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碳纳米管场发射荧光管的制备及性能研究
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摘要
场发射光源具有低功耗、高亮度、长寿命、无污染等优点,近年来成为人们研究的热点。本文围绕碳纳米管场发射荧光管的实用化研究,针对其阳极荧光屏的制作,开展了阳极ITO透明导电层的研制、荧光粉层的涂敷工艺研究及荧光管的组装与测试三部分工作。
     首先,本文重点研究了ITO薄膜的溶胶—凝胶制备工艺。以硝酸铟、氯化锡、乙酰丙酮为原料配制溶胶,用提拉法在普通玻璃基底与玻璃管内壁上拉制湿膜,最后进行烧结热处理制备ITO薄膜。研究了铟离子浓度、掺锡摩尔比、热处理温度、热处理时间、镀膜次数等相关制备工艺参数对ITO薄膜结构、形貌及光电性能的影响,结论如下:
     (1)XRD分析结果表明Sn元素被有效的掺进了氧化铟晶格中,ITO薄膜具有立方铁锰矿结构,并呈[111]方向择优生长。
     (2)SEM分析结果表明ITO薄膜表面呈纳米粒子堆积而成的多孔结构。
     (3)ITO薄膜的方阻随溶胶中In 3+浓度的增加而降低,当In 3+浓度增加到一定值后,薄膜表面均匀性降低,薄膜方阻变化较小,在In3+浓度为0.2 mol/L时,薄膜的导电性与均匀性最好。
     (4)ITO薄膜的方阻随掺锡比的增加而降低,掺锡比大于5%后薄膜方阻变化缓慢,在掺锡比为15%时方阻最小;ITO薄膜的可见光平均透过率随掺锡比的增大而增大。
     (5)ITO薄膜的方阻随热处理温度、热处理时间及膜厚的增加而降低,分别在450℃及8 h时薄膜的方阻最小;ITO薄膜的可见光平均透过率随热处理温度的增加而增大,随膜厚的增加而减小。
     (6)采用最佳工艺参数制备了具有良好光电性能的场发射荧光管阳极ITO导电层,其中ITO薄膜的方阻为360Ω/□,可见光平均透过率约为82%。
     其次,采用电泳法涂覆荧光粉层,研究了相关制备工艺参数(包括荧光粉浓度、电解质浓度、电泳电压、电泳时间)对沉积荧光粉层厚度与表面形貌的影响,确定了制备荧光粉层的最佳工艺参数为:荧光粉浓度10 g/L、电解质浓度0.128 g/L,电泳电压100 V,电泳时间2 min,获得了表面均匀、厚度理想的阳极荧光层。
     最后,组装碳纳米管场发射荧光管,并在真空环境下进行动态点亮测试。结果表明,碳纳米管场发射荧光管可以瞬间点亮、连续调光,当阳极电压为5 kV时,发光亮度为3519 cd /m2。
Field emission light source has drawn wide attention for its low power consumption, high brightness, long working-life and non-pollution. This paper focused on the practical research of carbon nanotube field emission fluorescent devices and the fabrication of anode fluorescent screen, carrying out the fabrication of ITO film anode, the coating of phosphor layer, as well as the assembling and testing of fluorescent tube.
     Firstly, ITO conductive anode films were fabricated on glass tube substrates by sol-gel process. The sol was prepared using indium nitrate, stannic chloride and acetylacetone. Then, the wet-films were prepared on glass substrates by dip-coating method. In the end, the ITO films were obtained after sintering process. The effect of various process parameters, including In3+ concentration, Sn-doped proportion, sintering temperature and time, as well as layer number of the film, on the structure, surface morphology and opt-electric properties of ITO films were studied and discussed. Certain conclusions were obtained as follow:
     (1) XRD results suggested that Sn was effectively doped into the lattice of indium oxide, and the ITO film has the Polyerystalline eubicbixbyitel In2O3 structure.
     (2) SEM results indicated that the surface of ITO films presented a porous structure accumulated by nano-particles.
     (3) The sheet resistance of ITO films decreased as the increase of In3+concentration in the sol. When In3+ concentration increased to a certain level, the uniformity of the thin film reduced, while the sheet resistance changed slightly. When In3+ concentration was 0.2 mol/L, the sheet resistance and the uniformity of the film reached to the best level.
