石墨烯及其典型聚合物纳米复合材料的制备方法、结构与机理研究
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摘要
石墨烯是由碳原子构成的单原子厚度的二维层状材料,具有奇异的特点和优异的性能,是当前国际研究热点,受到物理、化学、材料、电子、能源、生物和信息技术等领域的广泛关注。石墨烯可以显著地提高聚合物的性能,石墨烯/聚合物纳米复合材料(GPNC)是石墨烯最具希望的应用之一。但是,GPNC的基础研究和实际应用仍然面临着许多科学和技术问题,其中主要包括三个方面：(1)石墨烯的高效制备方法；(2)分散性良好的GPNC规模化制备方法；(3)对于GPNC性能与微结构的内在本质关系的研究。
本论文设计了密闭氧化法、氨-水合肼复合还原法和母粒-熔融复合法,分别用于制备氧化石墨(GO)、石墨烯和GPNC,具备简便、高效和高质量等优点;母粒-熔融复合法兼顾了GPNC的良好分散性与规模化制备的可行性,初步解决了GPNC的工业化生产和实际应用所面临的关键技术问题。重点研究了GPNC的微观结构、力学性能、热稳定性和火安全性能以及相关机理。为了研究石墨烯的片层阻隔效应、石墨烯片层的导热性以及石墨烯与聚合物基体之间的界面相互作用对GPNC结构与性能的影响,选取了聚乳酸(PLA)、聚乙烯醇(PVA)和聚苯乙烯(PS)三种与石墨烯具有不同的界面相互作用的聚合物作为基体.基于GO、石墨烯以及不同的聚合物基体进行对比研究,初步揭示了GPNC微观结构与性能之间的本质关系,阐明了石墨烯影响GPNC热稳定性和火安全性的机理。本论文为GPNC的基础研究和实际应用奠定了一定的理论和实验基础,并初步开拓了切实可行的工业化生产技术路线。
设计了密闭氧化法和氨-水合肼复合还原法,从而实现氧化石墨和石墨烯的高效制备。密闭氧化法是将石墨在反应釜中与强酸和强氧化剂进行氧化反应的方法,包括加料、低温处理(温度为5℃以下,时间为1小时以上)和高温反应(温度为60-160℃,时间为1小时以上)三个步骤。相比于传统的Hummers法,密闭氧化法简化了制备过程,降低了制备操作和温度控制的要求,实现GO的尺寸和形貌的可控性。氨-水合肼复合还原法是用氨水和水合肼对GO进行联合还原的方法。相比于传统的水合肼还原法,氨-水合肼复合还原法制备的石墨烯还原程度高,产物中含氧官能团——尤其是羟基——数量少,厚度仅为0.4-0.6nm,是目前最接近理论值(0.34nm)的报道之一。
设计了母粒-熔融复合法,应用于石墨烯/PLA纳米复合材料,实现了通过工业加工设备制备具有良好分散性的GPNC。石墨烯在PLA中形成良好的分散和层离状态,显著地提高了材料的结晶性能、导电性、力学性能和火安全性能。从材料的结构和性能的相互验证中,推断出影响石墨烯/PLA纳米复合材料性能的机理,研究表明：(1)石墨烯在PLA中形成连通的导电、导热网络,并存在一定的阂值；(2)石墨烯具有增强GPNC力学性能的作用,同时因为阻隔PLA分子间的相互作用而具有降低GPNC力学性能的作用,两者的相互竞争导致纳米复合材料的力学性能在石墨烯含量为0.08%-0.2%时出现反复和拐点；(3)石墨烯的高导热性是降低石墨烯/PLA纳米复合材料热解温度和点燃时间的主要原因；(4)石墨烯片层的片层阻隔效应是降低石墨烯/PLA纳米复合材料的热解失重速率与热释放速率的主要原因。
文献报道认为石墨烯(或GO)与PVA之间的氢键作用是导致纳米复合材料性能增强的根本原因,但是这一论断与相关文献的统计规律相抵触。因此,对GO/PVA和石墨烯/PVA纳米复合材料的分散性、结晶、电学性能、力学性能和热稳定性等进行了对比研究。GO和石墨烯均显著地提高了PVA的性能。研究表明：(1)石墨烯的分散性差于GO,但是有更好的性能增强效果,这与相关文献一致；(2)氢键的作用主要是促使石墨烯或GO形成良好的分散；(3)石墨烯片层自身结构的完整性,即石墨烯晶格结构的完整性,是提高石墨烯/PVA纳米复合材料性能的根本原因；(4)石墨烯片层的片层阻隔效应是提高纳米复合材料热稳定性的主要原因,石墨烯的高导热性是降低纳米复合材料热解温度的主要原因,两者的相互竞争使石墨烯/PVA纳米复合材料的热解温度随着石墨烯添加量的增加而先降低后升高。
