典型碳纳米材料的高压结构相变研究
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摘要
以单壁碳纳米管和石墨烯为代表的碳纳米材料因其独特的结构，优异的力学、热学、光学、电学性能以及在纳米电子学、纳米器件学、功能化材料等方面所具有的广阔应用前景和丰富的应用价值而成为材料科学领域的研究热点。高压可以有效地改变物质中分子或原子之间的距离，从而改变物质内部的电子分布，能带结构等等，进而在宏观上影响或改变物质的各种物理化学特性，它是产生新物质新材料、发现新规律新理论的重要手段。利用高压实验技术对碳纳米材料开展高压研究，一方面有助于我们了解其高压行为并深入理解碳材料的各种性质；另一方面，由于碳原子成键形式的灵活性和多样性，使得碳纳米材料的高压研究成为合成优异性能的新碳结构特别是新型超硬材料的重要方法和途径。这些都赋予了碳纳米材料高压研究以丰富的内涵。
本论文以单壁碳纳米管（SWNTs）、C_(60)peapods（C_(60)@SWNTs）以及石墨烯纳米片等几种典型的碳纳米材料为主要对象，利用金刚石对顶砧装置对它们开展了详细的高压结构相变研究。
单壁碳纳米管的高压研究方面，很多工作都表明其横截面的形状在压力作用下会发生结构上的变化。当碳管的管状结构发生坍缩之后，在更高压力的作用下它将会进一步发生怎么样的结构变化目前还不十分清楚。本文中对直径分布在1.3nm的高质量的电弧法制备的单壁碳纳米管（arc-SWNTs）样品进行了多个激发光波长的高压拉曼光谱研究。通过对碳管样品拉曼特征峰特别是G-band的详细分析，获得了单壁碳纳米管在高压下发生多个结构相变的完整的物理图像：在2GPa和5GPa碳管的横截面分别发生了由圆形变到椭圆形，再由椭圆形到扁平的跑道状的结构变化；在更高压力15-17GPa左右不同的坍缩碳管之间或是同一碳管的管壁间形成了由sp3键组成的内部键连结构，从而使得G-band的峰位和峰宽出现了突变。这一实验结果为理解单壁碳纳米管特有的高压行为和了解其高压相变机制提供了极其重要的参考价值。从31GPa卸压后的arc-SWNTs样品的高分辨电镜测试和拉曼光谱测试表明大部分碳管样品的结构在卸压后得到了恢复。碳管中形成的sp3键连结构对高压下的碳管起到了很好保护作用，从而使其表现出了非常优异的结构稳定性。
我们进一步对直径分布范围在0.6-1.3nm的宽直径分布的HiPco-SWNTs型碳管进行了使用多种传压介质和不使用传压介质的高压拉曼光谱研究。结合arc-SWNTs样品的高压实验结果，我们对影响碳管高压行为的各种因素进行了详细的分析。研究发现碳管RBM峰的频率ωRBM随压力变化的斜率dωRBM/dp即依赖于碳管的直径又依赖于具体的实验条件。通过与理论计算结果的对比，指出在使用传压介质的情况下，除了压力下碳-碳键硬化效应的影响外，传压介质对碳管RBM的压致频移具有显著的贡献作用，并且与大直径碳管相比，传压介质和小直径的碳管（直径小于0.8nm的碳管）之间有着更强的相互作用。在未使用传压介质的情况下，碳管与碳管间的相互作用对RBM压致频移起着主导作用，而且碳管的管径越小管间相互作用越强。对从不同压力卸压后HiPco-SWNTs样品的研究表明，在不使用传压介质条件下，碳纳米管的塌缩压力依赖于碳管直径，而在使用传压介质的情况下塌缩压力对碳管的直径没有太明显的依赖关系。相比之下，对于arc-SWNTs样品，不论是否使用传压介质，它在经过了31GPa左右的高压处理后都具有很高的结构稳定性。这些结果表明，碳纳米管高压下塌缩后的结构可逆性不仅受到碳纳米管样品自身因素的影响，而且还和其他实验条件密切相关。
在单壁碳纳米管特殊的中空管道中加入C_(60)分子，便得到了一种全新的全碳纳米复合结构材料C_(60)peapod。目前，对peapod的高压工作一般都集中在相对较低的压力范围来研究限域在碳管内的C_(60)分子的变化行为。而在更高的压力下，C_(60)peapod将会有怎样的高压行为和结构变化，目前还缺少实验和理论上的研究。本文利用拉曼光谱、透射电镜及XRD等实验手段对从31GPa、37GPa、52GPa和81GPa卸压的几个C_(60)peapod样品分别进行了结构相变研究。发现37GPa以及更高压力处理后的样品发生了不可逆变化，卸压后所有碳管的管状结构都遭到了破坏。52GPa和81GPa卸压样品的XRD和高分辨电镜等数据表明peapod样品中形成了可以在常压下得到保持的与理论提出的Cco-C8结构相吻合的超硬相。高压实验后金刚石压砧上出现了明显的压痕表明了该结构的超硬特性。与碳管相比，C_(60)peapod样品形成可以在常压下得到保持的超硬结构所需要的压力值明显降低，这说明在碳管的中空孔道中加入C_(60)分子对于降低碳管向超硬结构转变的压力条件具有十分显著的作用。我们的实验发现对于新型碳超硬纳米材料的制备和优异性能材料的合成都具有非常重要的指导意义。
