臺灣博碩士論文加值系統

本研究以Sr(NO3)2、Fe(NO3) 3．9H2O、Ti粉及glycine（NH2CH2COOH）為反應物，已成功藉由「類乾式」燃燒合成法合成添加不同比例鈦酸鍶（SrFe12O19+xSrTiO3,，x=0.00、 0.05、 0.10、 0.15 和 0.20）之鍶鐵氧磁體粉末。經過均勻的混合及完全脫水後，可以得到均勻具可燃性的先驅物。在室溫下引燃先驅物，燃燒反應會伴隨大量氣體及產生大量疏鬆的產物。將初合成產物在不同溫度下煅燒（直到1200℃），再研究煅燒溫度對產物特性和相變化的影響。我們將所得的粉體以XRD、TG-DSC-MS、SEM、TEM、VSM和表面積量測儀作鑑測，對物質特性作分析。當x=0時，我們在煅燒溫度約1000℃時就可以得到幾乎是純的鍶鐵氧體。煅燒溫度為1050℃時，會產生晶體粒徑範圍約在60-75 nm且為單一磁區的純鍶鐵氧體（SrFe12O19），此時最大矯頑磁力（maximum intrinsic coercivity，iHc）為5.95kOe，飽和磁化量（magnetization value，Mmax）為60.13 emu/g，殘餘磁化量（residual magnetization，Mr）為31.75 emu/g。當煅燒溫度升到1200℃時，最大磁化量亦增加為68.52 emu/g；但最大矯頑磁力則降低了。根據實驗的數據，我們也提出了鍶鐵氧體生成的機制。我們再將以不同x值所合成出來的粉末以不同溫度煅燒，並和聚氨酯混合形成測試樣品。我們以向量網路分析儀來量測此複合型材料樣品，在1-12 GHz時的複數介電常數以及導磁率。當鈦酸鍶（SrTiO3）分別從0~20 mol％加進鍶鐵氧體，其效果不只是改善了介電常數值，也使導磁率得到了提昇。煅燒溫度對介電常數值以及導磁率的影響和加入鈦酸鍶的影響雷同。我們根據產物型態觀察、XRD以及磁性量測來對煅燒溫度和鈦酸鍶掺入量多寡所會產生的影響作判斷、解釋。

In this work, fine powders of SrFe12O19 with different contents of SrTiO3 additive (SrFe12O19+xSrTiO3, x=0.00, 0.05, 0.10, 0.15 and 0.20, respectively) were successfully prepared via a quasi-dry combustion synthesis route using Sr(NO3)2, Fe(NO3)3．9H2O, glycine (NH2CH2COOH) and Ti powder as reactants. By directly mixing and thoroughly dehydrating, a flammable dried mixture with good homogeneity can be obtained. Once ignited in the air at room temperature, it underwent a combustion process, and with a large amount of gas smoke, a voluminous loose product was yielded. The as-synthesized powder was calcined at various temperatures, up to 1200 ℃, to study the effects of calcination temperature on phase development and products’ properties. The resultant powders were characterized by X-ray diffractometry, infrared (IR) spectrometer, simultaneous thermalgravity (TG)-differential scanning calorimetry (DSC)-mass spectrometry (MS) analysis, scanning electron microscope (SEM), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and measurement of surface area. When x=0.00 was used, a nearly pure SrFe12O19 product was obtained at temperatures as low as 1000 ℃. Pure single-magnetic-domain SrFe12O19 powders with the crystalline size ranging from ~60 to 75 nm could be observed at 1050 ℃, which exhibited an maximum intrinsic coercivity (iHc) of 5.95 kOe, the attained magnetization value (Mmax, measured at 15kOe) of 60.13 emu/g as well as the residual magnetization (Mr) of 31.75 emu/g. Whereas, upon calcining at 1200 ℃, the Mmax increased further, to 68.52 emu/g; but the iHc value reduced. According to the experimental results obtained, a possible mechanism for the formation of strontium ferrite is proposed. The as-synthesized powders and the calcined ones, obtained using different x values, were introduced into polyurethane matrix to prepare a testing specimen. The relative complex permittivity ( ) and permeability ( ) of the composite materials were measured in the frequency range of 1-12 GHz by using a network analyzer. When the amount of SrTiO3 additive incorporated into SrFe12O19 varied from 0 to 20 mol%, not only improved the as expected, but also modified the . The effect of calcination temperature on the values of and was similar to that of amount of SrTiO3 additive. The influences of both the calcinations temperature and amount of SrTiO3 additive were explained judging from the results of observations of products’ morphology, XRD analysis of phase component and measurements of magnetic properties.

誌謝 ii
摘要 iii
ABSTRACT iv
目錄 vi
表目錄 viii
圖目錄 ix
1. 緒論 1
1.1 前言……………………………………………………………………………1
1.2 研究動機及目的………………………………………………………………3
1.3 電磁波吸收體原理……………………………………………………………4
1.4 吸波材料………………………………………………………………………8
2. 文獻回顧與研究方法……………………………………………………………..9
2.1 文獻回顧………………………………………………………………………9
2.2 奈米材料對吸波特性的理論探討……………………………………………9
2.3 電磁波吸收體種類…………………………………………………………..10
2.4 鐵氧磁體……………………………………………………………………..11
2.5 實驗方法簡介（新式燃燒合成法）……………………………………......15
3. 實驗…………………………………………………………………..…………..18
3.1 藥品…………………………………………………………………………..18
3.2 分析儀器設備……………………………………………………………..…18
3.3 儀器分析檢測……………………………………………………………......19
3.4 鍶鐵氧磁體（SrFe12O19）之製備……………………………………………21
3.5 試片的製作…………………………………………………………………..22
4. 結果與討論………………………………………………………………………26
4.1 鍶鐵氧體（SrFe12O19）特性研究..……………………………………….…26
4.1.1 相變化……………………………………………………………...…26
4.1.2 IR光譜分析……………………………………………………...……28
4.1.3 熱分析……………………………………………………………...…30
4.1.4 顯微結構分析……………………………………………………...…34
4.1.5 磁滯特性…………………………………………………………...…38
4.2 鍶鐵氧體掺入鈦酸鍶（SrFe12O19＋x SrTiO3）特性研究…………….…41
4.2.1 溫度對時間概況…………………………………………………...…41
4.2.2 相變化及型態觀察…………………………………………………...42
4.2.3 電磁特性…………………………………………………………...…45
4.3 鍶鐵氧體掺入鈦酸鍶（SrFe12O19＋x SrTiO3）特性研究…………….…52
5. 結論………………………………………………………………………………54
參考文獻…………………………………………………………………………….56
論文發表…………………………………………………………………………….62
自傳………………………………………………………………………………….64

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