为了验证母粒-熔融复合法通过工业生产设备制备GPNC的可行性,以及研究过渡金属和石墨烯在提高聚合物材料的火安全性能方面的协效作用,基于GO、石墨烯、负载二氧化锆(Zr-Gr)和负载氢氧化镍(Ni-Gr)的石墨烯,通过密炼机和双螺杆挤出机制备了以PS为基体的纳米复合材料。母粒中的PS防止石墨烯片层在干燥和加工过程中发生团聚；熔融复合过程中,螺杆对PS熔体和石墨烯的剪切作用促使石墨烯片层充分层离；两者的综合作用使石墨烯在PS中形成良好的分散性和层离状态。GO/PS纳米复合材料的热失重速率峰值对应温度最大增幅为10.8℃,石墨烯/PS的最大增幅为14.0℃,Zr-Gr/PS的最大增幅为10.5℃,Ni-Gr/PS的最大增幅为17.5℃。以上四种纳米复合材料的热释放速率峰值最大降幅分别为23%、34%、42%和41%,CO生成量显著降低,表明金属化合物与石墨烯形成了协同作用。研究表明：(1)实现了在现有的工业生产设备的基础上通过母粒-熔融复合法制备具有良好的分散性的GPNC,为GPNC的工业化生产和实际应用奠定了一定的实验和技术基础；(2)通过GO与石墨烯之间以及PLA、PVA和PS三个体系之间的相互对比,证明了石墨烯片层的片层阻隔效应和界面相互作用是提高聚合物材料热稳定性和火安全性能的主要原因；(3)过渡金属化合物和石墨烯在聚合物材料火安全性能上存在协效作用。
采用六氯环三磷腈和环氧丙醇对GO进行表面修饰,制备出含环氧基团的改性氧化石墨(FGO),并通过原位聚合法制备了FGO/环氧树脂纳米复合材料。FGO与环氧树脂之间的化学键形成了强的界面相互作用,促使FGO形成良好的分散,显著地提高纳米复合材料的性能,如储能模量的最大增幅为131%,硬度的最大增幅为32%,热失重速率峰值的最大降幅为27%。
Graphene, a monolayer of sp2carbon atoms with many unique properties, has gained much attention from various areas, such as the physics, chemistry, material, electron, energy, biology and information technique fields. One of the most promising applications of graphene is the graphene/polymer nanocomposite (GPNC), in which graphene causes significant improvements in various properties. There are still challenges in the academic research and practical application of GPNC:1) preparation of graphene with high efficiency;2) preparation of GPNC with good dispersion and in large quantities;3) investigation of the relationship between the structure and properties as well as the mechanism for the enhanced properties. In order to overcome those challenges, this paper mainly focused on three aspects:1) high efficient preparation of graphite oxide (GO) and graphene;2) a masterbatch-melt blending method to prepare GPNC;3) investigations of the structure, properties and mechanism of the improved properties in GPNC. In order to clarify the roles of the physical barrier effect of graphene, the high thermal conductivity of graphene and the interface interaction between graphene and polymer matrix on the thermal stability and fire safety properties of GPNC, poly(lactic acid)(PLA), poly(vinyl alcohol)(PVA) and polystyrene (PS) was choosen as the polymeric matrix of GPNC. By the compoarisons between GO, graphene and the three kinds of polymers, the mechanism of the improved thermal stabilitiy and fire safety propeties was studied.