石墨烯纳米片是一种厚度在纳米尺寸的准二维碳纳米材料。我们对石墨烯纳米片样品进行了高压拉曼光谱研究。发现了石墨烯纳米片的高压相变行为：在15GPa左右石墨烯纳米片发生了层间的sp3成键的结构相变。对微米石墨和体石墨的高压研究表明其相变压力在19GPa左右，这明显高于石墨烯纳米片的相变压力。石墨烯纳米片和体石墨在厚度尺寸上的不同是造成它们相变压力不同的原因。提出石墨烯纳米片特殊的有限层数的层状结构和独特的相变成核过程是造成其相变压力降低的主要机制。卸压后样品的透射电镜表征和拉曼光谱测试进一步支持了石墨烯纳米片发生结构相变的物理图像。
Since their unique chemical and physical properties and great potentialapplications in the fields of nanoelectronics and multi-functional materials, carbonnanomaterials, such as single-wall carbon nanotubes (SWNTs) and graphene havebeen the subject of intense investigations. High pressure can effectively change thedistances between molecules and atoms to affect the electron distribution and energyband structure of materials, which will greatly influence or even change the propertiesof materials. High pressure is a powerful method to synthesize new materials, to findnew laws and theories of physics. Carrying out high pressure experiments on carbonnanomaterials can help us deeply understand their various properties and furtherprovide an important way to obain new carbon strutures and new carbon materialssuch as the superhard carbon materials, due to the flexibility of carbon to form sp, sp2,and sp3bonds. These arouse great value in the field of high pressure research oncarbon nanomaterials.
In this thesis, we carried out high pressure research on some typical carbonnanomaterials, such as single-wall carbon nanotubes (SWNTs), C_(60)peapods(C_(60)@SWNTs), and graphene nanoplates by using diamond anvil cell (DAC) to makedetailed research on their structural transitions under pressure.
