碳纳米材料的X射线吸收谱学研究
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摘要
纳米材料研究是理论和实验领域的一个热门课题。碳纳米材料由于具有独特的结构和优异的物理化学性质,在复合材料、微电子器件、生物医学以及灵敏传感器等领域有着广泛的潜在应用。然而,在碳纳米材料走向实际应用的过程中,对其进行相应的功能化和电子结构调制是非常关键的一步。因此,在碳纳米材料的修饰改性以及掺杂方面的研究具有非常重要的研究和应用意义。
本论文利用X射线近边吸收谱对碳纳米管的修饰和纯化以及石墨烯的掺杂和氧化还原进行了系统的研究,展示了X射线近边吸收谱在碳纳米材料结构表征和机理研究中的特殊功能。
a、利用X射线近边吸收谱研究了碳纳米管的硝酸修饰过程以及在这个过程中所产生的碳碎片问题：
1)通过X射线近边吸收谱对单壁碳纳米管的稀硝酸处理过程进行了系统的研究。实验结果清楚的表明了碳纳米管管壁吸附的碳碎片的存在,这种碳碎片将有效减少硝酸对碳纳米管管壁的直接氧化。吸收谱实验显示硝酸处理后产生的羧基基团同时存在于碳碎片和单壁碳纳米管管壁上,但单壁碳纳米管管壁只被轻微的氧化。硝酸氧化后的碳碎片可以通过氢氧化钠溶液清洗来去除,去除碳碎片之后,进一步的硝酸处理能够直接修饰单壁碳纳米管的侧壁。实验证明去除吸附的碳碎片才能够对单壁碳纳米管管壁进行有效的修饰。吸收谱还显示碳碎片主要来源于碳纳米管制备过程中所产生的无定形碳和在硝酸处理过程中被打碎的单壁碳纳米管。
2)还利用X射线近边吸收谱对单壁碳纳米管和多壁碳纳米管的浓硝酸处理进行了对比研究。吸收谱结果表明,单壁碳纳米管很容易被浓硝酸破坏形成碳碎片,所产生的羧基基团主要存在于碳碎片上。而多壁碳纳米管结构相对比较稳定,而且管壁层数多,能够在侧壁上产生大量的共价氧化基团。前面的研究已经证明稀硝酸能够有效的修饰单壁碳纳米管。因此,对于不同结构的碳纳米管应当选择适当的硝酸处理条件,这样才能有效的提高碳纳米管的功能化程度。
3)同时还用X射线近边吸收谱研究了退火处理对氧化碳碎片的去除效果。吸收谱结果证明在惰性气体中对硝酸处理过的单壁碳纳米管进行退火处理能够有效的去除吸附在碳纳米管上的氧化碳碎片,而这些氧化碳碎片是很难通过水的冲洗来去除的。除了以前所报道的氢氧化钠溶液清洗外,本实验提出了另外一种去除氧化碳碎片的办法。
b、通过X射线近边吸收谱对碳纳米管的共价与非共价修饰进行了详细的研究：
1)利用X射线近边吸收谱研究了不同温度下气态硝酸对多壁碳纳米管的氧化修饰。吸收谱结果表明,硝酸气体能够有效的氧化修饰多壁碳纳米管,通过对处理温度的控制能够有效的调节修饰到多壁碳纳米管表面的氧化基团的数量。更重要的是这种实验方法简单,样品不需要进行过滤和清洗,可以进行大批量的改性功能化。
2)同时还利用X射线近边吸收谱研究了单壁碳纳米管的苯丙氨酸和甘氨酸吸附。吸收谱结果证实了氨基酸的吸附。吸附到单壁碳纳米管上的甘氨酸的C=0π*峰出现一个明显的能量位移,说明氨基酸和单壁碳纳米管间存在着相互作用。
c、基于X射线近边吸收谱对石墨烯的N掺杂和氧化还原过程中电子结构及局域结构的变化进行了研究：
1)结合X射线近边吸收谱和光电子能谱研究了氧化石墨烯在N掺杂过程中结构随温度的变化。N掺杂的石墨烯是通过把氧化石墨烯放到氨气气氛中退火得到的。吸收谱结果表明,石墨烯中主要存在三种N掺杂结构：吡啶型、氨基和石墨型。在低温下,掺杂的N主要是以氨基的形式存在,这些氨基会在高温下分解。而在高温下,N原子倾向于取代石墨层中的碳原子而形成吡啶型和石墨型结构。N的光电子能谱也证实了这个实验结果。从0的K边吸收谱上同时发现大量的氧化基团存在于氧化石墨烯上,并随着退火温度的升高而迅速减少。
2)同时还利用X射线近边吸收谱研究了氧化石墨烯在氢气和水合肼中的还原过程。实验结果发现,这两种还原方法都能够实现氧化基团的大量减少。氢气需要在较高的温度下才能还原环氧基团,而水合肼则比较容易与环氧基团发生反应。此外,水合肼还原会在石墨烯中引入一些N原子。
Nano-materials researches represent a hot topic in both theoretical and experimental physics. Due to their unique structures extraordinary physical and chemical properties, carbon-based materials will make possible new applications in the field of composite materials, microelectronic devices, biomedicine, sensors etc. However, the route toward real applications needs the control of functionalization and of the electronic properties of carbon-based nano-materials and additional investigations are required to learn how modify and dope these materials.