A pressurized oxidation and an ammonia-hydrazine-based multiplex reduction were developed to prepare GO and graphene, respectively. The pressurized oxidation was carried out in reactor with three steps:adding react agents, low temperature treatment (<5℃,>1hr) and high temperature reaction (60-160℃,>1hr). GO was prepared by the pressurized oxidation with fairly easy operation and controllable morphology and size. The ammonia-hydrazine-based multiplex reduction prepared graphene which can be easily observed by atomic force microscopy with a thickness (0.4-0.6nm) which is fairly closed to the ideal value.
A masterbatch-melt blending was employed to prepare graphene/PLA nanocomposites. The graphene was well dispersed and exfoliated in the PLA, and the crystallinity, electrical conductivity, mechanical properties and fire safety performance of the nanocomposites were obviously improved. The mechanism of the improved properties were investigated:1) the graphene started to form a conducting network at the loading content of0.08%;2) the graphene reinforced the mechanism properties of the nanocomposites, but it also cut down the interaction among the PLA molecules and hence reduced the mechanical properties, competition of the reinforcing and the reducing caused inflexions at0.08%-0.2%;3) the high thermal conductivity of graphene was the main reason for the decreased thermal degradation temperature and ignition time, and the mass barrier effect of graphene is the cause of the reduced degradation rate and heat release rate.
In the earlier literature, the hydrogen bonding between graphene (or GO) and PVA was regarded as the causes of property enhancements. GO/PVA and graphene/PVA nanocomposites were studied in order to investigate the mechanism of the improved properties. GO and graphene caused obvious property enhancements such as storage modulus and electrical conductivity. There are mainly four conclusions:1) graphene presented a poorer dispersion than GO but caused more property enhancements;2) the hydrogen bonding mainly contributed to the dispersion of the graphene (or GO) layers;3) the main cause of the improved properties was the completeness of graphene (or GO) structure;4) the mass barrier effect was the main reason for the improved thermal stability; when the loading amount was small, the thermal degradation temperature was decreased due to the high thermal conductivity of graphene; when the loading amount was large, the mass barrier effect dominated so the thermal degradation temperature was increased.
PS-based nanocomposites were prepared based on GO, graphene, ZrO2-loaded graphene and Ni(OH)2-loaded graphene (joint title:Gs). The Gs were well dispersed and exfoliated due to two reasons:1) the PS in the masterbatch prevented the Gs from aggregation during drying and processing;2) the shearing effect during the melt blending further improved dispersion and exfoliation. The thermal degradation was increased with2%Gs (10.8℃with GO,14.0℃with graphene,10.5℃with ZrO2-loaded graphene and17.5℃with Ni(OH)2-loaded graphene). The peak heat release rate of the above four kinds of nanocomposites was reduced by23%,34%,42%and41%, respectively. There were three conclusions:1) the master-melt blending was feasible for the industrial processing of GPNC, which pioneers a viable path to the practical producing and application of GPNC;2) the mass barrier and interface interaction were found to be the main reasons for the improved thermal stability;3) there was synergism effect between the loaded metal and graphene on the fire safety properties of the PS-based nanocomposites.
The masterbatch-melt blending was feasible with thermoplastic polymers but was not available in thermosetting polymers such as epoxy resin. In order to obtain good dispersion and strong interface interaction, GO was modified with hexachlorocyclotriphosphazene and glycidol and then incorporated into epoxy by the in-situ curing. The storage modulus (131%), hardness (32%) and electrical conductivity (6.5magnitude orders) were obviously increased and the maximum degradation rate was decreased by27%.
