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論文中文名稱:奈米α-Al2O3/Ni核殼結構複合粉體之製備 [以論文名稱查詢館藏系統]
論文英文名稱:Synthesis of Nano-Sized α-Al2O3/Ni Core-Shell Composite Powders [以論文名稱查詢館藏系統]
院校名稱:臺北科技大學
學院名稱:工程學院
系所名稱:材料及資源工程系所
中文姓名:諶昱涵
英文姓名:Yu-Hen Chenn
研究生學號:92338009
學位類別:碩士
語文別:中文
口試日期:2005-07-25
論文頁數:80
指導教授中文名:王錫福
口試委員中文名:徐永富;顏富士;韋文誠
中文關鍵詞:α-Al2O3觸媒核-殼結構化學還原
英文關鍵詞:α-Al2O3 catalystcore-shell structurechemical reduction
論文中文摘要:本研究之目的在於開發奈米α-Al2O3粉體觸媒,吾人在奈米α-Al2O3粉體表面披覆上金屬,使其作為高溫觸媒載體,作者選擇Ni為金屬披覆層,使其與α-Al2O3形成核-殼結構之複合粉體。實驗方面採用化學還原法,利用聯胺(N2H4)作為還原劑,將金屬鹽前驅物NiSO4.6H2O、Ni(AC)2.6H2O、NiCl2.4H2O中的金屬Ni離子還原,並在α-Al2O3上形成金屬Ni披覆層。實驗分兩階段,先調整濃度、溫度、 pH值及反應時間等參數,另外輔助生長抑制劑於反應中,獲得我們要的奈米鎳粒子,然後進行各項物性及化性分析,包括XRD、SEM、TEM、Zeta Potential等,獲得理想的製程條件後,將其運用於披覆實驗中,最後輔助PSS及錯離子於反應溶液中,幫助核-殼結構之形成。在鹼性環境下(pH值等於11)、溫度大於80℃,且金屬前驅鹽為低濃度時,可以將前驅鹽完全還原成鎳,並披覆於α-Al2O3上形成不完全核-殼結構。
論文英文摘要:In this study, the coating of Ni on the fine α-Al2O3 (<200nm) surface was performed using chemical reducing process. The processing conditions such as pH value , temperature , concentration of metal salt precursor , and response time were optimized though analyzing the characteristic of coating layer. A typical procedure was as follows: NiCl2.6H2O in water solution was added to α-Al2O3 suspension . The suspension was then mechanical stirred and adjusted the pH to 11 , at temperature of 80℃ for 30 min , then carry on every physical and chemical analyses , including XRD、FTIR、TEM and SEM.
論文目次:摘 要 i
ABSTRACT ii
誌 謝 iii
目 錄 v
表目錄 viii
圖目錄 ix
第一章 前言 1
1.1 奈米科學的興起 1
1.2 奈米材料 3
1.3 奈米粉體的發展 6
1.4 複合奈米粒子的製備 8
第二章 基礎理論 12
2.1 研究方向 12
2.1.1 奈米觸媒 12
2.1.2 奈米鎳觸媒 14
2.2 複合奈米粒子之製備 15
2.2.1 無機物殼層披覆法 16
2.2.2 高分子殼層披覆法 24
2.2.3 生物巨分子殼層披覆法 26
2.2.4 其他披覆法 28
2.3 奈米鎳粉合成之簡介 30
2.3.1 化學還原法 30
2.3.2 成核原理 32
2.3.3 核-殼(core-shell)奈米粒子理論計算原理 39
第三章 實驗方法與步驟 40
3.1 披覆Ni的實驗流程 40
3.1.1 實驗藥品 40
3.1.2 製備純金屬鎳的實驗流程 40
3.1.3 披覆金屬鎳的實驗流程 42
3.2 氧化鋁粉末前處理 44
3.2.1 披覆聚電解質 44
3.2.2 披覆APTS 46
3.3 鎳前驅鹽之處理 47
3.3.1 慢速低入 47
3.3.2 輔助錯離子 47
3.4 分析與檢測的儀器 49
3.4.1 X-ray繞射儀(XRD) 49
3.4.2 掃描式電子顯微鏡(SEM) 49
3.4.3 電子穿透式顯微鏡(TEM) 49
3.4.4 表面電位分析儀(Zeta potential) 50
3.4.5 傅立葉轉換紅外線光譜儀(FTIR) 50
第四章 結果與討論 51
4.1 化學還原法製備金屬鎳 51
4.2 化學還原法披覆金屬鎳 58
4.2.1 披覆於氧化鋁塊材 58
4.2.2 披覆於氧化鋁粉體(以氯化鎳為前驅鹽) 63
4.2.3 披覆於氧化鋁粉體(以硫酸鎳、醋酸鎳為前驅鹽) 65
4.3 參數探討 67
4.3.1 添加速率對披覆金屬鎳的影響 67
4.3.2 表面改質對披覆金屬鎳的影響 70
4.3.3 輔助錯離子對披覆金屬鎳的影響 72
第五章 結論 73
參考文獻 74
論文參考文獻:[1] Richard P. Feynman,Surely You’re Joking Mr. Feynman:Adventures of a Curious Character,台北:天下文化(2003)
[2] M. Henini and J. M. Karam,Low dimensional structures and devices: micro- and nano-technology,Microelectronics Journal,28, 4(1997)367-370
[3] 張立德、牟季美,奈米材料和奈米結構,台中:滄海書局(2000)2-18
[4] 程國慧,給奈米熱降降溫,市場報 (2001)
[5] WTEC Panel Report on Nanostructure Science and Technology R&D Status and Trends in Nanoparticles,Nanostructured Materials and Nanodevices,8(1999)70-75
[6] Ineke Malsch,Nanotechnology in Europe: Scientific Trends and Organizational Dynamics,Nanotechnology,10, 1 (1999)1-7
[7] 經濟部技術處ITIS計畫,奈米材料於材料及化工產業的應用規畫(2003)。
[8] Duncan J Shaw,Introduction to Colloid and Surface Chemistry 4/e,台北:高立圖書(1999)1-6