In this thesis, a systematic study on the modification and purification of carbon nanotubes (CNTs) as well as on the doping and redox of graphene has been performed by means of X-ray absorption fine structure (XANES) spectroscopy. It shows the unique capabilities of the XANES spectroscopy to characterize structures and bonding of carbon-based nano-materials.
a) XANES spectroscopy has been applied to investigate the modification of CNTs by nitric acid and the production of carbonaceous fragments during the process.
1. This local spectroscopy has been used to identify changes induced on single-walled carbon nanotubes (SWCNTs) treated by mild nitric acid. Experimental results confirm the occurrence of carbonaceous fragments absorbed on SWCNTs, and these fragments would reduce the direct modification of SWCNTs by nitric acid.
XANES indicate the carboxyl groups created by the nitric acid treatment have been found on both carbonaceous fragments and the side-walls of SWCNTs. Moreover, these carbonaceous fragments can be removed by a washing treatment with sodium hydroxide. SWCNTs walls are weakly oxidized by the nitric acid treatment although, after the fragments removal a direct oxidation process of SWCNTs has been observed. Data address the removal of carbonaceous fragments on SWCNTs as an efficient method for side-wall modification of SWCNT. XANES also indicate that carbonaceous fragments are the result of the synthesis process and/or of the nitric acid treatment.
2. A comparative XANES study of the modification of both SWCNTs and multi-walled carbon nanotubes (MWCNTs) via concentrate nitric acid has been performed. Data indicate that SWCNTs are easily destroyed by concentrate nitric acid treatment generating the carbonaceous fragments that contain the majority of carboxyl groups. However, due to their higher structural stability and thicker tube walls, high sidewall modification was observed on MWCNTs. An effective modification on SWCNTs by mild nitric acid treatment has been studied before. It was suggested that a proper selection of treatment conditions and CNTs type may effectively control the modifications of these materials.
3. XANES spectroscopy was also used to investigate the removal of oxidative carbonaceous fragments absorbed on SWCNTs. Data show that the annealing treatment in an inert gas atmosphere may effectively remove these fragments hardly removed by water washing. Results point out an alternative procedure to separate the tightly adsorbed fragments from SWCNTs respect to the previously reported NaOH washing.
b. XANES spectroscopy was applied to carefully investigate covalent and non-covalent modifications of CNTs.
1) We investigated the modification of MWCNTs via gas nitric acid vs. temperature. XANES indicate that MWCNTs can be effectively modified by gas nitric acid and the amount of oxygen-functional groups can be controlled by the modulation of the temperature. If compared to the liquid nitric acid treatment this method is easy and modified samples do not need washing and filtration. This gas-phase route is also suitable for mass production.
2) We studied also the adsorption of phenylalanine and glycine on SWCNTs and the adsorption of amino acids has been confirmed by XANES analysis. An observed energy shift of the C 1s to C=Oπ* peak for glycine absorbed on SWCNTs has been identified and assigned to the interaction between the amino acid and SWCNTs.
c. The electronic and local structures of graphene after N-doping and redox have been also studied by XANES spectroscopy.
1) In this study we combined XANES and X-ray photoelectron spectroscopy (XPS) to investigate the structural changes of N-doping graphene at different annealing temperatures. N-doping graphene samples were obtained by annealing the graphene oxide in an ammonia atmosphere. N K-edge XANES spectra indicate three different N-doping structures in the graphene layer:pyridine, amino and graphitic type. At low temperature, the doped nitrogens are of amino type and would decompose increasing the temperature. At high temperature, most of the doped nitrogens replace carbon atoms in the graphene layer forming both pyridine and graphitic doping structure. N 1 s XPS analysis is in good agreement with XANES data. In addition,O K-edge XANES spectra reveal that many oxygen-containing functional groups occur on the graphene oxide layer and are greatly reduced with temperature.