     (4) The sheet resistance of ITO films decreased as the increase of the Sn-doped proportion. The sheet resistance changed slowly when Sn-doped proportion was higher than 5%, and It achieved the minimum when Sn doping ratio was 15%. The average visible transmittance of ITO films increased when the Sn-doped proportion increased.
     (5) The sheet resistance of ITO films decreased as the increase of sintering temperature and time, as well as film thickness. When the sample was sintering at 450℃for 8h, its sheet resistance reached the minimum value. The average visible transmittance of ITO films increased with the augment of sintering temperature and decreased with the increase of film thickness.
     (6) An anode ITO conductive layer of field emission fluorescent tube with excellent opt-electric performances was obtained in the end. The sheet resistance of the ITO film prepared by the same processing condition was 360Ω/□, and the average visible transmittance was about 82%.
     In addition, phosphor layers were fabricated by electrophoretic deposition. The effect of various process parameters, including phosphor concentration, electrolyte concentration, electrophoretic voltage and electrophoretic time, on the thickness and surface morphology of phosphor layers were analyzed. The best process parameters were obtained: the phosphor concentration was 10 g/L, the electrolyte concentration was 0.128 g/L, electrophoretic voltage was 150 V while the electrophoretic time was 2 min. An anode fluorescent tube with homogeneous surface and ideal thickness was fabricated at last.
     In the end, the carbon nanotube field emission fluorescent tube was assembled, lightened and tested in vacuum atmosphere. The results showed that carbon nanotube field emission fluorescent tube could be lightened instantly, and the light could be continuously modulated as well. When the anode voltage was 5kV, the brightness was 3519 cd/m2.
引文
[1]周太明.光源原理与设计.上海:复旦大学出版社, 2009,409~411
    [2] Lee N S, Chung D S, Han I T. Application of carbon nanotubes to field emission display Diamond and Related Materials, 2001, 10(2): 265-270
    [3] Kwo J L, Yokoyama M, Wang W C. Characteristics of flat panel display using carbon nanotubes as electron emitters. Diam Relat Mater, 2000, 9(3-6): 1270-1274.
    [4] Choi Y S, Kang J H, Park Y J, et al. An under-gate triode structure field emission display with carbon nanotube emitters. Diam Relat Mater, 2001, 10(9-10): 1705-1708.
    [5] Wang Q H, Yan M, Chang R P H. Flat panel display prototype using gated carbon nanotube field emitters. Appl Phys Lett, 2001, 78(9): 1294-1296.
    [6] Chubun N, Lazarev N, Sheshin E. Vacuum fluorescent light source with carbon fibres field emission cathode. Proceedings of the IEEE International Vacuum Micro-electronics Conference, 1995, p516-520.
    [7] E Czerwosz, S Waszuk, M Sucha, et al. Lighting sources with a cold cathode electrontube. Technical science 2008, 56(2): 117-123
    [8] Woo-Sung Cho, Hyeon-Jae Lee, Yang-Doo Lee, et al. Carbon Nanotube-Based Triode Field Emission Lamps Using Metal Meshes With Spacers. Electron device letters, 2007, 28(5): 386-388
    [9] M Yu Leshukov, A S Baturin, N N Chadaev, et al. Characterizations of light sources with carbon fiber cathodes. Applied Surface Science, 2003, 215: 60–264.
    [10] Leychenko A S, Leshukov M Yu, Chadaev N N, et al. Effective lamp for LCD backlightning with the field emission cathode. Source: IVNC and IFES 2006 - Technical Digest - l9th International Vacuum Nanoelectronics Conference and 50th International Field Emission Symposium, 2006: 383-384.
    [11] Psuja P, Strek W, Hreniak D, et al. Fabrication of a low-voltage light emitting device based on carbon nanotubes and rare-earth doped nanocrystals. Source: Proceedings of 2005 International Students and Young Scientists Workshop - Photonics and Microsystems, 2005: 65-67
    [12] Leshukov, M Yu; Chadaev, N N; Sheshin, E P. Field emission light source with carbon fibers bundle cathode. Source: Technical Digest of the 18th International Vacuum Nanoelectronics Conference, 2005: 340-341.
    [13] M Yu Leshukov, E P Sheshin. New design of electron gun for field emission light sources with carbon fibers cathode. Hydrogen materials science and chemistry of carbon nanomaterials, 2007: 255-258.
