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中文論文名稱 以改進式共沉澱法製備硬磁性鐵酸鋇
英文論文名稱 Magnetic properties of BaFe12O19 prepared by a modified co-precipitation
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 100
學期 2
出版年 101
研究生中文姓名 朱婉婷
研究生英文姓名 Wan-Ting Chu
學號 698401170
學位類別 碩士
語文別 中文
口試日期 2012-07-17
論文頁數 90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 鐵酸鋇  共沉澱法  硬磁性磁體 
英文關鍵字 BaFe12O19  Hard magnets  Co-precipitation 
學科別分類
中文摘要 本實驗利用共沉澱法來製備BaFe12O19硬磁性粉體。實驗程序中,起始水溶液為含有生成BaFe12O19所需化學劑量比的硝酸鐵與硝酸鋇,沉澱劑為氨水,而反應液態介質為水和丙酮的混合溶液。固定反應液態介質的總體積並探討改變反應液態介質中水和丙酮比例(R值:丙酮使用體積量/水和丙酮總體積量)對製得的鐵酸鋇粉體性質影響。離心收集到的沉澱物經過90℃乾燥後先做300℃5小時的預熱處理以形成所需的前驅物粉體,接著再進行600℃到1000℃5小時的煆燒處理。前驅物粉體與煆燒後所得粉體藉由熱分析儀、X-光繞射分析儀、紅外線光譜儀、掃描式電子顯微鏡、穿透式電子顯微鏡和超導量子干涉磁量儀對其特性分析。實驗結果顯示當R值為0.6時所得前驅物經600℃煆燒處理後就可出現鐵酸鋇的結晶相態,且900℃煆燒則可得到單一相態鐵酸鋇。而煆燒達1000℃時得到的鐵酸鋇粉體有67 emu/g高飽和磁化強度、33 emu/g的殘留磁場強度和5 kOe矯頑磁力。
英文摘要 BaFe12O19 powder, a hard magnetic ceramic, was synthesized using a co-precipitation method. In preparation, the following materials were used: an aqueous solution of ferric and barium nitrates, in a stoichiometric ratio to form BaFe12O19, as starting solution, ammonium as precipitating agent and a mixed liquids containing acetone and water as reaction liquid medium. By fixing the total volume of the reaction liquid medium, effects of the acetone fraction R ( = volume of acetone used/total volume of the reaction medium) in the liquid medium on the characteristics of the obtained barium ferrite powder were investigated. After precipitation and centrifugal filtration, the collected solid precipitants were dried at 90℃ and then preheated at 300℃ to form the solid precursors. The solid precursors were then calcined at different temperatures ranging from 600℃ to 1000℃. The calcined powder was characterized using thermal analyzer, x-ray diffractometer, infrared spectrometer, scanning electronic microscope, transmission electronic microscope and superconducting quantum interference device. When R = 0.6, BaFe12O19 crystalline phase was first appeared in the powder calcined at 600℃and BaFe12O19 monophase powder was obtained at 900℃. The BaFe12O19 powder obtained at R = 0.6 and 1000℃ possessed good magnetic properties: saturation magnetization of 67 emu/g, remanence magnetization of 32~33 emu/g and coercive force of 5 kOe.
論文目次 主目錄
中文摘要.....................................................................................................I
英文摘要..................................................................................................III
主目錄......................................................................................................V
圖目錄.....................................................................................................VII
表目錄......................................................................................................XI
第一章 緒論............................................................................................. 1
第二章 文獻回顧與理論基礎..................................................................4
2-1 鐵酸鋇分子結構.................................................................................4
2-2 鐵酸鋇磁性質.....................................................................................6
2-2-1 飽和磁化強度...............................................………............…6
2-2-2 矯頑磁力.…….………….........................................................8
2-3 理論密度……………………...........................................................10
2-4 BaFe12O19粉體製備方法……...........................................................11
2-4-1 傳統固態反應法....................................………............…….11
2-4-2 水熱合成法.….………….......................................................12
2-4-3 溶膠-凝膠法…………...........................................................13
2-4-4 噴霧熱解法....................................………............………….14
2-4-5 檸檬鹽先驅物法.…………....................................................15
2-4-6 化學共沉澱法………….........................................................16
第三章 實驗步驟與儀器分析................................................................20
3-1 實驗步驟.......................................................................................... 20
3-2 特性分析...........................................................................................23
3-3 儀器分析...........................................................................................24
3-3-1 X光繞射分析儀.....................................................................24
3-3-2 傅氏轉換紅外線光譜儀.........................................................26
3-3-3 掃描式電子顯微鏡.................................................................27
3-3-4 穿透式電子顯微鏡……………….........................................28
3-3-5 熱重損失分析儀與熱差掃描分析儀.....................................29
3-3-6 超導量子干涉磁量儀.............................................................30
第四章 結果與討論................................................................................31
4-1 粉體熱行為表現與特性分析...........................................................31
4-1-1 前驅物粉體熱行為表現.........................................................31
4-1-2 鐵酸鋇特性分析….................................................................50
4-2 鐵酸鋇之形態與磁性分析...............................................................66
第五章 結論............................................................................................83
參考文獻..................................................................................................85

