高质量多壁碳纳米管的制备方法和应用研究
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摘要
碳纳米管具有十分独特的结构和优异的物理化学性能，在纳米电子器件、复合材料、传感器等诸多领域有着巨大的应用前景。目前，工业化的碳纳米管以CVD方法生长为主，由于其生长温度低，石墨化程度低，导致结构缺陷多，严重制约了它们优异性能的发挥。其他的碳管合成方法或生产成本高，或比较耗时，且产量较低，不能够满足实际应用。因此，探索高质量、低缺陷的碳纳米管的低成本、批量化制备具有非常重要的现实意义。本论文的主要工作是围绕高质量、低缺陷的多壁碳纳米管的大量制备及其在场发射和铜复合材料的应用展开，获得的主要结果包括：
1.采用一种新颖的快速自加热方法高温退火处理CVD多壁碳纳米管，能够有效地提高多壁碳纳米管的有序结构，减少缺陷。介绍了一种简单、高效、可靠的剪切碳纳米管的方法，剪切后的碳纳米管主要集中在200–300nm。
2.探索出在低压空气中电弧放电法制备多壁碳纳米管的工艺，通过深入细致地研究得出了碳管最佳制备条件。对阴极圆柱状沉积物进行详细地观察，根据观察结果给出了电弧放电条件下多壁碳纳米管可能的生长机理。通过对电弧放电设备改造，实现多壁碳纳米管的半连续化生产和连续化生产，并详细介绍了生产的操作流程。
3.以Fe做催化剂，FeS做促进剂，通过电弧放电法成功地在低压空气中制备出双壁碳纳米管，同时研究了制备双壁碳纳米管的最佳条件。由于空气易得，无需预抽真空，该方法简化了制备流程，有望实现低成本、大产量制备双壁碳纳米管。提纯后的碳纳米管纯度为90wt.%以上，为以后开展对双壁碳纳米管的研究工作打下了基础。最后，给出了Fe–FeS催化剂电弧放电法生长碳纳米管的可能生长机理。
4.对在空气气氛中制备的多壁碳纳米管和双壁碳纳米管分别进行场致发射测试。对于多壁碳纳米管，直接采用阴极沉积物薄片中间富含多壁碳纳米管的松软区域进行测试，发现空气中750oC下保持30min的热处理过程，能有效地提高多壁碳纳米管的场发射性能；对于双壁碳纳米管，开发了一种制备具有尖端结构的碳纳米管膜的方法，这种尖端结构的双壁碳纳米管膜呈现出非常优异的场发射性能。
5.采用磁控溅射法、衬底增强化学镀法和分子级混合工艺三种方式制备多壁碳纳米管/铜复合材料，对所制备的复合材料进行形貌、结构表征和薄膜电阻的测试，结果显示，在磁控溅射法制备的多壁碳纳米管/铜复合材料中，碳纳米管表面可以形成一层致密而均匀的铜层；以锌片为衬底，采用衬底增强化学镀法制备的多壁碳纳米管/铜复合材料中，碳纳米管表面沉积的铜纳米粒子呈现立方体状，并串连在一起；分子级混合工艺制备的经过氢气还原的多壁碳纳米管/铜复合粉体，碳纳米管多数都埋入或贯穿在铜纳米球体中；通过第一性原理对铜原子吸附在单壁碳纳米管的电学性能进行计算，根据结果提出了铜提供高浓度电子在碳纳米管高迁移率系统的电子结构内流动，形成导电性增强机制的导电模型；多壁碳纳米管/铜复合材料组成的非酶性电化学传感器对葡萄糖的检测具有非常好的灵敏性、选择性和稳定性。
Carbon nanotubes (CNTs) have potential applications in different fileds, includingnanoelectronic devices, composite materials, and sensors, etc., due to their uniquestructure and good physical and chemical properties. At present, the main industrialgrowth of CNTs is chemical vapor deposition (CVD) method. However, CVD CNTs havevery disordered structures and a high content of defects including vacancies, danglingbonds, edges and dislocations, as a result of the idiosyncrasy of CVD conditions at lowtemperature. These have seriously restricted their excellent performance. The othersynthesis methods are always high cost, time-consuming, and low yield, which can notsatisfy the practical application. Therefore, to explore the large scale and low costpreparation of high quality and low defect CNTs has very important practical significance.This dissertation is mainly focused on the large scale synthesis of multi-walled carbonnanotubes (MWCNTs) with high quality and low defect and their application. The mainresults are as follows:
1. A rapid high-temperature annealing technique has been developed, demonstrating agreat potential for defects reduction and structural enhancement of CVD MWCNTs. Highresolution TEM, Raman spectra, TGA and electrical resistivity measurement of nanotubepowders have been employed in order to evaluate the rapid high temperature annealingeffects. Moreover, a novel, simple, and effective method has been developed to cut theconventional long and entangled MWCNTs. The cutting process was carried out by theinteractive collision of CNTs with the silicon carbide particles adhered on the abrasivepapers. After cutting, the lengths of the most CNTs are200–300nm.