[9] 中華民國粉末冶金協會、中華民國產業科技發展協進會,陶瓷技術手冊,台北:全華科技圖書,20(1994)
[10] 陳東煌,奈米複合粒子的備製與應用,化工技術,11, 3(2003)180-193
[11] Sugimoto, T,Fine Particles:Synthesis, Chararcterization, and Mechanisms of Growth,Marcel Dekker, N. Y.(2000)。
[12] 詹佳樺、陳暉,奈米粒子之包覆技術,化工技術,11, 3(2003)204-215
[13] Frank Caruso,Nanoengineering of Particle Surfaces,Advanced Materials,13, 1(5)(2001)11-22
[14] Lu, Y.,Yin, Y.,Nano Letters,2(2002)183-186
[15] 賀有郛、趙桂蓉,高觸媒活性的支撐態金觸媒,化工技術,11, 9(2003)178-183
[16] 陳郁文,奈米金屬在觸媒上的應用,化工技術,9, 6(2001)194-198
[17] 吳乃立、吳同峰,金屬氧化物小於10nm晶粒的量產合成,化工技術,9, 9(2001)160-166
[18] 林生佃、林修正,金屬觸媒之特性與應用,化工技術,2, 3(1994)55-60
[19] Y. D. Li, C. W. Li, H. R. Wang, L. Q. Li, Y. T. Qian,Preparation of nickel ultrafine powder and crystalline film by chemical control reduction,Materials Chemistry and Physics,59(1999)88-90
[20] Chou, K. S. and K. C. Huang,Studies on the Chemical Synthesis of Nanosized Nickel Powder and its Stability,Journal of Nanoparticle Research,3(2001)127-132
[21] Hirai, H., N. Yakura, Y. Seta, and S. Hodoshima,Characterization of palladium nanoparticles protected with polymer as hydrogenation catalyst,Reactive and Functional Polymers,37(1998)121-131。
[22] Kan-Sen Chou, Chiang-Yuh Ren,Synthesis of nanosized silver particles by chemical reduction method,Materials Chemistry and Physics,64(2000)241-246。
[23] Kevin E. Elkims, Tejaswi S. Vedantam, J. P. Liu, Hao Zeng, Shouheng Sun, Y. Ding,Ultrafine FePt Nanoparticles Prepared by the Chemical Reduction Method,Nano Letters,3, 12(2003)1647-1649。
[24] L. K. Kurihara, G. M. Chow, P. E. Schoen,Nanocrystalline metallic powders and films produced by the polyol method,NanoStructured Materials,5, 6(1995)607-613。
[25] 顏耀平,奈米小紅娘,靜宜大學化學電子報,9(2001)
[26] I.A. Aksay, D.M. Dabbs, M. Sarikaya,Mullite for Structural、Electronic and Optical Applications,Journal of the American Ceramic Society,74(1991)2343-2358
[27] Ramón Torrecillas, José M. Calderón, José S. Moya, Michael J. Reece, Craig K. L. Davies, Christian Olagnon and Gilbert Fantozzi,Suitability of mullite for high temperature applications,Journal of the European Ceramic Society,19, 13-14(1999)2519-2527
[28] Yue-feng Tang, Zhi-da Ling, Yi-nong Lu, Ai-dong Li, Hui-qin Ling, Yi-jun Wang,Preparation of composite coating particles of α-Al2O3–SiO2 by heterogeneous nucleation-and-growth processing,Materials Letters,56(2002)446-449
[29] Vishwas V. Hardikar and Egon Matijevi,Coating of Nanosize Silver Particles with Silica,Journal of Colloid and Interface Science,221, 1(2000)133-136
[30] Masahiro Ohmori and Egon Matijevic,Preparation and properties of uniform coated colloidal particles:Silica on hematite,Journal of Colloid and Interface Science,150, 2(1992)594-598
[31] Masahiro Ohmori and Egon Matijevic,Preparation and Properties of Uniform Coated Inorganic Colloidal Particles:Silica on Iron,Journal of Colloid and Interface Science,160, 2(1992)288-292
[32] Liz-Marzan L. M., Giersig M., Mulvaney P.,Synthesis of Nanosized Gold-Silica Core-Shell Particles,Langmuir,12, 18(1996)4329-4335