Extensive high pressure studies on SWNTs have shown that the cross-section ofnanotubes will change in shape under pressure. However, what structural transitionswill happen in a higher pressure region after the pressure-induced collapse hasoccurred in SWNTs? This issue is still not clear up to now. In our work, we studiedthe high-pressure Raman spectra of high quality single-walled carbon nanotubes(arc-SWNTs) with a narrow diameter distribution of1.3nm by using different lasers.Through detailed analysis of the Raman signals of our SWNTs sample, we obtained the whole physical picture of the structural transitions in SWNTs under pressure. Thepressure-induced changes in Raman signals at around2GPa and5GPa can beattributed to the nanotubes’ cross-section changes from circle to ellipse and then to aflattened shape, respectively. At around15-17GPa both the Raman wavenumber andthe linewidth of the G-band as a function as pressure exhibit anomalies. We suggestthat the interlinked configuration with sp3bonds is formed among nanotubes or evenbetween the two opposite walls of a collapsed nanotube for this anomaly, which couldbe corresponding to the anomalies in G-band wavenumber and width. Our HRTEMobservations and Raman measurements on the decompressed samples show that theSWNTs are almost recovered even from31GPa. It is proposed that the formation ofinterlinking sp3C-C bonds in SWNTs stabilize the nanotube structure and thusenhance significantly the high pressure stability of SWNTs.
Raman spectra of HiPco-SWNTs with diameters of0.6–1.3nm was furtherstudied under high pressure. It is found that the pressure dependence of the radialR-band frequency, dω/dp, is diameter and experimental condition dependent.Compared with the theoretical calculation, we believe that besides thepressure-induced hardening of the C-C bond, the effect from PTM contributessignificantly to the pressure-induced upshift of RBMs in the experiments with PTMs,and the interaction between PTM and nanotubes becomes stronger in nanotubes withdiameters smaller than~0.8nm. In the experiments without a PTM, the intertubeinteractions dominate the upshift of RBMs, i.e., the smaller the nanotube diameter, thestronger the intertube interactions. The results thus indicate that the smaller diameternanotubes should have stronger coupling to the PTM in the case with a PTM, andinstead stronger intertube interactions between each other in the case without a PTM.For the HiPco SWNTs upon decompression, it is found that the pressure for thecollapse of a nanotube is diameter dependent in the experiments without a PTM butshows little diameter dependence in the case with a PTM. In contrast, the arc-SWNTsshow high stability even after31GPa compression with or without a PTM. Theseresults suggest that the reversibility of the collapse for a nanotube depends on thenanotube itself and also on other experimental conditions.
The encapsulation of C_(60)molecules into SWNTs can result in a self-assemblednanotube-C_(60)hybrid structure, the so-called peapods C_(60)@SWNTs, a new carboncomposite nanomaterial. Nowadays the high pressure studies on C_(60)peapods mainly focus on the behaviors of confined C_(60)in a relative low pressure region. The structuraltransitions of C_(60)peapods under the higher pressure region are still absent both in theexperimental and theoretical studies. By using Raman spectroscopy, HRTEM andXRD technique, we investigated the structural phase transitions of decompressed C_(60)peapod samples from different pressures of31GPa,37GPa,52GPa,81GPa. It isfound that the initial structure of C_(60)peapod is absolutely destroyed when it isdecompressed from37GPa and the above pressure value. The X-ray diffractionpattern and HRTEM observations on the52GPa and81GPa decompressed samplesindicate that a new quenchable suprhard carbon phase is formed, which is highlyconsistent with the Cco-C8structure proposed by a theoretical work. The ring crackindentations on the diamond anvils following the original boundary of sample in thegasket are found, indicating the exceptional hardness of this new phase. Compared tothe carbon nanotubes, the pressure value to get the quenchable suprhard carbon phaseis obviously reduced. This indicates that the insertion of C_(60)into SWNTs could highlylower the pressure condition to obtain the quenchable suprhard carbon phase. Ourexperimental findings have great guiding significance for the synthesis of newsuperhard carbon materials and the materials with unique properties.
