新型稀土复合催化剂合成单壁碳纳米管及其高压结构相变研究
摘要
控制单壁碳纳米管的生长、高产率制备具有不同结构的纳米管一直是倍受关注的课题。催化剂的选择是解决这一问题的关键。通过对比分析,选择了与Y具有相似电子结构的稀土元素Ho,深入系统的研究新的复合催化剂Ho/Ni合成碳管。高产率地获得了高纯度的单壁碳纳米管;寻找到碳纳米管合成最优控制条件及其对碳管直径和结构的影响规律;还通过简单地改变等离子气流,极为简便地获得了长达20厘米的条带状纳米管聚集体。
我们深入、系统地研究了14个新型稀土金属/镍在合成单壁碳纳米管中的催化作用和规律。揭示出系列稀土金属/镍的催化效果规律:3价、4价的稀土金属的催化效果好,2价的稀土金属催化效果极差;在3价、4价的金属中,钬、铒、钇的催化效果更佳。随着稀土金属原子半径减少,样品中小直径的单壁碳管部分也在减小,而大直径的碳管部分增加。发现稀土金属的催化效果与其碳化物的形成能力有关,催化效果好的3价和4价稀土金属,均能形成金属碳化物,而催化效果差的二价金属很难形成金属碳化物,为进一步理解碳管的形成机制提供了线索。这些结果不仅对高产率合成单壁碳纳米管,也对进一步控制合成单壁碳纳米管有重要的指导意义,为制备不同结构的单壁碳纳米管提供了合适的选择体系。
首次采用近红外激发波长,在位研究了具有宽直径分布的单壁碳纳米管在不同静水压条件下的高压拉曼光谱,探讨了单壁碳纳米管在高压下的结构变化规律。首次在高于14Gpa的压力下仍观察到碳管的基本呼吸模(R-band),在一定压力范围内,观察到切向振动模的频率随压力的升高存在反常的平台现象(G-band平台),同时在平台起始压力点附近,伴随着基本呼吸模强度的明显降低,而且RBM频率近线性地贯穿G-band平台;采用第一性原理模拟了碳管在高压下的结构变化及其相应的拉曼光谱,揭示出碳管在高压下发生了由圆到椭圆再到扁平椭圆结构的形变。G平台的出现和R-band的强度下降可以作为判断高压下碳管发生相变的依据。
The unique structure of single-walled carbon nanotubes (SWNTs) and their fascinating physical and chemical properites imply a great potential in nanoscience and in technological applications. In this thesis, we systemically study the synthesis and characterization of SWNTs with a series of novel rare-earth/Ni as catalyst by arc discharge and investigate the high pressure induced structural transition of SWNTs.
The properties of SWNTs are strongly dependent on their structure, such as helicity and diameter. The applications of SWNTs require large-scale synthesis of SWNTs with desired nanostructures and with high purity. One of the most critical parameters in SWNTs synthesis is the catalyst used. It has been found that the catalyst has strong effect on the nanostructure and the yield and even the macroscopical morphology of as-synthesized SWNTs. Therefore, to explore and study new high efficiency catalyst for large-scale synthesis of SWNTs is always nessary and important. Such studies will provide valuable information to control the synthesis of SWNTs and further understand the growth mechanism of SWNTs.
One of the most widely used methods, the DC arc discharge method, can produce SWNTs with a high degree of crystallinity and low defect concentration on a large scale. Here, we synthesize SWNTs in high yield and high purity by this method with a new bimetallic catalyst Ho/Ni for the first time. The morphologies, diameter distribution and the content of SWNTs in the products are characterized by SEM, TEM, Raman spectroscopy, TGA and UV-NIR spectroscopies. Long SWNTs ribbons, consisting of roughly aligned and relatively high purity SWNTs bundles have been synthesized with Ho/Ni as catalyst by using a simple modified arc discharge apparatus. The introduction of Ho/Ni as catalyst and the convection enhanced by the modification of the apparatus play important roles in the formation of these ribbons. Changing the Ho and Ni concentrations in the catalyst hardly affects the diameter distribution but strongly affects the yield of SWNTs. An optimal range of Ho/Ni composition for synthesis of SWNTs with relatively high purity and yield has been obtained. The best yield of SWNTs obtained by Ho/Ni catalyst is as good as the highest yield of SWNTs by Y/Ni catalyst ever reported. The present synthesis process can be easily manipulated and is promising for large-scale production. We also discuss the growth mechanism of SWNTs and suggest that Ho play important roles for enhancing the nucleation ratio of SWNTs in the SWNTs growth process.