[33] Albert P. Philipse, Michel P. B. van Bruggen, Chellapah Pathmamanoharan,Magnetic silica dispersions:preparation and stability of surface-modified silica particles with a magnetic core,Langmuir,10, 1(1994)92-99
[34] Ung T., Liz-Marzan L. M., Mulvaney P.,Controlled Method for Silica Coating of Silver Colloids. Influence of Coating on the Rate of Chemical Reactions,Langmuir,14, 14(1998)3740-3748
[35] Frank Caruso, Heinz Lichtenfeld, Michael Giersig and Helmuth Mohwald,Electrostatic Self-Assembly of Silica Nanoparticle-Polyelectrolyte Multilayers on Polystyrene Latex Particles,Journal of the American Chemical Society,120(1998)8523-8524
[36] Frank Caruso, Harald Fiedler, Klaus Haage,Assembly of β-glucosidase multilayers on spherical colloidal particles and their use as active catalysts,Colloids and Surfaces,169(2000)287–293
[37] Theirry Cassagneau and Frank Caruso,Contiguous Silver Nanoparticle Coatings on Dielectric Spheres,Advanced Materials,14, 10(2002)732-736
[38] David I. Gittins, Andrei S. Susha, Frank Caruso,Denes Nanoparticulate Thin Films via Gold Nanoparticle Self-Assembly,Advanced Materials,14, 7(2002)508-512
[39] Frank Caruso, Gisela Kaltenpoth, Lorenz slansky,Conductive core-shell particles:An Approach to Self-Assembly Mesoscopic Wires,Advanced Materials,15, 13(2003)1113-1118
[40] Katja H. Rhodes, Sean A. Davis, Frank Caruso, Baojian Zhang and Stephen Mann,Hierarchical Assembly of Zeolite Nanoparticles into Ordered Macroporous Monoliths Using Core-Shell Building Blocks,American Chemical Society,12(2000)2832-2834
[41] Frank Caruso, Marina Spasova,| Andrei Susha, Michael Giersig and Rachel A. Caruso,Magnetic Nanocomposite Particles and Hollow Spheres Constructed by Sequential Layering Approach,American Chemical Society,13(2001)109-116
[42] E.L. Bizdoacaa, M. Spasovaa, M. Farlea, M. Hilgendorffb, F. Caruso,Magnetically directed self-assembly of submicron spheres with a Fe3O4 nanoparticle shell,Journal of Magnetism and Magnetic Materials,240(2002)44–46
[43] Frank Caruso, Marina Spasova, Veronica Salgueirino-Maceira and L. M. Liz-Marzan,Multilayer Assemblies of Silica-Encapsulated Gold Nanoparticles on Decomposable Colloid Templates,Advanced Materials,13, 14(2001)1090-1094
[44] Shicheng Zhang, Jie Chen and Xingguo Li,Preparation of uniform CdSe / polyelectrolyte multilayers on the surface of SiO2 spheres,Institute of Physics Publishing,15(2004)477-479
[45] Frank Caruso and Helmuth Mohwald,Preparation and Characterization of Ordered Nanoparticle and Polymer Composite Multilayers on Colloids,Langmuir,15(1999)8276-8281
[46] Rachel A. Caruso, Andrei Susha and Frank Caruso,Multilayered Titania, Silica, and Laponite Nanoparticle Coatings on Polystyrene Colloidal Templates and Resulting Inorganic Hollow Spheres,American Chemical Society,13(2001)400-409
[47] S. J. Oldenburg, R. D. Averitt, S. L. Westcott and N. J. Halas,Nanoengineering of optical resonances,Chemical Physics Letters,288, 2-4(1998)243-247