Graphene nanoplate is a quasi two-dimensional carbon nanomaterial with thethickness in nano-scale. High pressure Raman study on graphene nanoplates has beencarried out in a diamond anvil cell. A phase transformation has been observed ingraphene nanoplates at15GPa, which can be explained by the interlayer couplingwith sp3bonds formed in the material. For graphite and micro-graphite, the transitionpressure is19GPa, which is obvious higher than that of graphene nanoplates. Thedifferent thickness of graphene nanoplates/graphite could be responsible for thedifferent phase transition pressure in our experiments. And the lower phase pressurein graphene nanoplates is explained by their specical limited-number layer structureand nucleation process in phase transition. Our TEM observations and Ramanmeasurements on the decompressed samples of graphene nanoplates further support the proposed transformation picture.
本论文以单壁碳纳米管（SWNTs）、C_(60)peapods（C_(60)@SWNTs）以及石墨烯纳米片等几种典型的碳纳米材料为主要对象，利用金刚石对顶砧装置对它们开展了详细的高压结构相变研究。
单壁碳纳米管的高压研究方面，很多工作都表明其横截面的形状在压力作用下会发生结构上的变化。当碳管的管状结构发生坍缩之后，在更高压力的作用下它将会进一步发生怎么样的结构变化目前还不十分清楚。本文中对直径分布在1.3nm的高质量的电弧法制备的单壁碳纳米管（arc-SWNTs）样品进行了多个激发光波长的高压拉曼光谱研究。通过对碳管样品拉曼特征峰特别是G-band的详细分析，获得了单壁碳纳米管在高压下发生多个结构相变的完整的物理图像：在2GPa和5GPa碳管的横截面分别发生了由圆形变到椭圆形，再由椭圆形到扁平的跑道状的结构变化；在更高压力15-17GPa左右不同的坍缩碳管之间或是同一碳管的管壁间形成了由sp3键组成的内部键连结构，从而使得G-band的峰位和峰宽出现了突变。这一实验结果为理解单壁碳纳米管特有的高压行为和了解其高压相变机制提供了极其重要的参考价值。从31GPa卸压后的arc-SWNTs样品的高分辨电镜测试和拉曼光谱测试表明大部分碳管样品的结构在卸压后得到了恢复。碳管中形成的sp3键连结构对高压下的碳管起到了很好保护作用，从而使其表现出了非常优异的结构稳定性。
我们进一步对直径分布范围在0.6-1.3nm的宽直径分布的HiPco-SWNTs型碳管进行了使用多种传压介质和不使用传压介质的高压拉曼光谱研究。结合arc-SWNTs样品的高压实验结果，我们对影响碳管高压行为的各种因素进行了详细的分析。研究发现碳管RBM峰的频率ωRBM随压力变化的斜率dωRBM/dp即依赖于碳管的直径又依赖于具体的实验条件。通过与理论计算结果的对比，指出在使用传压介质的情况下，除了压力下碳-碳键硬化效应的影响外，传压介质对碳管RBM的压致频移具有显著的贡献作用，并且与大直径碳管相比，传压介质和小直径的碳管（直径小于0.8nm的碳管）之间有着更强的相互作用。在未使用传压介质的情况下，碳管与碳管间的相互作用对RBM压致频移起着主导作用，而且碳管的管径越小管间相互作用越强。对从不同压力卸压后HiPco-SWNTs样品的研究表明，在不使用传压介质条件下，碳纳米管的塌缩压力依赖于碳管直径，而在使用传压介质的情况下塌缩压力对碳管的直径没有太明显的依赖关系。相比之下，对于arc-SWNTs样品，不论是否使用传压介质，它在经过了31GPa左右的高压处理后都具有很高的结构稳定性。这些结果表明，碳纳米管高压下塌缩后的结构可逆性不仅受到碳纳米管样品自身因素的影响，而且还和其他实验条件密切相关。
在单壁碳纳米管特殊的中空管道中加入C_(60)分子，便得到了一种全新的全碳纳米复合结构材料C_(60)peapod。目前，对peapod的高压工作一般都集中在相对较低的压力范围来研究限域在碳管内的C_(60)分子的变化行为。而在更高的压力下，C_(60)peapod将会有怎样的高压行为和结构变化，目前还缺少实验和理论上的研究。本文利用拉曼光谱、透射电镜及XRD等实验手段对从31GPa、37GPa、52GPa和81GPa卸压的几个C_(60)peapod样品分别进行了结构相变研究。发现37GPa以及更高压力处理后的样品发生了不可逆变化，卸压后所有碳管的管状结构都遭到了破坏。52GPa和81GPa卸压样品的XRD和高分辨电镜等数据表明peapod样品中形成了可以在常压下得到保持的与理论提出的Cco-C8结构相吻合的超硬相。高压实验后金刚石压砧上出现了明显的压痕表明了该结构的超硬特性。与碳管相比，C_(60)peapod样品形成可以在常压下得到保持的超硬结构所需要的压力值明显降低，这说明在碳管的中空孔道中加入C_(60)分子对于降低碳管向超硬结构转变的压力条件具有十分显著的作用。我们的实验发现对于新型碳超硬纳米材料的制备和优异性能材料的合成都具有非常重要的指导意义。
石墨烯纳米片是一种厚度在纳米尺寸的准二维碳纳米材料。我们对石墨烯纳米片样品进行了高压拉曼光谱研究。发现了石墨烯纳米片的高压相变行为：在15GPa左右石墨烯纳米片发生了层间的sp3成键的结构相变。对微米石墨和体石墨的高压研究表明其相变压力在19GPa左右，这明显高于石墨烯纳米片的相变压力。石墨烯纳米片和体石墨在厚度尺寸上的不同是造成它们相变压力不同的原因。提出石墨烯纳米片特殊的有限层数的层状结构和独特的相变成核过程是造成其相变压力降低的主要机制。卸压后样品的透射电镜表征和拉曼光谱测试进一步支持了石墨烯纳米片发生结构相变的物理图像。
