臺灣博碩士論文加值系統

本研究將鐵鎳粉末由聚矽氮烷(PSZ)處理，於不同溫度與氣體熱處理後探討界面結構對磁性之影響。先以PSZ在鐵鎳上水解羥基為起始劑，經過模壓後加熱縮合，硬化形成界面阻絕層，接著在700°C與1100°C的氮氣與空氣中熱裂解，對最終混成複合材料界面結構的化學結構、型態觀察、磁性分析影響進行探討。
傅立葉轉換紅外光譜儀(FTIR)觀測PSZ水解縮合變化，以及不同溫度與氣體熱裂解下PSZ化學結構的差異，進一步用化學分析影像能譜儀(XPS)分析矽與氧原子的鍵結。掃描式電子顯微鏡(SEM)觀察表面型態，並使用能量散佈能譜儀(EDX)進行表面分析，探討熱處理後元素的變化。以X光繞射儀(XRD)顯示樣品熱處理後鐵鎳原子的排列狀態。從超導量子干涉磁量儀(SQUID)，探討熱處理後飽和磁化量與矯頑力，並使用阻抗分析儀(LCR)量測1~100MHz下電感特性。最後量測熱裂解PmPSZ之體積電阻、包覆前後之腐蝕效應與結晶型態，比較有無PSZ界面對鐵鎳粉末熱處理的差異。
量測結果顯示，低黏度之PSZ分散於鐵鎳粉末中，水解後黏度上升能使鐵鎳粉末塑形，在界面上熱縮合形成網狀烷氧基矽化合物(alkoxysilane)改質金屬表面，包覆性隨著溫度上升與SiO2之析出而下降。在改質過之界面完整情況下，PmPSZ之磁性與矯頑力(Coercivity)隨溫度上升而增加，複合材料PmPSZ最大導磁率介於10~20MHz之間，於700/N2下熱處理可以使最大導磁率提高14%，飽和磁化量維持在95%以上。

In this study, polysilazane(PSZ) was applied as polymer-derived ceramic (PDC) within NiFe(Pm) particles. The PmPSZ composites were modifying by controlled water hydrolysis to form interface capable of molding magnetic powder under 180°C. Different atmosphere, from nitrogen and air had been preparing for heat treatment at 700°C and 1100°C respectively.
Spectroscopic techniques from XPS and FTIR have identified chemical exchanges during condensation and pyrolysis. The results from XRD and SEM show the crystallization behavior and the morphology of interface. And the ultimate magnetic properties of the metal-ceramic composites have been measured by SQUID and LCR.
The results suggest an alkylsiloxane network interface could be derived after hydrolysis condensation by PSZ. The coverage networks provide insulator and corrosion resistance layers for NiFe during high temperature but are influenced by the atmosphere. By controlling the atmosphere and heat treatment temperature, it is possible to enhance the magnetic properties of PmPSZ composites. According to the analysis of LCR meter, PmPSZ composites have the maximum permeability within 10~20MHz. After the 700°C/N2 heat treatment process, the maximum value rises up 14%.

摘要 I
Abstract III
致謝 V
目錄 VI
圖目錄 IX
表目錄 XI
第1章 緒論 1
1.1 前言 1
1.2 研究背景 1
1.3 研究方法 3
第2章 文獻回顧 4
2.1 磁性材料 4
2.1.1 磁性材料種類 4
2.1.2 軟磁材料 7
2.1.3 鐵鎳合金 10
2.2 磁性複合材料 11
2.2.1 矽基鐵磁複合材料 14
2.3 矽氮結構 15
2.3.1 矽化合物 15
2.3.2 聚矽氮烷 16
2.3.3 有機聚矽氮烷 18
2.3.4 溶膠-凝膠法 21
第3章 實驗方法 24
3.1 樣品製作 24
3.2 實驗架構 26
3.3 實驗 27
3.3.1 熱重損失分析儀(TGA) 27
3.3.2 阻抗分析儀(LCR) 28
3.3.3 傅立葉轉換紅外線光譜儀(FTIR) 29
3.3.4 掃描式電子顯微鏡(SEM) 30
3.3.5 光繞射儀(XRD) 31
3.3.6 化學分析影像能譜儀(XPS) 32
3.3.7 超導量子干涉磁量儀(SQUID) 33
第4章 結果與討論 34
4.1 PSZ硬化分析 34
4.1.1 熱重分析 34
4.2 化學鍵結分析 36
4.2.1 FTIR 36
4.2.2 XPS 40
4.3 微結構分析 45
4.3.1 XRD 45
4.3.2 SEM 48
4.4 磁性分析 53
4.4.1 阻抗分析儀 53
4.4.2 SQUID 56
第5章 結論 59
參考文獻 60

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