by SEM, TEM, XRD, TGA and rheologicalmeasurement. The good dispersion of GO-PPD in PC matrix could inhibitthe cell expansion and had high nucleation efficiency during foaming. The average cell diameter and cell density of PC/GO-PPD were0.76μmand5.69×1011cells cm~3, respectively.Compared to that of the bulknanocomposites, the insulator to semiconductor transition of the foamsshifted to lower GO-PPD content because the conductive network wasnot destroyed by the micron-sized cells.
引文
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