Since their unique chemical and physical properties and great potentialapplications in the fields of nanoelectronics and multi-functional materials, carbonnanomaterials, such as single-wall carbon nanotubes (SWNTs) and graphene havebeen the subject of intense investigations. High pressure can effectively change thedistances between molecules and atoms to affect the electron distribution and energyband structure of materials, which will greatly influence or even change the propertiesof materials. High pressure is a powerful method to synthesize new materials, to findnew laws and theories of physics. Carrying out high pressure experiments on carbonnanomaterials can help us deeply understand their various properties and furtherprovide an important way to obain new carbon strutures and new carbon materialssuch as the superhard carbon materials, due to the flexibility of carbon to form sp, sp2,and sp3bonds. These arouse great value in the field of high pressure research oncarbon nanomaterials.
In this thesis, we carried out high pressure research on some typical carbonnanomaterials, such as single-wall carbon nanotubes (SWNTs), C_(60)peapods(C_(60)@SWNTs), and graphene nanoplates by using diamond anvil cell (DAC) to makedetailed research on their structural transitions under pressure.
Extensive high pressure studies on SWNTs have shown that the cross-section ofnanotubes will change in shape under pressure. However, what structural transitionswill happen in a higher pressure region after the pressure-induced collapse hasoccurred in SWNTs? This issue is still not clear up to now. In our work, we studiedthe high-pressure Raman spectra of high quality single-walled carbon nanotubes(arc-SWNTs) with a narrow diameter distribution of1.3nm by using different lasers.Through detailed analysis of the Raman signals of our SWNTs sample, we obtained the whole physical picture of the structural transitions in SWNTs under pressure. Thepressure-induced changes in Raman signals at around2GPa and5GPa can beattributed to the nanotubes’ cross-section changes from circle to ellipse and then to aflattened shape, respectively. At around15-17GPa both the Raman wavenumber andthe linewidth of the G-band as a function as pressure exhibit anomalies. We suggestthat the interlinked configuration with sp3bonds is formed among nanotubes or evenbetween the two opposite walls of a collapsed nanotube for this anomaly, which couldbe corresponding to the anomalies in G-band wavenumber and width. Our HRTEMobservations and Raman measurements on the decompressed samples show that theSWNTs are almost recovered even from31GPa. It is proposed that the formation ofinterlinking sp3C-C bonds in SWNTs stabilize the nanotube structure and thusenhance significantly the high pressure stability of SWNTs.
