钛基钠米金刚石涂层场发射阴极工艺研究
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摘要
目前市场上对平板显示器的需求日益增多，而在各类平板显示器中，场致发射平板显示器兼有阴极射线管显示器和液晶显示器的优点，具有极大的发展潜力。
本文介绍了一种器件结构和制备工艺简单，易于实现大屏幕显示，且适于批量生产的新型场发射阴极，即在金属钛衬底上均匀涂覆纳米金刚石涂层，然后在高温下退火处理实现两者的牢固键合，并形成欧姆接触。
从理论上研究了制备金属基金刚石纳米涂层场发射阴极的可能性，并根据相关理论，提出一整套工艺设想。
重点探索了涂覆金刚石纳米涂层的方法、实现金刚石与金属钛的热粘接工艺以及氢等离子体处理的工艺参数，筛选出了在本实验系统中的最佳方法和工艺条件。
采用XRD、SEM、TEM、LRM和EDS等测试分析手段，对实验样品进行检测分析。分析结果表明，热处理后，样品表面确实生成了TiC，实现了金刚石纳米涂层与金属Ti的键合。自行设计组建了场发射性能测试系统，并用其测试了样品的场发射性能，表明实现热粘接后样品具有较好的场发射性能。
With both CRT's and LCD's virtue, FED has a bright future in all kinds of PDF.
In this thesis, a new type of field emission cathode was described, that is using simple technique to deposit commercial nano-diamond powder on Ti substrates, bonding diamond and Ti, and form Ohmic-contact by proper high temperature to form cathodes. This methods is adapt to large area and batch production.
Feasibility of preparation of this kind of cathode was investigated theoretically, and a series of technique was proposed.
The method of preparing the uniform coating, the techniques of thermal bonding and hydrogen plasma treatment was investigated experimentally. The optimum coating method and technological parameters was summarized.
The cathode sample was characterized by XRD, TEM, SEM, LRM and EDS methods. The result indicated that the surface of sample contain TiC, which verifying bonding was formed between diamond coating and Ti substrate. The field emitting property of samples were measured with testing system designed and constructed by ourselves. Cathode prepared by experiment indicated preferable field emission property.
本文介绍了一种器件结构和制备工艺简单，易于实现大屏幕显示，且适于批量生产的新型场发射阴极，即在金属钛衬底上均匀涂覆纳米金刚石涂层，然后在高温下退火处理实现两者的牢固键合，并形成欧姆接触。
从理论上研究了制备金属基金刚石纳米涂层场发射阴极的可能性，并根据相关理论，提出一整套工艺设想。
重点探索了涂覆金刚石纳米涂层的方法、实现金刚石与金属钛的热粘接工艺以及氢等离子体处理的工艺参数，筛选出了在本实验系统中的最佳方法和工艺条件。
采用XRD、SEM、TEM、LRM和EDS等测试分析手段，对实验样品进行检测分析。分析结果表明，热处理后，样品表面确实生成了TiC，实现了金刚石纳米涂层与金属Ti的键合。自行设计组建了场发射性能测试系统，并用其测试了样品的场发射性能，表明实现热粘接后样品具有较好的场发射性能。
With both CRT's and LCD's virtue, FED has a bright future in all kinds of PDF.
In this thesis, a new type of field emission cathode was described, that is using simple technique to deposit commercial nano-diamond powder on Ti substrates, bonding diamond and Ti, and form Ohmic-contact by proper high temperature to form cathodes. This methods is adapt to large area and batch production.
Feasibility of preparation of this kind of cathode was investigated theoretically, and a series of technique was proposed.
The method of preparing the uniform coating, the techniques of thermal bonding and hydrogen plasma treatment was investigated experimentally. The optimum coating method and technological parameters was summarized.
The cathode sample was characterized by XRD, TEM, SEM, LRM and EDS methods. The result indicated that the surface of sample contain TiC, which verifying bonding was formed between diamond coating and Ti substrate. The field emitting property of samples were measured with testing system designed and constructed by ourselves. Cathode prepared by experiment indicated preferable field emission property.