2. The development of preparing straight MWCNTs on a large scale is demonstratedusing direct current arc discharge in low pressure air. The process is time-saving,economical and non-hazardous. It is found the optimum conditions for the highest yield of MWCNTs. Base on the detailed investigation on the internal organization of cathodedeposit, the growth process of MWCNTs by arc discharge method in low pressure air isdepicted. The semi-continuous and continuous initial productions of MWCNTs areachieved by the modification of arc discharge equipment. And the production processesare introduced in detail.
3. Double-walled carbon nanotubes (DWCNTs) have been effectively synthesized byarc discharge in low pressure air using a mixture of Fe catalyst and FeS promoter.Compared with conventional arc methods, this method is easier to implement withoutusing expensive high purity gas sources. And it also simplifies the preparation processbecause of the absence of pre-vacuum. This method is expected to be low-cost, largeproduction preparation of DWCNTs. The optimum conditions for the preparation ofDWCNTs are investigated. DWCNT purification is employed by combining method usingwet selection in magnetic field, oxidation in air, treatment in hydrochloric acid andcentrifugation, which can effectively remove the impurities in samples, such as amorphouscarbon, metal catalyst particles and graphite particles, etc.. After purification, the purity ofDWCNTs is more than90wt.%, which is the foundation for the future to carry outresearch on DWCNTs. Finally, the possible growth mechanism of DWCNTs using Fe–FeS catalyst by arc discharge is given.
4. Field emission tests of MWCNTs and DWCNTs prepared in low pressure air by arcdischarge are carried out, respectively. For MWCNTs, the field emission performances ofMWCNTs in black core region of cathode deposits before and after burning at750oC for30min in air have been investigated detailedly. The results indicate that simple burningcan improve dramatically the field emission properties. For DWCNTs, a tip structuralDWCNT film has been successfully fabricated by a mixing process of electrophoresis,electroplating and electrocorrosion. The field emission properties of tip structuralnanotube film is significantly increased compared with DWCNT film fabricated byelectrophoresis. The mixing process is not complicated, does not require expensive equipments and facilities, and not subject to special conditions, which provide a simpleand effective way to improve the contact between CNTs and substrate. Based on the fieldemission results, tip structural DWCNT film is superior for field emission, which can beapplied as field emission flat panel displays and cold electron sources in display devices.
5. In order to prepare CNTs/Cu composite materials, radio frequency (RF) magnetronsputtering, substrate-enhanced electroless deposition (SEED) and molecular-level mixingare used. A composite material based on Cu nanoparticles with good crystallinitydeposited uniformly on the arc-prepared MWCNTs has been developed by RF magnetronsputtering. The CNTs/Cu composite prepared by SEED process shows that Cunanoparticles deposited on the surface of MWCNTs are cube shape, and are connectedtogether in series. The CNTs/Cu composite powders prepared by molecular-level mixingprocess show that nanotubes are implanted or through Cu nanosphere. The electronicstructure of Cu atom adsorbed on a single-walled carbon nanotube (SWCNT/Cu) isstudied by the First Principles calculations. Based on the experimental results andtheoretical calculations, we propose an electron conductive model of CNT/Cu composite,that is the high concentration of electrons provided by Cu flows in CNTs with the highmobility electronic structure, forming the conductivity enhancement mechanism. A sort ofnon-enzymatic electrochemical sensor is fabricated based on a composite of Cunanoparticles and arc-synthesized MWCNTs by using SEED method for detecting glucose.It exhibits excellent sensitivity, good specifity and high stability.