Raman spectra of HiPco-SWNTs with diameters of0.6–1.3nm was furtherstudied under high pressure. It is found that the pressure dependence of the radialR-band frequency, dω/dp, is diameter and experimental condition dependent.Compared with the theoretical calculation, we believe that besides thepressure-induced hardening of the C-C bond, the effect from PTM contributessignificantly to the pressure-induced upshift of RBMs in the experiments with PTMs,and the interaction between PTM and nanotubes becomes stronger in nanotubes withdiameters smaller than~0.8nm. In the experiments without a PTM, the intertubeinteractions dominate the upshift of RBMs, i.e., the smaller the nanotube diameter, thestronger the intertube interactions. The results thus indicate that the smaller diameternanotubes should have stronger coupling to the PTM in the case with a PTM, andinstead stronger intertube interactions between each other in the case without a PTM.For the HiPco SWNTs upon decompression, it is found that the pressure for thecollapse of a nanotube is diameter dependent in the experiments without a PTM butshows little diameter dependence in the case with a PTM. In contrast, the arc-SWNTsshow high stability even after31GPa compression with or without a PTM. Theseresults suggest that the reversibility of the collapse for a nanotube depends on thenanotube itself and also on other experimental conditions.
The encapsulation of C_(60)molecules into SWNTs can result in a self-assemblednanotube-C_(60)hybrid structure, the so-called peapods C_(60)@SWNTs, a new carboncomposite nanomaterial. Nowadays the high pressure studies on C_(60)peapods mainly focus on the behaviors of confined C_(60)in a relative low pressure region. The structuraltransitions of C_(60)peapods under the higher pressure region are still absent both in theexperimental and theoretical studies. By using Raman spectroscopy, HRTEM andXRD technique, we investigated the structural phase transitions of decompressed C_(60)peapod samples from different pressures of31GPa,37GPa,52GPa,81GPa. It isfound that the initial structure of C_(60)peapod is absolutely destroyed when it isdecompressed from37GPa and the above pressure value. The X-ray diffractionpattern and HRTEM observations on the52GPa and81GPa decompressed samplesindicate that a new quenchable suprhard carbon phase is formed, which is highlyconsistent with the Cco-C8structure proposed by a theoretical work. The ring crackindentations on the diamond anvils following the original boundary of sample in thegasket are found, indicating the exceptional hardness of this new phase. Compared tothe carbon nanotubes, the pressure value to get the quenchable suprhard carbon phaseis obviously reduced. This indicates that the insertion of C_(60)into SWNTs could highlylower the pressure condition to obtain the quenchable suprhard carbon phase. Ourexperimental findings have great guiding significance for the synthesis of newsuperhard carbon materials and the materials with unique properties.
Graphene nanoplate is a quasi two-dimensional carbon nanomaterial with thethickness in nano-scale. High pressure Raman study on graphene nanoplates has beencarried out in a diamond anvil cell. A phase transformation has been observed ingraphene nanoplates at15GPa, which can be explained by the interlayer couplingwith sp3bonds formed in the material. For graphite and micro-graphite, the transitionpressure is19GPa, which is obvious higher than that of graphene nanoplates. Thedifferent thickness of graphene nanoplates/graphite could be responsible for thedifferent phase transition pressure in our experiments. And the lower phase pressurein graphene nanoplates is explained by their specical limited-number layer structureand nucleation process in phase transition. Our TEM observations and Ramanmeasurements on the decompressed samples of graphene nanoplates further support the proposed transformation picture.
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