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研究生:李鳳釵
研究生(外文):Feng-Chan Lee
論文名稱:家用微波爐用於材料合成之研究
論文名稱(外文):Modification of the domestic microwave oven for material synthesis study
指導教授:張聰慧張聰慧引用關係
指導教授(外文):Tsong-Huei Chang
學位類別:碩士
校院名稱:明新科技大學
系所名稱:化學工程與材料科技系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2011
畢業學年度:99
語文別:中文
論文頁數:73
中文關鍵詞:片狀銅磷酸鋰鐵微波加熱法改裝家用微波爐
外文關鍵詞:microwave heatingmodified household microwavecopper flake
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本研究是利用微波加熱法(Microwave-aided Method)製備奈米及次微米材
料。在實驗中改裝了家用微波爐便於控溫和使用於材料之合成,期能達到以簡
便、便宜及節能的方式來製備各材料。其中熱媒部分使用碳化矽(SiC) ,以達到
耐高熱、吸收熱能及傳播熱能,故以SiC 做為吸收微波的吸收劑。改裝之微波爐
用於液態合成試驗中以合成片狀銅微粒子將次磷酸鈉(NaH2PO2·H2O)當作還原
劑,還原硝酸銅(Cu(NO3)2·3H2O),而四丁基氯化銨(TNBCl)當作模板,聚乙烯吡
咯烷酮(PVP)做為穩定劑。則固態合成中以合成磷酸鋰鐵(LiFePO4)為例子,將前
製動作完成之LiFePO4 粉末進行微波加熱。
實驗中合成出來的樣品用掃描式電子顯微鏡(SEM)、X 光粉末繞射儀(XRD)
等分析儀器來做鑑定。

This study a modified household microwave was used to prepare the interesting
materials such as nano and submicro material. A convenient、cheap and energy-saving
method was developed in the study. Moreover SiC was employed as a microwave
absorbent for absorbing microwave to heat up the synthesizing sample during
experiments. A testing experiment was applied to synthesize the copper flake using
the modified microwave oven.
In the experiment , sodium hypophosphite and tetrabutylammonium chloride were
employed as reducing agent and template, respectively. Techniques such as SEM and
XRD were applied to identify the synthesized samples.

摘要..................................................................................................................................I
Abstract.......................................................................................................................... II
致謝............................................................................................................................... III
目錄...............................................................................................................................IV
圖目錄.......................................................................................................................... VII
表目錄............................................................................................................................IX
第一章 緒論.................................................................................................................... 1
1.1 前言............................................................................................................... 1
1.2 文獻回顧........................................................................................................ 8
1.2.1 奈米、次微米材料之合成方法........................................................ 8
1.2.2 模板法(Template) ............................................................................ 8
1.2.3 溶媒熱法(Solvothermal Method) ................................................... 9
1.2.4 水熱法(Hydrothermal Method)...................................................... 9
1.2.5 微波加熱法(Microwave Heating Method).................................... 10
1.2.5.1 微波加熱原理....................................................................... 11
1.2.6 吸波材料-碳化矽(Silicon Carbide)............................................... 13
1.2.6.1 微波與微波吸收材料相互作用的原理............................... 13
1.2.6.2 碳化矽(Silicon Carbide)...................................................... 15
1.3 研究動機...................................................................................................... 17
V
第二章 實驗方法.......................................................................................................... 18
2.1 實驗藥品..................................................................................................... 18
2.2 實驗儀器..................................................................................................... 20
2.3 檢測儀器之原理簡介................................................................................. 21
2.3.1 場發射掃描式電子顯微(FE-SEM) .............................................. 21
2.3.1 X 光粉末繞射儀(X-ray Powder Diffractometer;XRD)............ 24
2.4 實驗步驟..................................................................................................... 26
2.4.1 家用微波爐之改裝步驟................................................................. 26
2.4.2 家用微波爐用於合成片狀銅之流程圖.......................................... 27
2.4.3 家用微波爐用於合成片狀銅之步驟.............................................. 28
2.4.4 家用微波爐用於合成LiFePO4 之流程圖...................................... 29
2.4.4 家用微波爐用於合成LiFePO4 之步驟.......................................... 30
第三章 結果與討論...................................................................................................... 31
3.1 家用微波爐之改裝...................................................................................... 31
3.2 碳化矽(SiC)對微波吸收之探討................................................................. 35
3.3 改裝家用微波爐合成片狀銅...................................................................... 37
3.3.1 固定 NaH2PO2·H2O=2.269M、Cu(NO3)2·3H2O=0.035M 及
TNBCl=0.06M................................................................................ 40
3.3.2 固定 NaH2PO2·H2O=2.092M、Cu(NO3)2·3H2O=0.816M 及
TNBCl=0.060M .............................................................................. 44
3.3.3 固定 NaH2PO2·H2O=4.201M、Cu(NO3)2·3H2O=1.536M 及
TNBCl=0.06M ................................................................................ 48
V I
3.3.4 微波加熱時間對合成銅的影響..................................................... 52
3.4 改裝家用微波爐合成LiFePO4.................................................................. 54