1.采用一种新颖的快速自加热方法高温退火处理CVD多壁碳纳米管，能够有效地提高多壁碳纳米管的有序结构，减少缺陷。介绍了一种简单、高效、可靠的剪切碳纳米管的方法，剪切后的碳纳米管主要集中在200–300nm。
2.探索出在低压空气中电弧放电法制备多壁碳纳米管的工艺，通过深入细致地研究得出了碳管最佳制备条件。对阴极圆柱状沉积物进行详细地观察，根据观察结果给出了电弧放电条件下多壁碳纳米管可能的生长机理。通过对电弧放电设备改造，实现多壁碳纳米管的半连续化生产和连续化生产，并详细介绍了生产的操作流程。
3.以Fe做催化剂，FeS做促进剂，通过电弧放电法成功地在低压空气中制备出双壁碳纳米管，同时研究了制备双壁碳纳米管的最佳条件。由于空气易得，无需预抽真空，该方法简化了制备流程，有望实现低成本、大产量制备双壁碳纳米管。提纯后的碳纳米管纯度为90wt.%以上，为以后开展对双壁碳纳米管的研究工作打下了基础。最后，给出了Fe–FeS催化剂电弧放电法生长碳纳米管的可能生长机理。
4.对在空气气氛中制备的多壁碳纳米管和双壁碳纳米管分别进行场致发射测试。对于多壁碳纳米管，直接采用阴极沉积物薄片中间富含多壁碳纳米管的松软区域进行测试，发现空气中750oC下保持30min的热处理过程，能有效地提高多壁碳纳米管的场发射性能；对于双壁碳纳米管，开发了一种制备具有尖端结构的碳纳米管膜的方法，这种尖端结构的双壁碳纳米管膜呈现出非常优异的场发射性能。
5.采用磁控溅射法、衬底增强化学镀法和分子级混合工艺三种方式制备多壁碳纳米管/铜复合材料，对所制备的复合材料进行形貌、结构表征和薄膜电阻的测试，结果显示，在磁控溅射法制备的多壁碳纳米管/铜复合材料中，碳纳米管表面可以形成一层致密而均匀的铜层；以锌片为衬底，采用衬底增强化学镀法制备的多壁碳纳米管/铜复合材料中，碳纳米管表面沉积的铜纳米粒子呈现立方体状，并串连在一起；分子级混合工艺制备的经过氢气还原的多壁碳纳米管/铜复合粉体，碳纳米管多数都埋入或贯穿在铜纳米球体中；通过第一性原理对铜原子吸附在单壁碳纳米管的电学性能进行计算，根据结果提出了铜提供高浓度电子在碳纳米管高迁移率系统的电子结构内流动，形成导电性增强机制的导电模型；多壁碳纳米管/铜复合材料组成的非酶性电化学传感器对葡萄糖的检测具有非常好的灵敏性、选择性和稳定性。
Carbon nanotubes (CNTs) have potential applications in different fileds, includingnanoelectronic devices, composite materials, and sensors, etc., due to their uniquestructure and good physical and chemical properties. At present, the main industrialgrowth of CNTs is chemical vapor deposition (CVD) method. However, CVD CNTs havevery disordered structures and a high content of defects including vacancies, danglingbonds, edges and dislocations, as a result of the idiosyncrasy of CVD conditions at lowtemperature. These have seriously restricted their excellent performance. The othersynthesis methods are always high cost, time-consuming, and low yield, which can notsatisfy the practical application. Therefore, to explore the large scale and low costpreparation of high quality and low defect CNTs has very important practical significance.This dissertation is mainly focused on the large scale synthesis of multi-walled carbonnanotubes (MWCNTs) with high quality and low defect and their application. The mainresults are as follows:
1. A rapid high-temperature annealing technique has been developed, demonstrating agreat potential for defects reduction and structural enhancement of CVD MWCNTs. Highresolution TEM, Raman spectra, TGA and electrical resistivity measurement of nanotubepowders have been employed in order to evaluate the rapid high temperature annealingeffects. Moreover, a novel, simple, and effective method has been developed to cut theconventional long and entangled MWCNTs. The cutting process was carried out by theinteractive collision of CNTs with the silicon carbide particles adhered on the abrasivepapers. After cutting, the lengths of the most CNTs are200–300nm.