A systematic experimental study has been carried out on the efficiency of a series of novel bimetallic catalysts based on Ni and the rare-earth elements in the synthesis of SWNTs. Most of rare earth metals studied here have not been reported as catalyst component for the synthesis of SWNTs, except for La, Ce, Tb and Y. We employ SEM, TEM, Raman spectroscopy and UV-NIR spectroscopy to study the effect of novel catalysts on the purity and nanostructure of as-synthesized SWNTs. The results indicate that the elements with a valence of +3 or +4 have an obvious catalytic effect and increase the yield of SWNTs dramatically, including La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er, Lu and Y. Among them, Ho/Ni, Er/Ni and Y/Ni give the best yield. However, those rare earth elements having a valence of +2 are not efficient catalysts, including Sm, Eu, Tm and Yb. We also find a rule of the influence of rare-earth elements on the diameter distribution of as-synthesized SWNTs when analyzed by a combination of Raman and UV-NIR spectroscopy. For the metals having an obvious catalytic effeciency, there is a tendency that the fraction of small-diameter tubes decreases while large-diameter tubes increases with decreasing ionic radius of the rare-earth element used. EDX and X-ray analyses indicate that the rare earth metals having an obvious catalytic effect deposit on the cathode deposits and form rare-earth carbides, whereas the inefficient catalyst metals have not been found in cathode deposits, except for a small amount of Tm present in the form of thulium carbide. Further analysis indicates that there is a very strong correlation between the ability to form rare-earth carbides and the catalytic efficiency for the formation of SWNTs.
SWNTs can be taken as a representative qusi-one-dimensional model material. The investigation of their structural evolution under high pressure is always an important topic, which can provide information on the stability and phase transitions of SWNTs under compression. In this work, we employ three excitation wavelengths to study the high pressure Raman spectra of SWNTs under hydrostatic and non-hydrostatic conditions. A near IR laser (830nm) is used in this work for the first time. For comparison, other two excitation wavelengths, 514.5 nm and 633 nm are used as well. The IR laser produces a strong Raman signal and gives us the opportunity to observe radial breathing modes even up to 14GPa for the first time. We find that a plateau occurs for the G-band under high pressure. But unlike what is observed in previous studies, the RBM frequencies shift up almost linearly throughout the plateau of the G-band, without an abrupt change. However, near the critical onset pressure where the G-band plateau starts, the intensity of the RBM significantly decreases. This phenomenon occurs regardless of whether a PTM is used or not, and does not depend on the identity of the PTM, on the diameter of tubes, or on the excitation laser. Based on the first principles calculations using the Local Density Approximation (LDA) in density functional theory (DFT), we simulate the structural changes of the chosen SWNT model and calculate the Raman frequencies of the deformed nanotube under compression, yielding the frequencies of the Raman modes as functions of structural evolution. The results indicate that when the structural transition of SWNTs cross-section from an ellipse-like shape to a flattened oval shape is induced, the change of both RBM and G-band in theory is well consistent with that observed in our experiments. The emergence of a pressure plateau for the G-band accompanied by a significant decrease in the intensity of RBM peaks thus can be used as a signature of the structural transition of SWNTs under high pressure.
我们深入、系统地研究了14个新型稀土金属/镍在合成单壁碳纳米管中的催化作用和规律。揭示出系列稀土金属/镍的催化效果规律:3价、4价的稀土金属的催化效果好,2价的稀土金属催化效果极差;在3价、4价的金属中,钬、铒、钇的催化效果更佳。随着稀土金属原子半径减少,样品中小直径的单壁碳管部分也在减小,而大直径的碳管部分增加。发现稀土金属的催化效果与其碳化物的形成能力有关,催化效果好的3价和4价稀土金属,均能形成金属碳化物,而催化效果差的二价金属很难形成金属碳化物,为进一步理解碳管的形成机制提供了线索。这些结果不仅对高产率合成单壁碳纳米管,也对进一步控制合成单壁碳纳米管有重要的指导意义,为制备不同结构的单壁碳纳米管提供了合适的选择体系。
首次采用近红外激发波长,在位研究了具有宽直径分布的单壁碳纳米管在不同静水压条件下的高压拉曼光谱,探讨了单壁碳纳米管在高压下的结构变化规律。首次在高于14Gpa的压力下仍观察到碳管的基本呼吸模(R-band),在一定压力范围内,观察到切向振动模的频率随压力的升高存在反常的平台现象(G-band平台),同时在平台起始压力点附近,伴随着基本呼吸模强度的明显降低,而且RBM频率近线性地贯穿G-band平台;采用第一性原理模拟了碳管在高压下的结构变化及其相应的拉曼光谱,揭示出碳管在高压下发生了由圆到椭圆再到扁平椭圆结构的形变。G平台的出现和R-band的强度下降可以作为判断高压下碳管发生相变的依据。
The unique structure of single-walled carbon nanotubes (SWNTs) and their fascinating physical and chemical properites imply a great potential in nanoscience and in technological applications. In this thesis, we systemically study the synthesis and characterization of SWNTs with a series of novel rare-earth/Ni as catalyst by arc discharge and investigate the high pressure induced structural transition of SWNTs.
