碳纳米管薄膜阴极的制备与场发射性能研究
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摘要
碳纳米管具有优异的电学、力学和热学性能,在场发射平板显示领域显示出诱人的应用前景。但是,碳纳米管在发射点密度、发射稳定性和均匀性等方面的性能都不够理想,碳纳米管场发射性能的改善是其走向产业化的重要一步。本论文以改善碳纳米管场发射性能为研究目的,从碳纳米管阴极制备工艺的改进与优化、阴极薄膜的后处理等方面开展了一系列工作,得出了一些有意义的研究成果。
利用纳米银的低温熔接性和良好导电性,首次以纳米银作为导电材料和粘结剂,在低的烧结温度(250oC)下,利用涂敷法制成了表面平整、导电性和场发射性能良好的碳纳米管冷阴极。当混合浆料中碳纳米管与纳米银的质量比率为1:2时,碳纳米管阴极具有最好的场发射性能;过高和过低的纳米银掺入量均会使场发射性能变差。进一步优化了碳纳米管/纳米银阴极膜的制备工艺,采用两步涂敷法,制得了双层结构的碳纳米管/纳米银阴极膜,明显增强了碳纳米管与基底的附着力,提高了碳纳米管的场发射性能。
采用电泳法沉积碳纳米管薄膜,首次系统研究了各种电泳工艺条件对沉积的碳纳米管薄膜场发射性能的影响,获得了利用电泳法沉积碳纳米管薄膜的较优化的工艺条件和工艺细节;研究了各种测试参数对碳纳米管场发射的影响,随测试时阴阳极间距的增加和系统真空度的提高,碳纳米管薄膜的开启电场和阈值电场增大,但发射稳定性明显改善。分析了碳纳米管场发射F-N曲线的非线性现象。
从降低表面功函数和增强碳纳米管与基底之间附着力的角度改善电泳沉积的碳纳米管薄膜的场发射性能。通过在碳纳米管薄膜表面形成低功函数的Ti碳化物,降低了碳纳米管发射体的表面功函数,增强了碳纳米管薄膜的场发射性能。通过在基底表面镀覆Ti膜,退火后碳纳米管和基底之间形成导电性Ti碳化物,增加了碳纳米管与基底之间的附着力,消除了碳纳米管与基底之间的界面势垒,使碳纳米管场发射的开启电场和阈值电场明显降低。
系统研究了Ar微波等离子体处理对电泳沉积和涂敷制备的碳纳米管微结构和场发射性能的影响。由于等离子体处理造成了利于场发射的各种微观几何结构的形成,降低了电子发射的表面势垒,提高了碳纳米管的场增强因子,从而改善了碳纳米管薄膜场发射的I-V性能,而等离子体处理后碳纳米管薄膜场发射电流稳定性和均匀性的提高则归因于等离子体处理后碳纳米管电子发射位的增加以及发射位位置在场强方向上的一致化。
Carbon nanotubes (CNTs) have superior electronic and mechanical and thermodynamic properties which make them attractive in different application fields, especially in the field of flat panel display. However, up to date, field emission properties of CNTs, such as the number density of electron emission sites, the stability and uniformity of field emission current and so on, are not satisfied for its application as cold cathode electron source. It is crucial to improve the field emission properties of CNTs for their commercial applications. In this work, a series of studies were proceeded round the improvement and optimization for the fabrication processes of CNTs cathodes film and the post-treatment of the as-prepared CNTs film with the purpose of improving the field emission properties, and some useful conclusions were obtained.
Based on the properties of low melting point and high conductivity, a new preparation process for carbon nanotubes(CNTs) cold cathode was studies in the first time through the replacement of traditional organic binder or Ag paste with Ag nano-particles. A flat CNTs films with good field emission performance was obtained after sintered 30 min under 250oC. The measurements reveal that the field emission properties are the best when the mass ratio of CNTs and Ag nano-particles is 1:2. Too many and too few Ag nano-particles in mixed paste all result in poor field emission properties. The fabrication process for CNTs/Ag nano-particles cathode was optimized by using a two-step coating method, The two-layer structure CNTs cathode obtained by using the two-step coating method showed improved field emission properties, which can due to the improved adhesion of CNTs to substrate.
CNTs film was fabricated using electrophoresis deposition technique. The effects of various process conditions and the measurement parameters on the field emission properties of CNTs were investigated comprehensively in the first time, and the relative optimized electrophoresis process conditions and details were obtained. With the increasing of the interelectrode distance and the decreasing of the residual gas pressure in vacuum chamber, the as-prepared CNTs film exhibited improved emission current stability, while turn on electrical field and threshold electrical field became high. The probably reason causing the non-linearity phenomenon on the Fowler-Nordheim (F-N) plots was also analyzed.
In order to improve the field emission properties of electrophoresis deposition CNTs film using the method of decreasing the work function of the emitterΦ, a thin Ti film was coated on the surface of CNTs cathode film. Titanium carbide with lowΦformed after annealing in vacuum chamber decreased the work functionΦof CNTs emitters, which caused the improvement of field emission properties. When the Ti film was coated on the substrate, conductive titanium carbide was also formed between CNTs and substrate after annealing. The field emission properties were improved by the existence of conductive titanium carbide which resulted in the enhancement of adhesion of CNTs on the substrate and the elimination of the interface potential barrier between CNTs and the substrate.
The effects of Ar microwave plasma treatment on the microstructure and field emission properties of coated CNTs/Ag nano-particles film and electrophoresis deposition CNTs film were studied systematically. It is found that the microstructure was changed and the field emission properties were improved obviously by the plasma treatment. We attributed the improved field emission I-V property to the increase ofβand decrease of electron emission potential barrier resulted by the changed microstructure. Meanwhile, plasma treatment removed a portion of protruding CNTs emitters on the film surface, which would allow a greater number of emitters to be active with compensation for a higher electrical field application, and raised the number density of electron emission sites, which lead an improvement in emission stability and uniformity.