引文
[01]．应根裕等编著，平板显示技术，人民邮电出版社
[02]．金长春，场发射显示，液晶与显示，1996．11(1)：52～59
[03]．柯春和等，场发射平板显示器件，真空电子技术，1994．2：10～15
[04]．柯春和等，场发射平板显示器件的进展，真空电子技术，1997．17(2)：119～128
[05]．柯春和等，场发射显示技术，真空电子技术，1996．6：52～60
[06]．王保平等，场致发射显示屏及其产品设计的相关技术，电子器件，1997．20(3)：25～30
[07]．罗恩泽等，场发射显示屏的基本原理及结构设计，彩色显像管，1998．2：27～32
[08]．曾益彬，场致发射阴极的研究与进展，龙岩师专学报，2000．18(3)：23～26
[09]．孙永伟等，金刚石薄膜场致发射的研究，重庆邮电学院学报，2000．12(1)：38～40
[10]．张连俊等，场致电子发射技术分析，电子器件，2000．23(3)：210～212
[11]．林志贤等，场致发射材料的特性，福州大学学报(自然科学版)，2000．28(4)：22～25
[12]．陈光华等，宽带隙薄膜材料场电子发射研究的背景、现状和问题，物理，2000．29(15)：278～282
[13]．黄安庆等，金刚石薄膜场发射进展，物理，1997．26(7)：414～417
[14]．金长春，场发射平板显示
[15]．唐敦乙等，金刚石薄膜场致发射的研究，上海交通大学学报，2000．34(2)：212～214
[16]．孙永伟等，金刚石薄膜场发射显示器，光电子技术，1999．19(3)：161～165
[17]．单莺译，场发射显示，光电子技术，1997．17(4)：305～307
[18]．黄安庆等，金刚石薄膜场发射进展，物理，1997．26(7)：414～417
[19]．廖梅勇等，金刚石的场致发射，半导体技术，1999．24(1)：55～57
[20]．陈光华等，新型金刚石薄膜场电子发射的特性，北京工业大学学报，2000．26(3)：116～119
[21]. M.W. Geis,et al., Diamond emitters fabrication and theory, J.Vac. Sci.Technol.B 1996.14(3): 2060～2067
[22]. N.S.Xu,et al., Therotical study of the threshold field for field electron emission from amorphous diamond thin films,J.Vac. Sci.Technol.B.2001.19(3): 1059-1063
[23]. Z.sun,et al., Phase transformation of diamond films during electron field emission, Appl. Sur. Sci.2001 (173):282-289
[24]．王明智等，金刚石表面的Ti、Mo、W镀层机界面反应对抗氧化性能的影响，复合材料学报，1996．13(2)：48～52
[25]．王岚等，金刚石-钛界面的扩散，硅酸盐学报，1998．26(2)：270～274
[26].T.Tachibana, et al., Correlation of the electrical properties of metal contacts on diamond films with the chemical nature of the metal-diamond interface. Ⅱ.Titanium contacts: A carbide-forming metal, Physical Review B 1992-Ⅱ
45(20):11975～11981
[27]. J.Ristein, Electronic properties of diamond surfaces—blessing or curse for devices?, Diamond and Related Materials. 2000.9:1129～1137
[28]. Fitzgerald et al., surface morphology and electronic properties of CVD diamond,J.Vac. Sci. Technol.B, 2000. vol. 18(6):2714～2721
[29]. L.Diederich et al., Photoelectron emission from the negative electron affinity caesiated natural diamond(100)surface, Diamond and Related Materials, 1998.7:660～665
[30]. P.W. May et al., The effect of diamond surface termination species upon field emission properties, Diamond and Related Materials, 1998.7:671～676
[31]. Y. Gotoh et al., Negative-and Positive-Temperature Dependences of Electron Emission properties of Hydrogen-and Oxygen-Terminated Diamond Field emitters,IEEE.2001:297
[32]. Q.chen et al., Nano-sized diamond obtained from explosive detonation and its application, Materials Research Bulletin, 2000.35:1915～1919
[33]. I.Lin et al., Modificatin of emission properties of diamond films due to surface treatment process, Diamond and Related Materials, 2000.9:1574～1581
[34]. T. Asano et al., Field Emission from Plasma-Treated Diamond particles, IEEE,2001:283～286
[35]. T. Sugino et al., Characteristics of metal-polycrystalline diamond contact field emitters, Diamond and Related materials, 1998.7:667～681