As compared to the tradition preparation methods, the pressurized oxidation, ammonia-hydrazine multiplex reduction and the masterbatch-melt blending were more convenient and efficient. The masterbatch-melt blending offered a feasible way toward the industrial processing of GPNC with good dispersion. The investigations of the properties and mechanism promoted the research of GPNC.
本论文设计了密闭氧化法、氨-水合肼复合还原法和母粒-熔融复合法,分别用于制备氧化石墨(GO)、石墨烯和GPNC,具备简便、高效和高质量等优点;母粒-熔融复合法兼顾了GPNC的良好分散性与规模化制备的可行性,初步解决了GPNC的工业化生产和实际应用所面临的关键技术问题。重点研究了GPNC的微观结构、力学性能、热稳定性和火安全性能以及相关机理。为了研究石墨烯的片层阻隔效应、石墨烯片层的导热性以及石墨烯与聚合物基体之间的界面相互作用对GPNC结构与性能的影响,选取了聚乳酸(PLA)、聚乙烯醇(PVA)和聚苯乙烯(PS)三种与石墨烯具有不同的界面相互作用的聚合物作为基体.基于GO、石墨烯以及不同的聚合物基体进行对比研究,初步揭示了GPNC微观结构与性能之间的本质关系,阐明了石墨烯影响GPNC热稳定性和火安全性的机理。本论文为GPNC的基础研究和实际应用奠定了一定的理论和实验基础,并初步开拓了切实可行的工业化生产技术路线。
设计了密闭氧化法和氨-水合肼复合还原法,从而实现氧化石墨和石墨烯的高效制备。密闭氧化法是将石墨在反应釜中与强酸和强氧化剂进行氧化反应的方法,包括加料、低温处理(温度为5℃以下,时间为1小时以上)和高温反应(温度为60-160℃,时间为1小时以上)三个步骤。相比于传统的Hummers法,密闭氧化法简化了制备过程,降低了制备操作和温度控制的要求,实现GO的尺寸和形貌的可控性。氨-水合肼复合还原法是用氨水和水合肼对GO进行联合还原的方法。相比于传统的水合肼还原法,氨-水合肼复合还原法制备的石墨烯还原程度高,产物中含氧官能团——尤其是羟基——数量少,厚度仅为0.4-0.6nm,是目前最接近理论值(0.34nm)的报道之一。
设计了母粒-熔融复合法,应用于石墨烯/PLA纳米复合材料,实现了通过工业加工设备制备具有良好分散性的GPNC。石墨烯在PLA中形成良好的分散和层离状态,显著地提高了材料的结晶性能、导电性、力学性能和火安全性能。从材料的结构和性能的相互验证中,推断出影响石墨烯/PLA纳米复合材料性能的机理,研究表明：(1)石墨烯在PLA中形成连通的导电、导热网络,并存在一定的阂值；(2)石墨烯具有增强GPNC力学性能的作用,同时因为阻隔PLA分子间的相互作用而具有降低GPNC力学性能的作用,两者的相互竞争导致纳米复合材料的力学性能在石墨烯含量为0.08%-0.2%时出现反复和拐点；(3)石墨烯的高导热性是降低石墨烯/PLA纳米复合材料热解温度和点燃时间的主要原因；(4)石墨烯片层的片层阻隔效应是降低石墨烯/PLA纳米复合材料的热解失重速率与热释放速率的主要原因。
文献报道认为石墨烯(或GO)与PVA之间的氢键作用是导致纳米复合材料性能增强的根本原因,但是这一论断与相关文献的统计规律相抵触。因此,对GO/PVA和石墨烯/PVA纳米复合材料的分散性、结晶、电学性能、力学性能和热稳定性等进行了对比研究。GO和石墨烯均显著地提高了PVA的性能。研究表明：(1)石墨烯的分散性差于GO,但是有更好的性能增强效果,这与相关文献一致；(2)氢键的作用主要是促使石墨烯或GO形成良好的分散；(3)石墨烯片层自身结构的完整性,即石墨烯晶格结构的完整性,是提高石墨烯/PVA纳米复合材料性能的根本原因；(4)石墨烯片层的片层阻隔效应是提高纳米复合材料热稳定性的主要原因,石墨烯的高导热性是降低纳米复合材料热解温度的主要原因,两者的相互竞争使石墨烯/PVA纳米复合材料的热解温度随着石墨烯添加量的增加而先降低后升高。