第四章 結論.................................................................................................................. 56
第五章 參考文獻.......................................................................................................... 57
V II
圖目錄
圖1- 1 一維金屬奈米材料之應用示意圖...................................................................... 4
圖1- 2 奈米科技產業應用範圍...................................................................................... 5
圖1- 3 電磁波能譜........................................................................................................ 11
圖1- 4 電磁波的傳播.................................................................................................... 12
圖1- 5 電磁波在電場中分子運動示意圖.................................................................... 13
圖1- 6 家用微波爐........................................................................................................ 17
圖2- 1 場發射掃描式電子顯微鏡(FE-SEM)基本構造……………………………. 21
圖2-2 FEG (FIELD EMISSION GUN)…………………………………………..………22
圖2- 3 六硼化鑭(LAB6)................................................................................................ 22
圖2- 4 鎢陰極(W FILAMENT)........................................................................................ 22
圖2- 5 晶體繞射X-RAY 時之布拉格定律繞射結構圖............................................... 24
圖2- 6 進行X 光繞射時之樣品旋轉示意圖............................................................... 25
圖2- 7 SHIMADZU LABX XRD-6000.............................................................................. 25
圖2- 8 改裝微波爐內部................................................................................................ 26
圖2- 9 合成片狀銅實驗步驟流程圖............................................................................ 27
圖2- 10 合成LIFEPO4 實驗步驟流程圖..................................................................... 29
圖3- 1 家用微波爐的外觀……………………………………………………………31
圖3- 2 微波爐的側面.................................................................................................... 32
圖3- 3 (A)旋轉軸取下後的洞(B)溫度控制器............................................................... 32
圖3- 4 磁控管................................................................................................................ 33
圖3- 5 凹型石英皿(A) 設計圖(B)實品........................................................................ 34
VI II
圖3- 6 未經過燒結之SIC ............................................................................................ 35
圖3- 7 設定400℃、10 分鐘碳化矽燒結情況............................................................ 36
圖3- 8 (A)、(B)設定500℃、10 分鐘碳化矽燒結情況............................................ 36
圖3- 9 片狀銅之合成XRD 圖..................................................................................... 39
圖3- 10 片狀銅之合成EDS 圖................................................................................... 39
圖3- 11 PVP 濃度為1.003M SEM 圖....................................................................... 42
圖3- 12 PVP 濃度為0.713M SEM 圖......................................................................... 42
圖3- 13 PVP 濃度為0.669M SEM 圖......................................................................... 42
圖3- 14 PVP 濃度為0.044M SEM 圖......................................................................... 46
圖3- 15 PVP 濃度為0.667M SEM 圖......................................................................... 46
圖3- 16 PVP 濃度為1.113M SEM 圖.......................................................................... 46
圖3- 17 PVP 濃度為1.113M SEM 圖.......................................................................... 50
圖3- 18 PVP 濃度為0.891M SEM 圖......................................................................... 50
圖3- 19 PVP 濃度為0.446M SEM 圖......................................................................... 50
圖3- 20 (A)合成時間為25 分鐘(B)合成時間為30 分鐘(C) 合成時間為45 分鐘.... 53
圖3- 21 LIFEPO4 之XRD 圖....................................................................................... 54
圖3- 22 (A)為經微波加熱之LIFEPO4 (B)經過微波加熱之LIFEPO4 ....................... 55
IX
表目錄
表1- 1 微波加熱國際 ISM 組織規範之頻率表.......................................................... 11
表1- 2 工業及研究用微波爐與家用微波爐比較表.................................................... 17
表3- 1 JCPDS file NO. 85-1326………………………………………………………37
表3- 2 片狀銅之X-光粉末繞射光譜分析................................................................. 38
表3- 3 PVP 為1.003M 濃度及溫度對照表............................................................... 40
表3- 4 PVP 為0.713M 濃度及溫度對照表.............................................................. 41
表3- 5 PVP 為0.669M 濃度及溫度對照表.............................................................. 41
表3- 6 PVP 為0.044M 濃度及溫度對照表.............................................................. 44
表3- 7 PVP 為0.667M 濃度及溫度對照表.............................................................. 44
表3- 8 PVP 為1.113M 濃度及溫度對照表.............................................................. 45
表3- 9 PVP 為0.267M 濃度及溫度對照表.............................................................. 48
表3- 10 PVP 為0.891M 濃度及溫度對照表............................................................ 48
表3- 11 PVP 為0.446M 濃度及溫度對照表............................................................ 49
表3- 12 濃度及溫度對照表.......................................................................................... 52
表3- 13 JCPDS FILE NO. 77-0179................................................................................ 54
表3- 14 LIFEPO4 之X-光粉末繞射光譜分析............................................................. 55

1. 丁志明、方冠榮、吳季珍、周維揚、胡裕民、翁鴻山、陳東煌、傅昭銘、馮榮
豐、黃榮俊、黃耀輝、張鼎張、劉全璞、蔡振章、蕭璦莉、謝達斌, (2008). 奈
米科技-基礎、應用與實作, 台北:高立圖書有限公司.
