淡江大學覺生紀念圖書館 (TKU Library)
進階搜尋


下載電子全文限經由淡江IP使用) 
系統識別號 U0002-2307200912094200
中文論文名稱 以共沉澱法製備鐵酸鋇粉體及其特性之分析
英文論文名稱 Preparation and characterization of the BaFe12O19 by co-precipitation method
校院名稱 淡江大學
系所名稱(中) 化學工程與材料工程學系碩士班
系所名稱(英) Department of Chemical and Materials Engineering
學年度 97
學期 2
出版年 98
研究生中文姓名 王唯穎
研究生英文姓名 Wei-Ying Wang
學號 696401339
學位類別 碩士
語文別 中文
口試日期 2009-06-19
論文頁數 68頁
口試委員 指導教授-余宣賦
委員-張裕祺
委員-尹庚鳴
中文關鍵字 共沉澱法  鐵酸鋇 
英文關鍵字 Co-precipitation method  barium ferrite 
學科別分類
中文摘要 本研究以改良後的共沉澱法合成出高磁性之六角鐵酸鋇粉體。將鋇、鐵硝酸鹽類依BaFe12O19化學計量比混合溶於100毫升的水溶液,再滴入溫度為30℃、400毫升的氨水和丙酮溶液中進行沉澱反應3小時。溶液中,氨水和丙酮的相對量藉由R值(R值定義為氨水使用的體積量/丙酮和氨水的總體積量)來調整,R值範圍為0到1。經離心程序後將所收集的粒子於300℃乾燥且之後於600到900℃間進行煆燒。煆燒後的粉體會經X-光繞射儀、紅外線光譜儀、掃描式電子顯微鏡、穿透式電子顯微鏡、振動樣品磁性量測儀等的測試來瞭解其特性。實驗結果指出鐵酸鋇的結晶能於650℃生成但是其樣品仍然含有部分的BaCO3和α-Fe2O3。要得到純鐵酸鋇粉體須將沉澱物煆燒溫度提高到800℃。當R值為0.6且煆燒溫度為800℃時,所得到鐵酸鋇粉體之飽和磁化強度為67.7 emu/g和矯頑磁力為4.84 kOe。
英文摘要 Hexagonal barium ferrite (BaFe12O19) powders with superior magnetic properties were synthesized using a modified co-precipitation method. One hundred milliliters of the aqueous solution, containing the stoichiometric amounts of barium and iron nitrates to form BaFe12O19, were added into the 400-mL solution of acetone and ammonia, which was controlled at 30 C, to undergo precipitation reaction for 3 h. The relative amounts of acetone and ammonia in the solution were varied according to R (define : volume of ammonia used/the total volume of the solution of acetone and ammonia) and R ranged from 0 to 1. After being centrifugally separated, the collected particles were dried at 300 C, followed by calcining at temperatures (T) between 600 ~ 900 C. The calcined particles were then characterized using x-ray diffractometer, infrared spectrometer, scanning electron microscope, transmittance electron microscope, and vibrating sample magnetometer. The experimental results indicated that crystalline BaFe12O19 was able to be formed at 650 C but the specimen still contained some BaCO3 and a-Fe2O3. To obtain pure BaFe12O19 powder, calcining the precipitates at 800 oC were required. When R = 0.6 and T = 800 oC, the obtained BaFe12O19 powder exhibited saturated magnetization of 67.7 emu/g and coercive force of 4.84 kOe.
論文目次 目錄
頁次
中文摘要…………………………………………………………………Ⅰ
英文摘要…………………………………………………………………Ⅱ
目錄......................................................Ⅲ
圖目錄……………………………………………………………………Ⅴ
表目錄……………………………………………………………………Ⅶ
第一章 緒論……………………………………………………………1
第二章 理論基礎與文獻回顧……………………………………………4
2-1 鋇鐵氧磁體晶體結構……………………………………4
2-2 鋇鐵氧磁體的磁性質……………………………………………………….6
2-2-1飽和磁化強度………………………………………………………...6
2-2-2矯頑磁力……………………………………………………………...8
2-2-3理論密度……………………………………………………………...9
2-3 文獻回顧……………………………………………………………...........10
2-3-1 傳統固態反應法…………………………………………………...10
2-3-2 玻璃結晶化法……………………………………………………...11
2-3-3 水熱合成法………………………………………………………...12
2-3-4 噴霧熱解法………………………………………………………...13
2-3-5 化學共沈澱法……………………………………………………...14
2-3-6 溶膠-凝膠法………………………………………………………..16
2-3-7 檸檬酸鹽先驅物法………………………………………………...18
第三章 實驗步驟與方法……………………………………………………………20
3-1 實驗步驟…………………………………………………………………...20
3-2 儀器分析與操作狀態……………………………………………………...24
3-2-1 XRD繞射析儀……………………………………………………...24
3-2-1-1 計算晶粒大小…………………………………………………26
3-2-2掃描式電子顯微鏡………………………………………………….28
3-2-3傅氏轉換紅外線光譜儀…………………………………………….30
3-2-4穿透式電子顯微鏡………………………………………………….32
3-2-5震動樣品磁性量測儀……………………………………………….33
第四章 結果與討論…………………………………………………………………35
4-1 比例R值的解釋…………………………………………………………...35
4-2 不同R值所製備300℃前驅物粉體之分析………………………………35
4-3 熱處理溫度對鋇鐵氧化物結構的影響…………………………………...41
4-4 不同R值,熱處理800℃所得粉體之磁性及其型態分析………………..52
第五章 結論…………………………………………………………………………63
參考文獻……………………………………………………………………………..64