[36]. V.V. Zhirnov et al., Anlysis of operation of diamond-based cold cathodes with different design parameters, IEEE.2001:279
[37]. W.B.Choi.et al., The effects of the interface and surface treatment on the electron emission from diamond coated field emitters, 9th International Vauum Microelectronics Conference,St. Petersburg 1996:228～292
[38]．马会中等，类金刚石薄膜冷阴极场发射研究进展，光电子．激光，1999．10(1)
[39]．茅东升等，高sp3键含量无氢非晶金刚石薄膜，中国科学(E)，1999．29(1)
[40]．茅东升等，界面过渡层对非晶金刚石薄膜电子场发射性能的影响，中国科学(E)，1999．29(6)
[41]．李运均等，脉冲激光沉积非晶碳-聚酰亚胺复合薄膜的场电子发射研究，中国激光 1997．24(10)
[42]. Kyung Ho Park et al., Stable and uniform electron emission from nanostructured carbon films; J.Vac. Sci.Technol.B19(3)2001
[43]．翟海潮等著，粘结与表面粘涂技术，化学工业出版社
[44]．邵乐喜等，纳米金刚石颗粒涂层的场电子发射，兰州大学学报，1996．35(1)
[45]．周江云等，金刚石粉末淀积层的场发射特性研究，发光学报，2000．21(4)
[46]．李俊峰等，金刚石薄膜阴极电子发射特性研究，真空科学与技术 1999．19(5)：389～391
[47]. D.He et al., Electron transport and electron field emission of nanodiamond synthesized by explosive detonation, Diamond and Related Materials, 2000.9:1600～1603
[48]．X射线衍射手册
[49]．钱苗根主编，材料表面技术及其应用手册，机械工业出版社
[50]．翟海潮等编著，实用胶粘剂配方手册，化学工业出版社
[51]．程时远等编著，粘剂，化学工业出版社
[52]．李子东编译，胶粘剂应用技术手册，上海科学技术文献出版社
[53]．陈根座等编著，胶粘剂应用手册，电子工业出版社
[54]. W. Zhu et al. Electron field emission from nanostructured diamond and carbon nanotubes, Solid-State Electronic 2001.45:921～928
[55]．王必本等，CVD金刚石膜的场发射机制，2000年亚太地区金刚石及相关材料会议论文集
[56]. K. Wu et al. Bistable characteristic and current jumps in field electron emission of nanocrystalline diamond films. J.Appl.Phys., 2001,Vol.90(9):4810～4814
[02]．金长春，场发射显示，液晶与显示，1996．11(1)：52～59
[03]．柯春和等，场发射平板显示器件，真空电子技术，1994．2：10～15
[04]．柯春和等，场发射平板显示器件的进展，真空电子技术，1997．17(2)：119～128
[05]．柯春和等，场发射显示技术，真空电子技术，1996．6：52～60
[06]．王保平等，场致发射显示屏及其产品设计的相关技术，电子器件，1997．20(3)：25～30
[07]．罗恩泽等，场发射显示屏的基本原理及结构设计，彩色显像管，1998．2：27～32
[08]．曾益彬，场致发射阴极的研究与进展，龙岩师专学报，2000．18(3)：23～26
[09]．孙永伟等，金刚石薄膜场致发射的研究，重庆邮电学院学报，2000．12(1)：38～40
[10]．张连俊等，场致电子发射技术分析，电子器件，2000．23(3)：210～212
[11]．林志贤等，场致发射材料的特性，福州大学学报(自然科学版)，2000．28(4)：22～25
[12]．陈光华等，宽带隙薄膜材料场电子发射研究的背景、现状和问题，物理，2000．29(15)：278～282
[13]．黄安庆等，金刚石薄膜场发射进展，物理，1997．26(7)：414～417
[14]．金长春，场发射平板显示
[15]．唐敦乙等，金刚石薄膜场致发射的研究，上海交通大学学报，2000．34(2)：212～214
[16]．孙永伟等，金刚石薄膜场发射显示器，光电子技术，1999．19(3)：161～165
[17]．单莺译，场发射显示，光电子技术，1997．17(4)：305～307
[18]．黄安庆等，金刚石薄膜场发射进展，物理，1997．26(7)：414～417
[19]．廖梅勇等，金刚石的场致发射，半导体技术，1999．24(1)：55～57
[20]．陈光华等，新型金刚石薄膜场电子发射的特性，北京工业大学学报，2000．26(3)：116～119
[21]. M.W. Geis,et al., Diamond emitters fabrication and theory, J.Vac. Sci.Technol.B 1996.14(3): 2060～2067
[22]. N.S.Xu,et al., Therotical study of the threshold field for field electron emission from amorphous diamond thin films,J.Vac. Sci.Technol.B.2001.19(3): 1059-1063
[23]. Z.sun,et al., Phase transformation of diamond films during electron field emission, Appl. Sur. Sci.2001 (173):282-289
[24]．王明智等，金刚石表面的Ti、Mo、W镀层机界面反应对抗氧化性能的影响，复合材料学报，1996．13(2)：48～52
[25]．王岚等，金刚石-钛界面的扩散，硅酸盐学报，1998．26(2)：270～274
