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研究生：	劉坤儒 Liu, Kun-Ru
論文名稱：	行星式球磨對Fe-Si-Cr合金粉末之顯微結構與電磁特性影響之研究 Effect of planetary ball milling on the microstructure and electromagnetic properties of Fe-Si-Cr alloy powders
指導教授：	向性一 Hsiang, Hsing-I
學位類別：	碩士 Master
系所名稱：	工學院 - 資源工程學系 Department of Resources Engineering
論文出版年：	2017
畢業學年度：	105
語文別：	中文
論文頁數：	83
中文關鍵詞：	Fe-Si-Cr合金、硬脂酸、氧化鋁、PCA 、行星式球磨、退火、氧化、超晶格
外文關鍵詞：	Fe-Si-Cr alloy, PCA, planetary ball milling, oxidation, superlattice
相關次數：	點閱：140 下載：20
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本研究利用平均粒徑約180 nm的α-Al2O3以及硬脂酸(Stearic acid)做為過程添加劑(PCA)，將Fe-Si-Cr合金粉末置於行星式球磨中進行研磨處理以細化，其中利用SEM分析球磨過程中形貌的改變，結果顯示硬脂酸與氧化鋁兩者確實皆可充當PCA的角色，使研磨過程中冷焊情況不會發生，而氧化鋁的添加更使得研磨效率上升，Fe-Si-Cr粉末之平均粒徑自50 μm遞減至4 μm，且氧化鋁有絕緣包覆Fe-Si-Cr合金顆粒的效果。
研磨過後的Fe-Si-Cr合金粉末若直接進行氧化處理，會因大量差排存在，而使得大量氧化鐵的生成;故在N2/H2的氣氛下施予退火處理，從TEM分析中可確認退火處理可有效消除差排，且磁性質有回升的現象，此外，在退火過程會因鉻與矽的擴散速度不同而產生氧化鉻、氧化鋁、氧化矽的多層包覆結構。若經退火處理後施予再氧化程序，會因退火過程中已產生的超晶格DO3相，使得氧化矽與氧化鉻的生成受到抑制，生成易造成剝層的氧化鐵結構。

In this study, Fe-Si-Cr alloy powders were planetary ball milled by adding α-Al2O3 (particle size is about 180 nm) or stearic acid as the process control agent (PCA). The morphologies of the powders after milling were characterized by using SEM, and the results showed α-Al2O3 and stearic acid could indeed act as PCA because to reduce the occurrence of cold welding. Moreover, the addition of alumina can promote grinding efficiency of Fe-Si-Cr alloy powders leading to mean particle size decreased from 50 μm to about 4 μm.
The oxidation treatment of the planetary ball milled Fe-Si-Cr alloy powders resulted in a large amount of iron oxide formation due to the oxygen easily diffused along the dislocation and reacted with iron. Therefore, the annealing treatments were performed under N2/H2 atmosphere. The annealing process could effectively eliminate the dislocation based on the TEM results and hence the magnetic properties were improved. The multilayer coating structure consisting of chromium oxide, alumina and silicon oxide sequentially from the surface to the center was observed on the Fe-Si-Cr alloy powder surface during annealing due to the difference in outward diffusion rate of Fe, Si and Cr. The formation of silicon oxide and chromium oxide were inhibited and on the other hand iron oxide was formed during re-oxidation for the milled Fe-Si-Cr alloy powders due to the existence of DO3 superlattice phase after annealing process under N2/H2 atmosphere.

摘要 I
致謝 VIII
目錄 IX
表目錄 XIII
圖目錄 XIV
第一章  緒論 1
1-1前言 1
1-2研究目的 2
第二章  文獻回顧 4
2-1金屬功率電感器(Metal Power Inductor) 4
2-1-1金屬功率電感器之簡介 4
2-1-2金屬功率電感器之工作原理與特性 7
2-1-2-1電感器之工作原理 7
2-1-2-2電感之感抗 8
2-1-2-3電感之自我諧振頻率(SRF) 8
2-1-2-4電感之直流疊加特性 9
2-1-2-5磁性材料之初導磁係數 9
2-1-2-6磁損耗[15-21] 11
2-2軟磁材料簡介與鐵矽鉻合金之研究進展 14
2-2-1絕緣包覆鐵粉之研究進展 15
2-2-2鐵矽鉻合金之研究進展	17
2-3金屬機械合金化與研磨(Mechanical Alloying and Milling) 18
2-3-1機械合金法機制 19
2-3-2過程添加劑(Process Control Agent, PCA) 21
2-4退火(annealing) 23
第三章  實驗步驟與方法 25
3-1實驗藥品 25
3-1-1起始原料 25
3-1-2其餘原料 27
3-2實驗流程 27
3-2-1球磨Fe-Si-Cr合金之實驗流程 27
3-2-2添加硬脂酸(stearic acid)球磨鐵矽鉻合金之實驗流程圖 28
3-2-3添加氧化鋁於行星式球磨其實驗過程與Al2O3@FeSiCr製備之流程 29
3-2-4研磨後的樣品之熱處理流程 30
3-3實驗儀器簡介與樣品特性分析 32
3-3-1行星式高能球磨機 32
3-3-2X-ray繞射相鑑定(XRD)與殘留應變分析 32
3-3-3掃描式電子顯微鏡(SEM) 33
3-3-4穿透式電子顯微鏡(TEM) 34
3-3-5X-ray螢光成份分析(XRF) 34
3-3-6直流電阻率分析 34
3-3-7比表面積分析 35
3-3-8傅立葉轉換紅外線光譜分析(FTIR) 35
3-3-9磁性質分析 35
3-3-10視孔隙率之量測 35
3-3-11振實密度分析 35
3-4樣品代號 36
第四章  結果與討論 37
4-1不同的過程添加劑對Fe-Si-Cr粉末之研究 37
4-1-1未添加PCA對Fe-Si-Cr粉末於行星式球磨時之影響 37
4-1-2添加Stearic acid對Fe-Si-Cr粉末於行星式球磨時之影響 38
4-1-3添加Al2O3對Fe-Si-Cr粉末於行星式球磨時之影響 40
4-1-4Al2O3@FeSiCr之材料特性 42
4-1-4-1Al2O3@FeSiCr之XRD分析 42
4-1-4-2Al2O3@FeSiCr之SEM顯微結構分析 45
4-1-4-3Al2O3@FeSiCr之TEM顯微結構分析 47
4-1-4-4Al2O3@FeSiCr之FT-IR分析 49
4-1-4-5電阻率之分析 50
4-1-4-6初導磁係數之分析 51
4-2行星式球磨後的Fe-Si-Cr合金於不同氧化熱處理對其性質之影響 53
4-2-1行星式球磨後的Fe-Si-Cr合金氧化性質之探討 53
4-2-2Al2O3@FeSiCr於N2/H2環境下退火製程之探討 56
4-2-2-1Al2O3@FeSiCr退火製程之XRD分析 56
4-2-2-2Al2O3@FeSiCr退火製程之TEM分析 59
4-2-2-3Al2O3@FeSiCr退火製程之初導磁係數分析 62
4-2-3Al2O3@FeSiCr再氧化製程之探討 63
4-2-3-1Al2O3@FeSiCr再氧化製程之XRD分析 63
4-2-3-2Al2O3@FeSiCr再氧化製程之TEM分析 64
4-2-3-3Al2O3@FeSiCr再氧化製程之初導磁係數分析 66
4-3Al2O3@FeSiCr堆積密度之分析 67
第五章  結論 69
參考文獻	70
附錄 80

                                    

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