圖目錄
頁次
圖1-1 水平及垂直記錄系統示意圖…………………………………………………3
圖2-1 磁鉛石(magnetoplumbite)型構造與磁性構造……………………………….5
圖2-2 BaFe12O19值的飽和磁化強度與溫度的變化關係……………………………7
圖3-1 共沉澱法實驗流程圖………………………………………………………..22
圖3-2 X光繞射對晶格所產生之繞射………………………………………………25
圖3-3 掃描式電子顯微鏡剖面機構示意圖………………………………………..29
圖3-4 VSM訊號傳遞示意圖………………………………………………………..34
圖4-1 不同R值,300℃前驅物粉體之XRD圖……………………….………….39
圖4-2 不同R值,300℃前驅物粉體之FT-IR圖……………………………………40
圖4-3 不同R值,300℃前驅物粉體,熱處理600℃ 5小時之XRD圖…………....44
圖4-4 不同R值,300℃前驅物粉體,熱處理600℃ 5小時之FT-IR圖...............…45
圖4-5 不同R值,300℃前驅物粉體,熱處理650℃ 5小時之XRD圖…................46
圖4-6 不同R值,300℃前驅物粉體,熱處理650℃ 5小時之FT-IR圖………...…47
圖4-7 不同R值,300℃前驅物粉體,熱處理700℃ 5小時之XRD圖…………....48
圖4-8 不同R值,300℃前驅物粉體,熱處理700℃ 5小時之FT-IR圖…………...49
圖4-9 不同R值,300℃前驅物粉體,熱處理800℃ 5小時之XRD圖……………50
圖4-10 不同R值,300℃前驅物粉體,熱處理800℃ 5小時之FT-IR圖………….51
圖4-11 不同R值,300℃前驅物粉體,熱處理800℃所得粉體之飽和磁化值……54
圖4-12 不同R值,300℃前驅物粉體,熱處理800℃ 5小時之磁性分析………...55
圖4-13 不同R值,300℃前驅物粉體,熱處理800℃ 5小時之SEM圖…………..60
圖4-14 不同R值,300℃前驅物粉體,熱處理800℃ 5小時之TEM圖…………..62

表目錄
頁次
表3-1 共沉澱實驗過程所需使用到的化學試劑和其級數………………………..21
表3-2 儀器分析與操作狀態………………………………………………………..23
表3-3 XRD應用所提供相對應資訊………………………………………………..27
表4-1 為不同R值,前驅物熱處理800℃所得粉體測磁性質……………54
參考文獻 參考文獻

1. 楊志信,垂直記錄原理,台灣資訊儲存技術協會會刊(2005)

2. Shirk, B.T., Buessem, W.R., “Temperature Dependence of Ms and K1 of BaFe12O19 and SrFe12O19 Single Crystals,”Journal of Applied Physics, 40, 1294-1296(1969)