2) The XANES spectroscopy has been also applied to investigate both chemical bonding and electronic structure of the graphene oxide layer after hydrogen and hydrazine reduction. Results indicate that both hydrogen and hydrazine may effectively reduce the graphene oxide. Hydrogen would react only at high temperature while hydrazine easily reacts with the epoxy groups. Actually, some N atoms are introduced in the graphene layers during the hydrazine reduction.
本论文利用X射线近边吸收谱对碳纳米管的修饰和纯化以及石墨烯的掺杂和氧化还原进行了系统的研究,展示了X射线近边吸收谱在碳纳米材料结构表征和机理研究中的特殊功能。
a、利用X射线近边吸收谱研究了碳纳米管的硝酸修饰过程以及在这个过程中所产生的碳碎片问题：
1)通过X射线近边吸收谱对单壁碳纳米管的稀硝酸处理过程进行了系统的研究。实验结果清楚的表明了碳纳米管管壁吸附的碳碎片的存在,这种碳碎片将有效减少硝酸对碳纳米管管壁的直接氧化。吸收谱实验显示硝酸处理后产生的羧基基团同时存在于碳碎片和单壁碳纳米管管壁上,但单壁碳纳米管管壁只被轻微的氧化。硝酸氧化后的碳碎片可以通过氢氧化钠溶液清洗来去除,去除碳碎片之后,进一步的硝酸处理能够直接修饰单壁碳纳米管的侧壁。实验证明去除吸附的碳碎片才能够对单壁碳纳米管管壁进行有效的修饰。吸收谱还显示碳碎片主要来源于碳纳米管制备过程中所产生的无定形碳和在硝酸处理过程中被打碎的单壁碳纳米管。
2)还利用X射线近边吸收谱对单壁碳纳米管和多壁碳纳米管的浓硝酸处理进行了对比研究。吸收谱结果表明,单壁碳纳米管很容易被浓硝酸破坏形成碳碎片,所产生的羧基基团主要存在于碳碎片上。而多壁碳纳米管结构相对比较稳定,而且管壁层数多,能够在侧壁上产生大量的共价氧化基团。前面的研究已经证明稀硝酸能够有效的修饰单壁碳纳米管。因此,对于不同结构的碳纳米管应当选择适当的硝酸处理条件,这样才能有效的提高碳纳米管的功能化程度。
3)同时还用X射线近边吸收谱研究了退火处理对氧化碳碎片的去除效果。吸收谱结果证明在惰性气体中对硝酸处理过的单壁碳纳米管进行退火处理能够有效的去除吸附在碳纳米管上的氧化碳碎片,而这些氧化碳碎片是很难通过水的冲洗来去除的。除了以前所报道的氢氧化钠溶液清洗外,本实验提出了另外一种去除氧化碳碎片的办法。
b、通过X射线近边吸收谱对碳纳米管的共价与非共价修饰进行了详细的研究：
1)利用X射线近边吸收谱研究了不同温度下气态硝酸对多壁碳纳米管的氧化修饰。吸收谱结果表明,硝酸气体能够有效的氧化修饰多壁碳纳米管,通过对处理温度的控制能够有效的调节修饰到多壁碳纳米管表面的氧化基团的数量。更重要的是这种实验方法简单,样品不需要进行过滤和清洗,可以进行大批量的改性功能化。
2)同时还利用X射线近边吸收谱研究了单壁碳纳米管的苯丙氨酸和甘氨酸吸附。吸收谱结果证实了氨基酸的吸附。吸附到单壁碳纳米管上的甘氨酸的C=0π*峰出现一个明显的能量位移,说明氨基酸和单壁碳纳米管间存在着相互作用。
c、基于X射线近边吸收谱对石墨烯的N掺杂和氧化还原过程中电子结构及局域结构的变化进行了研究：
1)结合X射线近边吸收谱和光电子能谱研究了氧化石墨烯在N掺杂过程中结构随温度的变化。N掺杂的石墨烯是通过把氧化石墨烯放到氨气气氛中退火得到的。吸收谱结果表明,石墨烯中主要存在三种N掺杂结构：吡啶型、氨基和石墨型。在低温下,掺杂的N主要是以氨基的形式存在,这些氨基会在高温下分解。而在高温下,N原子倾向于取代石墨层中的碳原子而形成吡啶型和石墨型结构。N的光电子能谱也证实了这个实验结果。从0的K边吸收谱上同时发现大量的氧化基团存在于氧化石墨烯上,并随着退火温度的升高而迅速减少。
2)同时还利用X射线近边吸收谱研究了氧化石墨烯在氢气和水合肼中的还原过程。实验结果发现,这两种还原方法都能够实现氧化基团的大量减少。氢气需要在较高的温度下才能还原环氧基团,而水合肼则比较容易与环氧基团发生反应。此外,水合肼还原会在石墨烯中引入一些N原子。
Nano-materials researches represent a hot topic in both theoretical and experimental physics. Due to their unique structures extraordinary physical and chemical properties, carbon-based materials will make possible new applications in the field of composite materials, microelectronic devices, biomedicine, sensors etc. However, the route toward real applications needs the control of functionalization and of the electronic properties of carbon-based nano-materials and additional investigations are required to learn how modify and dope these materials.