为了验证母粒-熔融复合法通过工业生产设备制备GPNC的可行性,以及研究过渡金属和石墨烯在提高聚合物材料的火安全性能方面的协效作用,基于GO、石墨烯、负载二氧化锆(Zr-Gr)和负载氢氧化镍(Ni-Gr)的石墨烯,通过密炼机和双螺杆挤出机制备了以PS为基体的纳米复合材料。母粒中的PS防止石墨烯片层在干燥和加工过程中发生团聚；熔融复合过程中,螺杆对PS熔体和石墨烯的剪切作用促使石墨烯片层充分层离；两者的综合作用使石墨烯在PS中形成良好的分散性和层离状态。GO/PS纳米复合材料的热失重速率峰值对应温度最大增幅为10.8℃,石墨烯/PS的最大增幅为14.0℃,Zr-Gr/PS的最大增幅为10.5℃,Ni-Gr/PS的最大增幅为17.5℃。以上四种纳米复合材料的热释放速率峰值最大降幅分别为23%、34%、42%和41%,CO生成量显著降低,表明金属化合物与石墨烯形成了协同作用。研究表明：(1)实现了在现有的工业生产设备的基础上通过母粒-熔融复合法制备具有良好的分散性的GPNC,为GPNC的工业化生产和实际应用奠定了一定的实验和技术基础；(2)通过GO与石墨烯之间以及PLA、PVA和PS三个体系之间的相互对比,证明了石墨烯片层的片层阻隔效应和界面相互作用是提高聚合物材料热稳定性和火安全性能的主要原因；(3)过渡金属化合物和石墨烯在聚合物材料火安全性能上存在协效作用。
采用六氯环三磷腈和环氧丙醇对GO进行表面修饰,制备出含环氧基团的改性氧化石墨(FGO),并通过原位聚合法制备了FGO/环氧树脂纳米复合材料。FGO与环氧树脂之间的化学键形成了强的界面相互作用,促使FGO形成良好的分散,显著地提高纳米复合材料的性能,如储能模量的最大增幅为131%,硬度的最大增幅为32%,热失重速率峰值的最大降幅为27%。
Graphene, a monolayer of sp2carbon atoms with many unique properties, has gained much attention from various areas, such as the physics, chemistry, material, electron, energy, biology and information technique fields. One of the most promising applications of graphene is the graphene/polymer nanocomposite (GPNC), in which graphene causes significant improvements in various properties. There are still challenges in the academic research and practical application of GPNC:1) preparation of graphene with high efficiency;2) preparation of GPNC with good dispersion and in large quantities;3) investigation of the relationship between the structure and properties as well as the mechanism for the enhanced properties. In order to overcome those challenges, this paper mainly focused on three aspects:1) high efficient preparation of graphite oxide (GO) and graphene;2) a masterbatch-melt blending method to prepare GPNC;3) investigations of the structure, properties and mechanism of the improved properties in GPNC. In order to clarify the roles of the physical barrier effect of graphene, the high thermal conductivity of graphene and the interface interaction between graphene and polymer matrix on the thermal stability and fire safety properties of GPNC, poly(lactic acid)(PLA), poly(vinyl alcohol)(PVA) and polystyrene (PS) was choosen as the polymeric matrix of GPNC. By the compoarisons between GO, graphene and the three kinds of polymers, the mechanism of the improved thermal stabilitiy and fire safety propeties was studied.