3. Pillai, V., Kumar, P., Multani, M.S., Shah, D.O., “ Structure and magnetic properties of nanoparticles of barium ferrite synthesized using microemulsion processing,” Colloids and Surfaces A : Physicochemical and Engineering Aspects, 80, 69-75(1993)

4. Sharrock, Michael P., “Particulate Magnetic Recording Media: A Review,” IEEE Transactions on Magnetics, 25, 4374-4389(1989)

5. Liu, X., Wang, J., Gan, L.-M., Ng, S.-C., “Improving the magnetic properties of hydrothermally synthesized barium ferrite,” Journal of Magnetism and Magnetic Materials, 195, 452-459(1999)

6. Cabañas, M.V., González-Calbet, J.M., Vallet-Regí, M., “Influence of the synthetic route on the BaFe12O19 properties,” Solid State Ionics , 63-65, 207-212(1993)

7. File No. 39-1433, Powder Diffraction File, compiled by the JCPDS-International Centre for Diffraction Data in cooperation with the American Society for Testing and Materials.

8. Smit, J., Wijn, H. P., Ferrites, J., pp.369 (New York: Wily,1959. This book is published in the Philips Technical Library series).

9. Stoner, E.C., Wohlfarth, E.P., “A mechanism of magnetic hysteresis in heterogeneous alloys,” IEEE Transactions on Magnetics, 27 (4), 3475-3518 (1991)

10. Temuujin, J., Aoyama, M., Senna, M., Masuko, T., Ando, C., Kishi, H., Minjigmaa, A., ”Crystallization of M-type hexagonal ferrites from mechanically activated mixtures of barium carbonate and goethite,” Bulletin of Materials Science, 29 (5), 457-460(2006)

11. 王玉瑞和李國瑋,由集塵灰以固態反應法製備BaFe12O19及NiFe2O4,國立台北科技大學材料科學與工程研究所碩士論文(2006)

12. Barb, D., Diamandescu, L., Rusi, A., TǍrǍbǍsanu-MihǍilǍ, D., Morariu, M., Teodorescu, V., “Preparation of barium hexaferrite by a hydrothermal method: structure and magnetic properties ,” Journal of Materials Science, 21 (4), 1118-1122(1986)

13. Wang, J., Wu, Y., Zhu, Y., Wang, P., ” Formation of rod-shaped BaFe12O19 nanoparticles with well magnetic properties ,” Materials Letters, 61 (7), 1522-1525(2007)

14. Messing, G.L., Zhang, S.C., Jayanthi, G.V., “Ceramic Powder Synthesis by Spray Pyrolysis,” Journal of the American Ceramic Society, 76(11), 2707 – 2726(1993)

15. Lee, H.M., Bae, S.-Y., Yu, J.-H., Kim, Y.-J., “Preparation of Unsintered Spherical BaFe12O19 Nanoparticles via an Alcohol-Assisted Spray-Pyrolysis Route,” Journal of the American Ceramic Society, 91 (9), 2856-2861(2008)

16. González-Carreño, T., Morales, M.P., Serna, C.J., ”Barium ferrite nanoparticles prepared directly by aerosol pyrolysis ,” Materials Letters 43 (3), 97-101(2000)

17. Hsiang, H.-I., Yao, R.-Q., ” Hexagonal ferrite powder synthesis using chemical coprecipitation ,” Materials Chemistry and Physics , 104 (1), 1-4(2007)


18. Moghaddam, K.S., Ataie, A., ” Role of intermediate milling in the processing of nano-size particles of barium hexaferrite via co-precipitation method,” Journal of Alloys and Compounds , 426 (1-2), 415-419(2006)

19. Lisjak, D., Drofenik, M., ” The low-temperature formation of barium hexaferrites ,” Journal of the European Ceramic Society, 26 (16), 3681-3686(2006)

20. Rashad, M.M., Radwan, M., Hessien, M.M., ” Effect of Fe/Ba mole ratios and surface -active agents on the formation and magnetic properties of co-precipitated barium hexaferrite,” Journal of Alloys and Compounds, 453 (1-2), 304-308(2008)