    [14] Psuja P, Cichy B, Górecka-Drzazga A,et al. Green/white light sources utilizing nanocrystalline YAG phosphores and MWNT field-emission cathodes. Source: IVNC and IFES 2006-Technical Digest-l9th International Vacuum Nanoelectronics Conference and 50th International Field Emission Symposium, 2006: 171-172.
    [15] Bonard J M; Stockli T; Noury O; et al. Field emission from cylindrical carbon nanotube cathodes: Possibilities for luminescent tubes. Applied Physics Letters, 2001, 78(18): 27-75.
    [16] Mirko Croci1, Imad Arfaoui, Thomas Sto¨ckli, et al. A fully sealed luminescent tube based on carbon nanotube field emission. Microelectronics Journal, 2004, 35: 329-336.
    [17] Yang Wei, Lin Xiao, Feng Zhu,et al. Cold linear cathodes with carbon nanotube emitters and their application in luminescent tubes. Nanotechnology, 2007, 18.
    [18] Wang, Hong-Xing, Harazono, Hideki,et al. Fabrication of high brightness flat field emission lamp with 6kV anode voltage for local dimming LCD BLU. Source: Digest of Technical Papers - SID International Symposium, 2008, 39(1): 74-76.
    [19] Choi, Young Chul; Lee, Ji Won; Lee, Su Kyung;et al. The high contrast ratio and fast response time of a liquid crystal display lit by a carbon nanotube field emission backlight unit. Nanotechnology, 2008, 19: 235-306
    [20] A G Rinzler, J H Hafner, P Nikolaev, et al. Unraveling nanotubes: field emission from an atomic wire. science, 1995, 269(5230): 1550-1553
    [21] Liu, G Y; Xia, S H; Lu, Y J;et al. Initial work of whole glass flat panel type vacuum fluorescent light source. Proceedings of the IEEE International Vacuum Microelectronics Conference, 2001,187-188.
    [22] Zhang, Yu; Deng, S Z; Chen, Jun; et al. A high brightness lighting element using carbon nanotube cathode.Source: IVNC and IFES 2006-Technical Digest-l9th International Vacuum Nanoelectronics Conference and 50th International Field Emission Symposium, 2006: 481-482.
    [23] Chen, Jun; Zhou, X; Deng, S Z; et al. The application of carbon nanotubes in high-efficiency low power consumption field-emission luminescent tube Ultr- amicroscopy. 2003, 95: 153-156.
    [24] Huang, J X; Chen, Jun; Deng, S Z; et al. A prototype cylindrical fluorescent lamp based on carbon nanotube field emission. Technical Digest of the 17th International Vacuum Nanoelectronics Conference, 2004: 50-51.
    [25] Iijima S. Helical microtubules of graphitic carbon. Nature, 1991, Vol. 354, p56.
    [26]Huang J X, Chen Jun, Deng S Z,et al. Optimization of carbon-nanotube cathode for a fluorescent lamp. Source: Technical Digest of the 18th International Vacuum Nanoelectronics Conference, 2005: 284-285.
    [27] Lai H J, Lin M C C,Yang M H. Synthesis of carbon nanotubes using polycyclic aromatic hydrocarbon as carbon sources in an arc discharge. Mater Sci Eng C, 2001, 16(1-2): 23-26.
    [28] Dai H. Carbon nanotubes: opportunities and challenges. Surf Sci, 2002, 500(1-3): 218-241.
    [29] Sen R. Carbon nanotubes by the metallocene route. Chem Phys lett, 1997, 267(3-4): 276-280.
    [30] Wang Q H, Setlur A A, Lauerhaas J M, et al. A nanotube based field emission flat panel display. Appl phys lett, 1998, 72(22): 2912-2913
    [31] Jung J E, Jin Y W, Choe J H, et al. Fabrication of triode-type field emission displays with high density carbon nanotube emitter arrays. Physica B, 2002, 323(1-4): 71-77.
    [32]姜辛,孙超,洪瑞江等.透明导电氧化物薄膜.高等教育出版社.2008, 8-9.
    [33] Ovadyahu Z, Ovryn B, kraner H W. Microstructure and elctro-optical properties of evaporated indium-oxide films. Electrochem, 1983, 130: 917-921.
    [34] SzOrenyi T, Lande L D, Bertoti I, et al. Excimer Laser Processing Of Indium tin oxide films:an potical investigation. J. Appl. Phys., 1995, 78: 6211-6219.