圖目錄
圖2-1 BaFe12O19晶體結構.........................................................................5
圖2-2 BaFe12O19的飽和磁化強度與溫度變化的關係.............................7
圖2-3 磁滯曲線圖....................................................................................8
圖3-1 BaFe12O19粉體製備實驗流程圖...................................................22
圖3-2 X光對晶體所產生之繞射............................................................25
圖3-3 掃描式電子顯微鏡剖面機構示意圖..........................................28
圖4-1 前驅物粉體在空氣流率30mL/min和加熱速率10℃/min下所得之TG/DSC圖: (a) R = 0, (b) R = 0.2, (c) R = 0.4, (d) R = 0.6, (e) R = 0.7 和 (f) R = 0.8.......................................................................................…34
圖4-2 R = 0前驅物粉體加熱至90℃、300℃、400℃、600℃和900℃後(不持溫)所得粉體的XRD圖…………………………………...…..36
圖4-3 R = 0前驅物粉體加熱至90℃、300℃、400℃、500℃、600℃和900℃後(不持溫)所得粉體的FT-IR圖…………………….........…37
圖4-4 R = 0.6前驅物粉體加熱至90℃、300℃、400℃、600℃和900℃後(不持溫)所得粉體的XRD圖…………………………….................39
圖4-5 R = 0.6前驅物粉體加熱至90℃、300℃、400℃、500℃、600℃和900℃後(不持溫)所得粉體的FT-IR圖.............................................40
圖4-6 R = 0.8前驅物粉體加熱至90℃、250℃、300℃、400℃、600℃和900℃後(不持溫)所得粉體的FT-IR圖.............................................43
圖4-7 R = 0.8前驅物粉體加熱至90℃、250℃、300℃、400℃、600℃和900℃後(不持溫)所得粉體的XRD圖..............................................44
圖4-8 前驅物粉體300℃預熱處理後在空氣流率30 mL/min和加熱速率10 ℃/min下所得之TG/DSC圖: (a) R = 0, (b) R = 0.2, (c) R = 0.4, (d) R = 0.6, (e) R = 0.7 和 (f) R = 0.8..................................................……48
圖4-9 R = 0.8,90℃乾燥、300℃(不持溫)和300℃(持溫5小時)後所得粉體的XRD圖.............................................................................49
圖4-10 R = 0前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的XRD圖........................54
圖4-11 R = 0前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的FT-IR圖.......................55
圖4-12 R = 0.2前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的XRD圖........................56
圖4-13 R = 0.2前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的FT-IR圖.......................57
圖4-14 R = 0.4前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的XRD圖..........................58
圖4-15 R = 0.4前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的FT-IR圖.........................59
圖4-16 R = 0.6前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的XRD圖..........................60
圖4-17 R = 0.7前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的XRD圖..........................61
圖4-18 R = 0.8前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的XRD圖..........................62
圖4-19 R = 0.6前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的FT-IR圖.........................63
圖4-20 R = 0.7前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的FT-IR圖.........................64
圖4-21 R = 0.8前驅物粉體熱處理溫度至90℃、300℃、600℃、700℃、800℃、900℃和1000℃後(5小時)所得粉體的FT-IR圖.........................65
圖4-22 不同R值,前驅粉體熱處理800℃所得粉體之SEM圖(a) R = 0, (b) R = 0.2, (c) R = 0.4, (d) R = 0.6, (e) R = 0.7 和 (f) R = 0.8.............................................................................................................69
圖4-23 不同R值,前驅粉體熱處理900℃所得粉體之SEM圖(a) R = 0, (b) R = 0.2, (c) R = 0.4, (d) R = 0.6, (e) R = 0.7和(f)R = 0.8.............................................................................................................70
圖4-24 不同R值,前驅粉體熱處理1000℃所得粉體之SEM圖(a) R = 0, (b) R = 0.2, (c) R = 0.4, (d) R = 0.6, (e) R = 0.7 和(f) R = 0.8............................................................................................................71
圖4-25 不同R值,前驅粉體熱處理1000℃所得粉體之TEM圖(a) R = 0, (b) R = 0.2, (c) R = 0.4, (d) R = 0.6, (e) R = 0.7 和(f) R = 0.8............................................................................................................73圖4-26 R=0時,前驅粉體熱處理(a)900℃和(b)1000℃所得粉體之磁性分析........................................................................................................74
圖4-27 R=0.2時,前驅粉體熱處理(a)900℃和(b)1000℃所得粉體之磁性分析......................................................................................................75
圖4-28 R=0.4時,前驅粉體熱處理(a)900℃和(b)1000℃所得粉體之磁性分析......................................................................................................76
圖4-29 R=0.6時,前驅粉體熱處理(a)800℃、(b)900℃和(c)1000℃所得粉體之磁性分析......................................................................................78
圖4-30 R=0.7時,前驅粉體熱處理(a)900℃和(b)1000℃所得粉體之磁性分析......................................................................................................79
圖4-31 R=0.8時,前驅粉體熱處理(a)900℃和(b)1000℃所得粉體之磁性分析......................................................................................................80
圖4-32 R值為0、0.6和0.8時,前驅物粉體熱處理溫度至1000℃後(5小時)所得粉體之磁性分析....................................................................82


表目錄
表2-1 BaFe12O19之Fe3+磁矩方向............................................…………...7
表3-1 實驗所需藥品……………….......................................................21
表3-2 實驗中溶劑之體積比…...............................................................21
表4-1 不同R值鐵酸鋇在不同熱處理溫度下之磁性質........................81

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