2. 馬遠榮, (2002). 奈米科技, 台北:商周出版社.
3. S. Bandyopadhyay , H. S. Nalwa, “Quantum Dots and Nanowires” , American
Scientific Publishers, (2003) .
4. S. Xu, X. Sun, H. Ye, T. You, X. Song, S. Sun, “Selective Synthesis of Copper
Nanoplates and Nanowires via a Surfactant-assisted Hydrothermal process”, Mater.
Sci. Eng. A. , 120 (2010) 1.
5. A. S. Edelstein, R. C. Cammarata,“Nanomaterials: Synthesis, Properties and
Applications”, Bristol: Institute of Physics Publishing, (1996).
6. 邏吉宗、戴明鳳、林鴻明、鄭振宗、蘇程裕、吳育民, (2008). 奈米科技導論, 台
北: 全華圖書出版社.
7. J. H. Fendler,“Naniparticles and Nanostructured Film: Preparation, Characterization
Applications”, New York: Wiley-VCH, (1998).
8. 廖建勛, 奈米材料的發展動態, 化工資訊2 月, (1998) 20.
9. 張立德, (2000) . 奈米材料, 北京: 化學工業出版社.
10. 張立德、牟季美, (2000). 納米材料與納米結構, 北京: 科學出版社.
11. 汪信, (2006). 奈米材料化學, 台北: 五南出版社.
12. 莊萬發, (2005). 超微粒子理論應用, 台南: 復漢出版社.
13. 蘇品書, (1989). 超微粒子材料技術, 台南: 復漢出版社.
5 8
14. N. A. Goldstein , “Handbook of Nanophase Materials” , New York:Marcel Dekker ,
(1997).
15. S. Gunter, (1994). “Clusters and Colloids:From Theory to Application”, New
York:Wiley-VCH.
16. 呂宗昕, (2005). 奈米科技與光觸媒, 台北: 商周出版社.
17. 黃德歡, (2002). 改變世界的奈米技術, 台北: (美國)瀛舟出版社.
18. 經濟部投資業務處, (2008). 奈米科技及應用之產業分析與投資機會.
19. S. Iijima, “Helecal Micro-tubules of Graphitic Carbon”, Nature, 354 (1991) 56.
20. 許樹恩、吳泰伯, (1996). X 光繞射原理與材料結構分析, 新竹:中國材料科學學
會.
21. 黃怡婷, (2010). 奈米銅線合成之研究, 明新科技大學化學工程與材料科技研究
所碩士學位論文.
22. J. Hu, T. W. Odom, C. M. Lieber, “Chemistry and Physics in One Dimension:
Synthesis and Properties of Nanowires and Nanotubes”, Acc. Chem. Res., 32 (1999)
435.
23. R. S. Wagner and W. C. Ellis, “Vapor-Liquid-Solid Mechanism of Single Crystal
Growth”, Appl. Phys. Lett., 4 (1964) 89.
24. W. Wenzhong, G. Yan, Q. Yitai, J. Mingrong, L. Xianming, “A Novel Pathway to
PbSe Nanowire at Room Temperature”, Adv. Mater. , 10 (1998) 1479.
25. C. Jerome, R. Jerome, “Electrochemical Synthesis of Polypyrrole Nanowires”,
Angew. Chem., Int. Ed. Engl., 37 (1998) 2488.