利用纳米银的低温熔接性和良好导电性,首次以纳米银作为导电材料和粘结剂,在低的烧结温度(250oC)下,利用涂敷法制成了表面平整、导电性和场发射性能良好的碳纳米管冷阴极。当混合浆料中碳纳米管与纳米银的质量比率为1:2时,碳纳米管阴极具有最好的场发射性能;过高和过低的纳米银掺入量均会使场发射性能变差。进一步优化了碳纳米管/纳米银阴极膜的制备工艺,采用两步涂敷法,制得了双层结构的碳纳米管/纳米银阴极膜,明显增强了碳纳米管与基底的附着力,提高了碳纳米管的场发射性能。
采用电泳法沉积碳纳米管薄膜,首次系统研究了各种电泳工艺条件对沉积的碳纳米管薄膜场发射性能的影响,获得了利用电泳法沉积碳纳米管薄膜的较优化的工艺条件和工艺细节;研究了各种测试参数对碳纳米管场发射的影响,随测试时阴阳极间距的增加和系统真空度的提高,碳纳米管薄膜的开启电场和阈值电场增大,但发射稳定性明显改善。分析了碳纳米管场发射F-N曲线的非线性现象。
从降低表面功函数和增强碳纳米管与基底之间附着力的角度改善电泳沉积的碳纳米管薄膜的场发射性能。通过在碳纳米管薄膜表面形成低功函数的Ti碳化物,降低了碳纳米管发射体的表面功函数,增强了碳纳米管薄膜的场发射性能。通过在基底表面镀覆Ti膜,退火后碳纳米管和基底之间形成导电性Ti碳化物,增加了碳纳米管与基底之间的附着力,消除了碳纳米管与基底之间的界面势垒,使碳纳米管场发射的开启电场和阈值电场明显降低。
系统研究了Ar微波等离子体处理对电泳沉积和涂敷制备的碳纳米管微结构和场发射性能的影响。由于等离子体处理造成了利于场发射的各种微观几何结构的形成,降低了电子发射的表面势垒,提高了碳纳米管的场增强因子,从而改善了碳纳米管薄膜场发射的I-V性能,而等离子体处理后碳纳米管薄膜场发射电流稳定性和均匀性的提高则归因于等离子体处理后碳纳米管电子发射位的增加以及发射位位置在场强方向上的一致化。
Carbon nanotubes (CNTs) have superior electronic and mechanical and thermodynamic properties which make them attractive in different application fields, especially in the field of flat panel display. However, up to date, field emission properties of CNTs, such as the number density of electron emission sites, the stability and uniformity of field emission current and so on, are not satisfied for its application as cold cathode electron source. It is crucial to improve the field emission properties of CNTs for their commercial applications. In this work, a series of studies were proceeded round the improvement and optimization for the fabrication processes of CNTs cathodes film and the post-treatment of the as-prepared CNTs film with the purpose of improving the field emission properties, and some useful conclusions were obtained.
Based on the properties of low melting point and high conductivity, a new preparation process for carbon nanotubes(CNTs) cold cathode was studies in the first time through the replacement of traditional organic binder or Ag paste with Ag nano-particles. A flat CNTs films with good field emission performance was obtained after sintered 30 min under 250oC. The measurements reveal that the field emission properties are the best when the mass ratio of CNTs and Ag nano-particles is 1:2. Too many and too few Ag nano-particles in mixed paste all result in poor field emission properties. The fabrication process for CNTs/Ag nano-particles cathode was optimized by using a two-step coating method, The two-layer structure CNTs cathode obtained by using the two-step coating method showed improved field emission properties, which can due to the improved adhesion of CNTs to substrate.
CNTs film was fabricated using electrophoresis deposition technique. The effects of various process conditions and the measurement parameters on the field emission properties of CNTs were investigated comprehensively in the first time, and the relative optimized electrophoresis process conditions and details were obtained. With the increasing of the interelectrode distance and the decreasing of the residual gas pressure in vacuum chamber, the as-prepared CNTs film exhibited improved emission current stability, while turn on electrical field and threshold electrical field became high. The probably reason causing the non-linearity phenomenon on the Fowler-Nordheim (F-N) plots was also analyzed.
In order to improve the field emission properties of electrophoresis deposition CNTs film using the method of decreasing the work function of the emitterΦ, a thin Ti film was coated on the surface of CNTs cathode film. Titanium carbide with lowΦformed after annealing in vacuum chamber decreased the work functionΦof CNTs emitters, which caused the improvement of field emission properties. When the Ti film was coated on the substrate, conductive titanium carbide was also formed between CNTs and substrate after annealing. The field emission properties were improved by the existence of conductive titanium carbide which resulted in the enhancement of adhesion of CNTs on the substrate and the elimination of the interface potential barrier between CNTs and the substrate.
The effects of Ar microwave plasma treatment on the microstructure and field emission properties of coated CNTs/Ag nano-particles film and electrophoresis deposition CNTs film were studied systematically. It is found that the microstructure was changed and the field emission properties were improved obviously by the plasma treatment. We attributed the improved field emission I-V property to the increase ofβand decrease of electron emission potential barrier resulted by the changed microstructure. Meanwhile, plasma treatment removed a portion of protruding CNTs emitters on the film surface, which would allow a greater number of emitters to be active with compensation for a higher electrical field application, and raised the number density of electron emission sites, which lead an improvement in emission stability and uniformity.
引文
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