2. The development of preparing straight MWCNTs on a large scale is demonstratedusing direct current arc discharge in low pressure air. The process is time-saving,economical and non-hazardous. It is found the optimum conditions for the highest yield of MWCNTs. Base on the detailed investigation on the internal organization of cathodedeposit, the growth process of MWCNTs by arc discharge method in low pressure air isdepicted. The semi-continuous and continuous initial productions of MWCNTs areachieved by the modification of arc discharge equipment. And the production processesare introduced in detail.
3. Double-walled carbon nanotubes (DWCNTs) have been effectively synthesized byarc discharge in low pressure air using a mixture of Fe catalyst and FeS promoter.Compared with conventional arc methods, this method is easier to implement withoutusing expensive high purity gas sources. And it also simplifies the preparation processbecause of the absence of pre-vacuum. This method is expected to be low-cost, largeproduction preparation of DWCNTs. The optimum conditions for the preparation ofDWCNTs are investigated. DWCNT purification is employed by combining method usingwet selection in magnetic field, oxidation in air, treatment in hydrochloric acid andcentrifugation, which can effectively remove the impurities in samples, such as amorphouscarbon, metal catalyst particles and graphite particles, etc.. After purification, the purity ofDWCNTs is more than90wt.%, which is the foundation for the future to carry outresearch on DWCNTs. Finally, the possible growth mechanism of DWCNTs using Fe–FeS catalyst by arc discharge is given.
4. Field emission tests of MWCNTs and DWCNTs prepared in low pressure air by arcdischarge are carried out, respectively. For MWCNTs, the field emission performances ofMWCNTs in black core region of cathode deposits before and after burning at750oC for30min in air have been investigated detailedly. The results indicate that simple burningcan improve dramatically the field emission properties. For DWCNTs, a tip structuralDWCNT film has been successfully fabricated by a mixing process of electrophoresis,electroplating and electrocorrosion. The field emission properties of tip structuralnanotube film is significantly increased compared with DWCNT film fabricated byelectrophoresis. The mixing process is not complicated, does not require expensive equipments and facilities, and not subject to special conditions, which provide a simpleand effective way to improve the contact between CNTs and substrate. Based on the fieldemission results, tip structural DWCNT film is superior for field emission, which can beapplied as field emission flat panel displays and cold electron sources in display devices.
5. In order to prepare CNTs/Cu composite materials, radio frequency (RF) magnetronsputtering, substrate-enhanced electroless deposition (SEED) and molecular-level mixingare used. A composite material based on Cu nanoparticles with good crystallinitydeposited uniformly on the arc-prepared MWCNTs has been developed by RF magnetronsputtering. The CNTs/Cu composite prepared by SEED process shows that Cunanoparticles deposited on the surface of MWCNTs are cube shape, and are connectedtogether in series. The CNTs/Cu composite powders prepared by molecular-level mixingprocess show that nanotubes are implanted or through Cu nanosphere. The electronicstructure of Cu atom adsorbed on a single-walled carbon nanotube (SWCNT/Cu) isstudied by the First Principles calculations. Based on the experimental results andtheoretical calculations, we propose an electron conductive model of CNT/Cu composite,that is the high concentration of electrons provided by Cu flows in CNTs with the highmobility electronic structure, forming the conductivity enhancement mechanism. A sort ofnon-enzymatic electrochemical sensor is fabricated based on a composite of Cunanoparticles and arc-synthesized MWCNTs by using SEED method for detecting glucose.It exhibits excellent sensitivity, good specifity and high stability.
引文
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