    [35] Smith J F, Aronson A J, Chen D, et al. Reactive magnetron deposition of transparent conductive films.Thin Solid Films, 1980, 72: 469-474.
    [36] Kawada A. Indium-tin oxide deposition by dc reactive sputtering on a low softening point material. Thin Solid Films, 1990, 191: 297-303.
    [37]Harding G L, Window B. DC magnetron reactively sputtered indium-tin-oxide film produced using argon oxygen hydrogen mixtures. Solar Energy Mater.1990, 20: 367-379.
    [38] Ryabova L A, Salun V S, Sorbinov I A.Transparent conductive films of In2O3: Sn prepared by the pyrolysis method.Thin Solid Films, 1982, 92: 327-332.
    [39] Maruyama T, Fukui K. Indium tin oxide thin films prepared by chemical vapor deposition. Thin Solid Films, 1991, 203: 297-301.
    [40] Furusaki,Tsuyoshi; Takahashi, Junichi; Kodaira, Kohei. Preparation of ITO thin films by sol-gel method. Journal of the Ceramic Society of Japan. International ed., 1994, 102(2): 202-207.
    [41]Djaoued Y. Sol-gel-prepared ITO film for electrochromic systems. Thin Solid Film, 1997, 293: 108.
    [42] Kim, Seon-Soon; Choi, Se-Young; Park, Chan-Gyung; et al. Transparent conductive ITO thinfilms through the sol-gel process using metal salts .Thin Solid Films, 1999, 347(1-2): 155-160.
    [43] Daoudi K. Tin-doped indium Oxide thin film deposited by sol-gel dip coating technique. Material Science and Engineering, 2002, 21: 313.
    [44] Stoica, T F; Teodorescu, V S; Blanchin, M G; et al. Internal structure of the nanosized sol-gel ITO thin films. Proceedings of the International Semiconductor Conference, 2001, 1: 63-66.
    [45] Stoica, T F; Teodorescu, V S; Blanchin, M G; et al. Morphology, structure and optical properties of sol-gel ITO thin films. Materials Science and Engineering B: Solid-State Materials for Advanced Technology, 2003, 101(1-3): 222-226.
    [46] Jiao, Zheng; Wu, Minghong; Gu, Jianzhong; et al. The gas sensing characteristics of ITO thin film prepared by sol-gel method. Sensors and Actuators, B: Chemical, 2003, 94(2): 216-221.
    [47] Hadj, Tahar, Radhouane Bel; Ban, Takayuki; Ohya, Yutaka; et al. Optical, structural, and electrical properties of indium oxide thin films prepared by the sol-gel method. Journal of Applied Physics, 1997, 82(2): 865.
    [48]黄剑峰.溶胶-凝胶原理与技术.化学工业出版社,2005,41
    [49] Ramanan, Sutapa Roy. Dip coated ITO thin-films through sol-gel process using metal salts. Thin Solid Films, 2001, 389(1-2): 207-212.
    [50]辛科.铟锡氧化物薄膜的制备工艺与性能研究[硕士论文].兰州大学, 2008.
    [51] Alam, M J;Cameron, D C. Characterization of transparent conductive ITO thin films deposited on titanium dioxide film by a sol-gel process. Surface and Coatings Technology, 2001, 142-144: 776-780.
    [52]刘家祥,甘勇,朴圣洁.胶体法制备透明导电ITO薄膜.稀有金属材料与工程, 2005,34(7),1169-1172
    [53]李芝华,任冬燕.溶胶凝胶法制备ITO透明导电薄膜的工艺研究.材料科学与工艺, 2006,14(2),174-177
    [54]陈健,张江,高善民.溶胶凝胶旋涂法制备ITO薄膜.纳米材料与结构,2007(3),132-135
    [55]高美珍,辛科,张锋等.热处理时间对溶胶-凝胶法制备ITO薄膜结构、形貌和性质的影响.材料导报, 2009,23(1),87-90
    [56]李晶. ITO透明导电薄膜的溶胶-凝胶法制备及工艺研究[硕士论文].中南大学, 2004
    [57] Burstein E. Anomalous optical absorption limit in InSb. Phys. Rev., 1954, 93: 632-633
    [58]李炜.场发射平板显示器阳极荧光材料及器件的研究[博士学位论文].中国科学院上海冶金研究所,2000
    [59]吴长沪.电泳法制备荧光屏.真空电子技术,1999(2): 19

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