A pressurized oxidation and an ammonia-hydrazine-based multiplex reduction were developed to prepare GO and graphene, respectively. The pressurized oxidation was carried out in reactor with three steps:adding react agents, low temperature treatment (<5℃,>1hr) and high temperature reaction (60-160℃,>1hr). GO was prepared by the pressurized oxidation with fairly easy operation and controllable morphology and size. The ammonia-hydrazine-based multiplex reduction prepared graphene which can be easily observed by atomic force microscopy with a thickness (0.4-0.6nm) which is fairly closed to the ideal value.
A masterbatch-melt blending was employed to prepare graphene/PLA nanocomposites. The graphene was well dispersed and exfoliated in the PLA, and the crystallinity, electrical conductivity, mechanical properties and fire safety performance of the nanocomposites were obviously improved. The mechanism of the improved properties were investigated:1) the graphene started to form a conducting network at the loading content of0.08%;2) the graphene reinforced the mechanism properties of the nanocomposites, but it also cut down the interaction among the PLA molecules and hence reduced the mechanical properties, competition of the reinforcing and the reducing caused inflexions at0.08%-0.2%;3) the high thermal conductivity of graphene was the main reason for the decreased thermal degradation temperature and ignition time, and the mass barrier effect of graphene is the cause of the reduced degradation rate and heat release rate.
In the earlier literature, the hydrogen bonding between graphene (or GO) and PVA was regarded as the causes of property enhancements. GO/PVA and graphene/PVA nanocomposites were studied in order to investigate the mechanism of the improved properties. GO and graphene caused obvious property enhancements such as storage modulus and electrical conductivity. There are mainly four conclusions:1) graphene presented a poorer dispersion than GO but caused more property enhancements;2) the hydrogen bonding mainly contributed to the dispersion of the graphene (or GO) layers;3) the main cause of the improved properties was the completeness of graphene (or GO) structure;4) the mass barrier effect was the main reason for the improved thermal stability; when the loading amount was small, the thermal degradation temperature was decreased due to the high thermal conductivity of graphene; when the loading amount was large, the mass barrier effect dominated so the thermal degradation temperature was increased.
PS-based nanocomposites were prepared based on GO, graphene, ZrO2-loaded graphene and Ni(OH)2-loaded graphene (joint title:Gs). The Gs were well dispersed and exfoliated due to two reasons:1) the PS in the masterbatch prevented the Gs from aggregation during drying and processing;2) the shearing effect during the melt blending further improved dispersion and exfoliation. The thermal degradation was increased with2%Gs (10.8℃with GO,14.0℃with graphene,10.5℃with ZrO2-loaded graphene and17.5℃with Ni(OH)2-loaded graphene). The peak heat release rate of the above four kinds of nanocomposites was reduced by23%,34%,42%and41%, respectively. There were three conclusions:1) the master-melt blending was feasible for the industrial processing of GPNC, which pioneers a viable path to the practical producing and application of GPNC;2) the mass barrier and interface interaction were found to be the main reasons for the improved thermal stability;3) there was synergism effect between the loaded metal and graphene on the fire safety properties of the PS-based nanocomposites.
The masterbatch-melt blending was feasible with thermoplastic polymers but was not available in thermosetting polymers such as epoxy resin. In order to obtain good dispersion and strong interface interaction, GO was modified with hexachlorocyclotriphosphazene and glycidol and then incorporated into epoxy by the in-situ curing. The storage modulus (131%), hardness (32%) and electrical conductivity (6.5magnitude orders) were obviously increased and the maximum degradation rate was decreased by27%.
As compared to the tradition preparation methods, the pressurized oxidation, ammonia-hydrazine multiplex reduction and the masterbatch-melt blending were more convenient and efficient. The masterbatch-melt blending offered a feasible way toward the industrial processing of GPNC with good dispersion. The investigations of the properties and mechanism promoted the research of GPNC.
引文
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