The properties of SWNTs are strongly dependent on their structure, such as helicity and diameter. The applications of SWNTs require large-scale synthesis of SWNTs with desired nanostructures and with high purity. One of the most critical parameters in SWNTs synthesis is the catalyst used. It has been found that the catalyst has strong effect on the nanostructure and the yield and even the macroscopical morphology of as-synthesized SWNTs. Therefore, to explore and study new high efficiency catalyst for large-scale synthesis of SWNTs is always nessary and important. Such studies will provide valuable information to control the synthesis of SWNTs and further understand the growth mechanism of SWNTs.
One of the most widely used methods, the DC arc discharge method, can produce SWNTs with a high degree of crystallinity and low defect concentration on a large scale. Here, we synthesize SWNTs in high yield and high purity by this method with a new bimetallic catalyst Ho/Ni for the first time. The morphologies, diameter distribution and the content of SWNTs in the products are characterized by SEM, TEM, Raman spectroscopy, TGA and UV-NIR spectroscopies. Long SWNTs ribbons, consisting of roughly aligned and relatively high purity SWNTs bundles have been synthesized with Ho/Ni as catalyst by using a simple modified arc discharge apparatus. The introduction of Ho/Ni as catalyst and the convection enhanced by the modification of the apparatus play important roles in the formation of these ribbons. Changing the Ho and Ni concentrations in the catalyst hardly affects the diameter distribution but strongly affects the yield of SWNTs. An optimal range of Ho/Ni composition for synthesis of SWNTs with relatively high purity and yield has been obtained. The best yield of SWNTs obtained by Ho/Ni catalyst is as good as the highest yield of SWNTs by Y/Ni catalyst ever reported. The present synthesis process can be easily manipulated and is promising for large-scale production. We also discuss the growth mechanism of SWNTs and suggest that Ho play important roles for enhancing the nucleation ratio of SWNTs in the SWNTs growth process.
A systematic experimental study has been carried out on the efficiency of a series of novel bimetallic catalysts based on Ni and the rare-earth elements in the synthesis of SWNTs. Most of rare earth metals studied here have not been reported as catalyst component for the synthesis of SWNTs, except for La, Ce, Tb and Y. We employ SEM, TEM, Raman spectroscopy and UV-NIR spectroscopy to study the effect of novel catalysts on the purity and nanostructure of as-synthesized SWNTs. The results indicate that the elements with a valence of +3 or +4 have an obvious catalytic effect and increase the yield of SWNTs dramatically, including La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er, Lu and Y. Among them, Ho/Ni, Er/Ni and Y/Ni give the best yield. However, those rare earth elements having a valence of +2 are not efficient catalysts, including Sm, Eu, Tm and Yb. We also find a rule of the influence of rare-earth elements on the diameter distribution of as-synthesized SWNTs when analyzed by a combination of Raman and UV-NIR spectroscopy. For the metals having an obvious catalytic effeciency, there is a tendency that the fraction of small-diameter tubes decreases while large-diameter tubes increases with decreasing ionic radius of the rare-earth element used. EDX and X-ray analyses indicate that the rare earth metals having an obvious catalytic effect deposit on the cathode deposits and form rare-earth carbides, whereas the inefficient catalyst metals have not been found in cathode deposits, except for a small amount of Tm present in the form of thulium carbide. Further analysis indicates that there is a very strong correlation between the ability to form rare-earth carbides and the catalytic efficiency for the formation of SWNTs.
SWNTs can be taken as a representative qusi-one-dimensional model material. The investigation of their structural evolution under high pressure is always an important topic, which can provide information on the stability and phase transitions of SWNTs under compression. In this work, we employ three excitation wavelengths to study the high pressure Raman spectra of SWNTs under hydrostatic and non-hydrostatic conditions. A near IR laser (830nm) is used in this work for the first time. For comparison, other two excitation wavelengths, 514.5 nm and 633 nm are used as well. The IR laser produces a strong Raman signal and gives us the opportunity to observe radial breathing modes even up to 14GPa for the first time. We find that a plateau occurs for the G-band under high pressure. But unlike what is observed in previous studies, the RBM frequencies shift up almost linearly throughout the plateau of the G-band, without an abrupt change. However, near the critical onset pressure where the G-band plateau starts, the intensity of the RBM significantly decreases. This phenomenon occurs regardless of whether a PTM is used or not, and does not depend on the identity of the PTM, on the diameter of tubes, or on the excitation laser. Based on the first principles calculations using the Local Density Approximation (LDA) in density functional theory (DFT), we simulate the structural changes of the chosen SWNT model and calculate the Raman frequencies of the deformed nanotube under compression, yielding the frequencies of the Raman modes as functions of structural evolution. The results indicate that when the structural transition of SWNTs cross-section from an ellipse-like shape to a flattened oval shape is induced, the change of both RBM and G-band in theory is well consistent with that observed in our experiments. The emergence of a pressure plateau for the G-band accompanied by a significant decrease in the intensity of RBM peaks thus can be used as a signature of the structural transition of SWNTs under high pressure.
引文
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