26. M. Stella, L. C. Marinakos, C. Brousseau III, A. Jones, D. L. Feldheim
“Templatesynthesis of One-Dimensional Au, Au-Poly(pyrrole), and Poly(pyrrole)
NanoparticleArrays”, Chem. Mater., 10 (1998) 1214.
27. H. Sakaue, A. Kojima, N. Osada, S. Shingubara T. Takahagi,“Highly Selective SiO2
5 9
Etching Using CF4/V2H4”, Jpn. J. Appl. Phys. , 36 (1997) 2477.
28. J. F. Liu, K. Z. Yang, Z. H. Lu, “Controlled Assembly of Regylar Composite
Nanowire Arrays and Their Multilayers Using Electropolymerized Polymers as
Templates”, J. Am. Chem. Soc. 119 (1997) 11601.
29. Y. Zhou, S.H. Yu, X. P. Cui, C. Y. Wang, Z. Y. Chen, “Formation of silver nanowires
by a novel solid-liquid phase arc discharge method”, Chem. Mater. 11 (1999) 545.
30. B. A. Korgel & D. Fitzmaurice, “Self-assembly of silver nanocrystals into
two-dimensional nanowire arrays”, Adv. Mater., 10 (1998) 661.
31. 傅耀賢, 新穎奈米線(棒)低溫合成技術簡介, 化工資訊與商情, 2 (2003).
32. J. Xuchuan, X. Xie, L. Lu, Z. Zhu, H. Wei, Q. Yitai, “Simultaneous In Situ
Formation of ZnS Nanowires in a Liquid Crystal Template by γ-Irradiation” Chem.
Mater., 13 (2001) 1213.
33. K. B. Tang, Y.-T. Qian, J.-H. Zeng, X.-G. Yang, “Solvothermal Route to
Semiconductor Nanowires” , Adv. Mater., 15 (2003) 448.
34. W. Wenzhong, G. Yan, Y. Ping, L. Fuyu, X. Yi, Q. Yitai, “A Novel Mild Route to
Nanocrystalline Selenides at Room Temperature”, J. Am. Chem. Soc. , 121 (1999)
4062.
35. Y. D. Li, H. W. Liao, Y. T. Qian, L. Yang, G. E. Zhou, “Nonaqueous Synthesis of
CdS Nanorod Semiconductor”, Chem. Mater. 10 (1998) 2301.
36. 劉育兆, (2004). 微波水熱法合成金屬氧化物奈米線及奈米管, 明新科技大學化
學工程研究所碩士學位論文.
37. 彭永旺, (2005). 以微波輔助酸處理純化奈米碳管之探討, 明新科技大學化學工
程研究所碩士學位論文.
38. U.S. EPA Method 3051, “Microwave-Assisted Acid Digestion of Sediments,
Sludges,Solids and Oils”, Washington D. C. , (1994).
6 0
39. 謝沐辰, (2004). 以油酸分散氫氧化鋁膠製造α相氧化鋁粉末程序之研究, 國立
成功大學資源工程學系碩士論文.
40. 和田忠太, (2004). 機械構造解剖圖鑑, 台北: 世茂出版社.
41. X. Liu, Z. Zhang, Y. Wu, “Absorption properties of carbon black/silicon carbide
microwave absorbers”, Eng. 42 (2010) 326.
42. E.T. Thostenson, T. W. Chou, “Microwave processing: fundamentals and
applications”, Appl. Sci. Manu. 30 (1999) 1055.
43. H. Zhang, J. Zhang, H. Zhang, “Computation of radar absorbing silicon carbide
foams andtheir silica matrix composites”, Mater. Sci. , 38 (2007) 857.
44. 王麗熙、張其土, 微波吸收劑的研究現狀與發展趨勢, 材料導報, 19 (2005) 26.
45. 鐘發春、鶴江平、王曉川、趙曉東, 聚合物材料的微波製備技術, 熱固性樹脂, 21
(2006) 43.
46. S. Pallavkar, T. H. Kim, J. Lin, J. Hopper, T. Ho, H. J. Jo, J. H. Lee,
“Microwave-Assisted Noncatalytic Destruction of Volatile Organic Compounds
Using Ceramic-Based Microwave Absorbing Media”, Chem. Res. , 49 (2010) 8461.
47. W. Lei, H. Yudai, J. Rongrong, J. Dianzeng, “Preparation and characterization of
nano-sized LiFePO4 by low heating solid-state coordination method and microwave
heating”, Elect. Act. 52 (2007) 6778.
48. 朱景森、汪浩、嚴揮, 微波技術在無機固相材料合成中的應用, 化學通報, 69
(2006) 97.

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