In this thesis, a systematic study on the modification and purification of carbon nanotubes (CNTs) as well as on the doping and redox of graphene has been performed by means of X-ray absorption fine structure (XANES) spectroscopy. It shows the unique capabilities of the XANES spectroscopy to characterize structures and bonding of carbon-based nano-materials.
a) XANES spectroscopy has been applied to investigate the modification of CNTs by nitric acid and the production of carbonaceous fragments during the process.
1. This local spectroscopy has been used to identify changes induced on single-walled carbon nanotubes (SWCNTs) treated by mild nitric acid. Experimental results confirm the occurrence of carbonaceous fragments absorbed on SWCNTs, and these fragments would reduce the direct modification of SWCNTs by nitric acid.
XANES indicate the carboxyl groups created by the nitric acid treatment have been found on both carbonaceous fragments and the side-walls of SWCNTs. Moreover, these carbonaceous fragments can be removed by a washing treatment with sodium hydroxide. SWCNTs walls are weakly oxidized by the nitric acid treatment although, after the fragments removal a direct oxidation process of SWCNTs has been observed. Data address the removal of carbonaceous fragments on SWCNTs as an efficient method for side-wall modification of SWCNT. XANES also indicate that carbonaceous fragments are the result of the synthesis process and/or of the nitric acid treatment.
2. A comparative XANES study of the modification of both SWCNTs and multi-walled carbon nanotubes (MWCNTs) via concentrate nitric acid has been performed. Data indicate that SWCNTs are easily destroyed by concentrate nitric acid treatment generating the carbonaceous fragments that contain the majority of carboxyl groups. However, due to their higher structural stability and thicker tube walls, high sidewall modification was observed on MWCNTs. An effective modification on SWCNTs by mild nitric acid treatment has been studied before. It was suggested that a proper selection of treatment conditions and CNTs type may effectively control the modifications of these materials.
3. XANES spectroscopy was also used to investigate the removal of oxidative carbonaceous fragments absorbed on SWCNTs. Data show that the annealing treatment in an inert gas atmosphere may effectively remove these fragments hardly removed by water washing. Results point out an alternative procedure to separate the tightly adsorbed fragments from SWCNTs respect to the previously reported NaOH washing.
b. XANES spectroscopy was applied to carefully investigate covalent and non-covalent modifications of CNTs.
1) We investigated the modification of MWCNTs via gas nitric acid vs. temperature. XANES indicate that MWCNTs can be effectively modified by gas nitric acid and the amount of oxygen-functional groups can be controlled by the modulation of the temperature. If compared to the liquid nitric acid treatment this method is easy and modified samples do not need washing and filtration. This gas-phase route is also suitable for mass production.
2) We studied also the adsorption of phenylalanine and glycine on SWCNTs and the adsorption of amino acids has been confirmed by XANES analysis. An observed energy shift of the C 1s to C=Oπ* peak for glycine absorbed on SWCNTs has been identified and assigned to the interaction between the amino acid and SWCNTs.
c. The electronic and local structures of graphene after N-doping and redox have been also studied by XANES spectroscopy.
1) In this study we combined XANES and X-ray photoelectron spectroscopy (XPS) to investigate the structural changes of N-doping graphene at different annealing temperatures. N-doping graphene samples were obtained by annealing the graphene oxide in an ammonia atmosphere. N K-edge XANES spectra indicate three different N-doping structures in the graphene layer:pyridine, amino and graphitic type. At low temperature, the doped nitrogens are of amino type and would decompose increasing the temperature. At high temperature, most of the doped nitrogens replace carbon atoms in the graphene layer forming both pyridine and graphitic doping structure. N 1 s XPS analysis is in good agreement with XANES data. In addition,O K-edge XANES spectra reveal that many oxygen-containing functional groups occur on the graphene oxide layer and are greatly reduced with temperature.
2) The XANES spectroscopy has been also applied to investigate both chemical bonding and electronic structure of the graphene oxide layer after hydrogen and hydrazine reduction. Results indicate that both hydrogen and hydrazine may effectively reduce the graphene oxide. Hydrogen would react only at high temperature while hydrazine easily reacts with the epoxy groups. Actually, some N atoms are introduced in the graphene layers during the hydrazine reduction.
引文
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