系統識別號 | U0002-2307200912094200 |
---|---|
DOI | 10.6846/TKU.2009.00863 |
論文名稱(中文) | 以共沉澱法製備鐵酸鋇粉體及其特性之分析 |
論文名稱(英文) | Preparation and characterization of the BaFe12O19 by co-precipitation method |
第三語言論文名稱 | |
校院名稱 | 淡江大學 |
系所名稱(中文) | 化學工程與材料工程學系碩士班 |
系所名稱(英文) | Department of Chemical and Materials Engineering |
外國學位學校名稱 | |
外國學位學院名稱 | |
外國學位研究所名稱 | |
學年度 | 97 |
學期 | 2 |
出版年 | 98 |
研究生(中文) | 王唯穎 |
研究生(英文) | Wei-Ying Wang |
學號 | 696401339 |
學位類別 | 碩士 |
語言別 | 繁體中文 |
第二語言別 | |
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 |
關鍵字(中) |
共沉澱法 鐵酸鋇 |
關鍵字(英) |
Co-precipitation method barium ferrite |
第三語言關鍵字 | |
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. |
第三語言摘要 | |
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 |
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