[48] Marinakos, S. M.; Novak, J. P.; Brousseau, L. C., III; House, A. B.; Edeki, E. M.; Feldhaus, J. C.; Feldheim, D. L,Gold Particles as Templates for the Synthesis of Hollow Polymer Capsules. Control of Capsule Dimensions and Guest Encapsulation,American Chemical Society,121(1999)8518-8522
[49] Liao, M. H., Wu, K. Y., and Chen, D. H.,Journal of Materials Chemistry,12(2002)3654
[50] Hofman-Caris,New Journal of Chemistry,18(1994)1087
[51] Quaroni, L., Chumanov, G.,Preparation of Polymer-Coated Functionalized Silver Nanoparticles,Journal of the American Chemical Society,121(1999)10642-10643
[52] Christof M. Niemeyer,Nanoparticles, Proteins, and Nucleic Acids: Biotechnology Meets Materials Science,Angewandte Chemie International Edition,40, 22(2001)4128-4158
[53] Tamil Selvan, Joachim P. Spatz, Harm-Anton Klok, Martin Möller,Gold-Polypyrrole Core-Shell Particles in Diblock Copolymer Micelles,Advanced Materials,10, 2(1998)132-134
[54] Karen L. Wooley,Shell Crosslinked Polymer Assemblies:Nanoscale Constructs Inspired from Biological Systems,Journal of Polymer Science. Part A:Polymer Chemistry,38, 9(2000)1397-1407
[55] Fung, K.K.; Qin, Boxiong; Zhang, X.X.,Passivation of α-Fe nanoparticle by epitaxial γ-Fe2O3 shell,Materials Science and Engineering:A,286, 1(2000)135-138
[56] Li, Y. L. and Ishigaki, T.,Journal of Materials Chemistry,407(2002)79
[57] S. Link, Z. L. Wang, M. A. El-Sayed,Alloy Formation of Gold-Silver Nanoparticles and the Dependence of the Plasmon Absorption on Their Composition,The Journal of Physical Chemistry:B,103,18(1999)3529-3533
[58] Naoki Toshima, Masafumi Harada, Yoshinao Yamazaki, Kiyotaka Asakura,Catalytic activity and structural analysis of polymer-protected gold-palladium bimetallic clusters prepared by the simultaneous reduction of hydrogen tetrachloroaurate and palladium dichloride,The Journal of Physical Chemistry,96, 24(1992)9927-9933
[59] N. Toshima, K. Kushihashi, T. Yonezawa, H. Hirai,Chemistry Letters,(1989)1769
[60] P. Y. Silvert, V. Vijayakrishnan, P. Vibert, R. Herrera-Urbina, K. T. Elhsissen,Synthesis and characterization of nanoscale Ag-Pd alloy particles,Nanostructured Materials,7, 6(1996)611-618
[61] P. Y. Silvert, K. Tekaia-Elhsissen,Synthesis of monodisperse submicronic gold particles by the polyol process,Solid State Ionics,82, 1-2(1995)53-60
[62] Raymonde Touroude, Paule Girard, Gilbert Maire, Jerzy Kizling, Magali Boutonnet-Kizling and Per Stenius,Preparation of colloidal platinum/palladium alloy particles from non-ionic microemulsions: Characterization and catalytic behaviour ,Colloids and Surfaces,67, 9(1992)9-19
[63] Sangregorio, M. Galeotti, U. Bardi, P. Baglioni,Langmuir,12(1996)5800
[64] 任鏘諭Chiang-Yuh Ren,奈米金屬微粒之製備及其性質研究「Preparation and Characterization of nanosized ultrafine metal particles」,國立清華大學化學工程學系碩士論文,(1998)
[65] 王鉦源Zhang-Yuan Wang,以化學還原法製備奈米級銀鈀微粉「Preparation of Nanosize Silver-Palladium Particles by Chemical Reduction Method」,國立成功大學化學工程學系碩士論文,(2002)
[66] 呂宗昕,電子陶瓷之溶液法粉體製備技術,化工技術,1, 6(1993)34-41
[67] 黃楷熒Kai-Ying Huang,化學還原法生成鎳絲及其反應機制探討,國立清華大學化學工程學系碩士論文,(2003)
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