21. Sürig, C., Hempel, K.A., Bonnenberg, D., ” Formation and microwave absorption of barium and strontium ferrite prepared by sol-gel technique,” Applied Physics Letters, 63 (20), 2836-2838(1993)

22. Martinez Garcia, R., Reguera Ruiz, E., Estevez Rams, E., Martinez Sanchez, R., ” Effect of precursor milling on magnetic and structural properties of BaFe12O19 M-ferrite,” Journal of Magnetism and Magnetic Materials, 223 (2), 133-137(2001)

23. Fortes, S.S., Duque, J.G.S., Macêdo, M.A., ” Nanocrystals of BaFe12O19 obtained by the proteic sol-gel process,” Physica B: Condensed Matter ,384 (1-2), 88-90(2006)

24. Shang, H., Wang, J., Liu, Q., ” Synthesis and characterization of nanocrystalline BaFe12O19 obtained by using glucose as a fuel,” Materials Science and Engineering A ,456 (1-2), 130-132(2007)

25. Mali, A., Ataie, A., “Structural characterization of nano-crystalline BaFe12O19 powders synthesized by sol–gel combustion route,” Scripta Materialia, 53(9), 1065-1070(2005)

26. Zhong, W., Ding, W., Jiang, Y., Zhang, N., Zhang, J., Du, Y., Yan, Q., ” Preparation and magnetic properties of barium hexaferrite nanoparticles produced by the citrate process ,” Journal of the American Ceramic Society ,80 (12), 3258-3262(1997)

27. Yu, H.-F., Huang, K.-C.,” Preparation and characterization of ester-derived BaFe12O19 powder,” Journal of Materials Research, 17 (1), 199-203(2002)

28. Yu, H.-F., Liu, P.-C., ” Effects of pH and calcination temperatures on the formation of citrate-derived hexagonal barium ferrite particles,” Journal of Alloys and Compounds, 416 (1-2), 222-227(2006)

29. Lee, W.-J., Fang, T.-T., ” The effect of the molar ratio of cations and citric acid on the synthesis of barium ferrite using a citrate process,” Journal of Materials Science 30 (17), 4349-4354(1995)

30. 汪建民主編,材料分析,中國材料科學學會(1998)

31. 鄭信民、林麗娟,X光繞射應用簡介,工業材料雜誌181期(2006)

32. 道斯,穿透式及掃描式電子顯微鏡生物技術,國立編譯館(1983)

33. 楊永盛、楊宗慶,電子顯微鏡原理與應用,文京圖書有限公司(1975)

34. 陳季南,穿透式電子顯微鏡在半導體製程之應用,電子月刊第三卷第三期(1997)

35. Socrates, G., Infrared and Raman Characteristic Group Frequencies Table and Charts, 3rd ed., Wiley, Chichester, UK, (2001)

36. Taha, S., Tosson, M., “The effect of temperature and phase state on the infrared spectrum of Ba(NO3)2,” Thermochimica, 236, 217-226(1994)

37. Huang, J.-G., Zhuang, H.-R., Li, W.-L., ” Synthesis and characterization of nano crystalline BaFe12O19 powders by low temperature combustion,” Materials Research Bulletin, 38, 149-159(2003)

38. 向性一和姚壬謙,化學共沉澱法製備Co2Z鐵氧磁體粉末之生成機構,國立成功大學資源工程研究所碩士論文(2004)

39. Battisha, I.K., Afify, H.H., Ibrahim, M., ” Synthesis of Fe2O3 concentrations and sintering temperature on FTIR and magnetic susceptibility measured from 4 to 300 K of monolith silica gel prepared by sol-gel technique,” Journal of Magnetism and Magnetic Materials, 306(2), 211-217(2006)

40. Xu, P., Han, X.-J., Wang, M.-J., “ Synthesis and Magnetic Properties of BaFe12O19 Hexaferrite Nanoparticles by a Reverse Microemulsion Technique,” The Journal of Physical Chemistry C, 111(16), 5866-5870(2007)









論文使用權限
  • 同意紙本無償授權給館內讀者為學術之目的重製使用,於2010-07-30公開。
  • 同意授權瀏覽/列印電子全文服務,於2010-07-30起公開。


  • 若您有任何疑問,請與我們聯絡!
    圖書館: 請來電 (02)2621-5656 轉 2281 或 來信