[26].T.Tachibana, et al., Correlation of the electrical properties of metal contacts on diamond films with the chemical nature of the metal-diamond interface. Ⅱ.Titanium contacts: A carbide-forming metal, Physical Review B 1992-Ⅱ
45(20):11975～11981
[27]. J.Ristein, Electronic properties of diamond surfaces—blessing or curse for devices?, Diamond and Related Materials. 2000.9:1129～1137
[28]. Fitzgerald et al., surface morphology and electronic properties of CVD diamond,J.Vac. Sci. Technol.B, 2000. vol. 18(6):2714～2721
[29]. L.Diederich et al., Photoelectron emission from the negative electron affinity caesiated natural diamond(100)surface, Diamond and Related Materials, 1998.7:660～665
[30]. P.W. May et al., The effect of diamond surface termination species upon field emission properties, Diamond and Related Materials, 1998.7:671～676
[31]. Y. Gotoh et al., Negative-and Positive-Temperature Dependences of Electron Emission properties of Hydrogen-and Oxygen-Terminated Diamond Field emitters,IEEE.2001:297
[32]. Q.chen et al., Nano-sized diamond obtained from explosive detonation and its application, Materials Research Bulletin, 2000.35:1915～1919
[33]. I.Lin et al., Modificatin of emission properties of diamond films due to surface treatment process, Diamond and Related Materials, 2000.9:1574～1581
[34]. T. Asano et al., Field Emission from Plasma-Treated Diamond particles, IEEE,2001:283～286
[35]. T. Sugino et al., Characteristics of metal-polycrystalline diamond contact field emitters, Diamond and Related materials, 1998.7:667～681
[36]. V.V. Zhirnov et al., Anlysis of operation of diamond-based cold cathodes with different design parameters, IEEE.2001:279
[37]. W.B.Choi.et al., The effects of the interface and surface treatment on the electron emission from diamond coated field emitters, 9th International Vauum Microelectronics Conference,St. Petersburg 1996:228～292
[38]．马会中等，类金刚石薄膜冷阴极场发射研究进展，光电子．激光，1999．10(1)
[39]．茅东升等，高sp3键含量无氢非晶金刚石薄膜，中国科学(E)，1999．29(1)
[40]．茅东升等，界面过渡层对非晶金刚石薄膜电子场发射性能的影响，中国科学(E)，1999．29(6)
[41]．李运均等，脉冲激光沉积非晶碳-聚酰亚胺复合薄膜的场电子发射研究，中国激光 1997．24(10)
[42]. Kyung Ho Park et al., Stable and uniform electron emission from nanostructured carbon films; J.Vac. Sci.Technol.B19(3)2001
[43]．翟海潮等著，粘结与表面粘涂技术，化学工业出版社
[44]．邵乐喜等，纳米金刚石颗粒涂层的场电子发射，兰州大学学报，1996．35(1)
[45]．周江云等，金刚石粉末淀积层的场发射特性研究，发光学报，2000．21(4)
[46]．李俊峰等，金刚石薄膜阴极电子发射特性研究，真空科学与技术 1999．19(5)：389～391
[47]. D.He et al., Electron transport and electron field emission of nanodiamond synthesized by explosive detonation, Diamond and Related Materials, 2000.9:1600～1603
[48]．X射线衍射手册
[49]．钱苗根主编，材料表面技术及其应用手册，机械工业出版社
[50]．翟海潮等编著，实用胶粘剂配方手册，化学工业出版社
[51]．程时远等编著，粘剂，化学工业出版社
[52]．李子东编译，胶粘剂应用技术手册，上海科学技术文献出版社
[53]．陈根座等编著，胶粘剂应用手册，电子工业出版社
[54]. W. Zhu et al. Electron field emission from nanostructured diamond and carbon nanotubes, Solid-State Electronic 2001.45:921～928
[55]．王必本等，CVD金刚石膜的场发射机制，2000年亚太地区金刚石及相关材料会议论文集
[56]. K. Wu et al. Bistable characteristic and current jumps in field electron emission of nanocrystalline diamond films. J.Appl.Phys., 2001,Vol.90(9):4810～4814