臺灣博碩士論文加值系統

本論文以多元醇法製備單分散之Ni、Ag、Co等金屬及其核殼型與合金型複合奈米粒子，並將其分散於高分子膠合劑中，探討其電磁波吸收特性。
關於金屬奈米粒子之製備，係於乙二醇溶液中，分別以聯氨與聚乙醯胺(PEI)為還原劑與保護劑，製得Ni、Ag、Co、Ni@Ag、Ni3Ag1、Ni1Ag1、Ni1Ag3、Co3Ag1、Co1Ag1、Co1Ag3、Co3Ni1、Co1Ni1、Co1Ni3、及CoNiAg等14種產品。其粒徑小且具單分散性，皆為面心立方體結構。且除Ag外，皆近乎超順磁。
關於電磁波吸收特性之研究，主要探討上述金屬奈米粒子在2-18GHz與18-40GHz兩個頻率範圍內反射損失及相關的介電係數與導磁係數。結果發現，Ag奈米粒子在兩個頻率範圍內皆無明顯的反射損失，而Co及Ni奈米粒子則僅分別於22.3 與31.8GHz有一最大反射損失。然而，Ni@Ag奈米粒子除了在31.5GHz處有一最大反射損失外，在10.8GHz處出現另一新的反射損失，展現雙頻電磁波吸收特性，推測可能是因核-殼界面在電磁場下產生之極化滯緩現象引發介電損失所致。又Ni1Ag1奈米粒子與Ni奈米粒子相似，僅有單頻吸收，但吸收頻率由31.8 GHz 位移到9.4GHz。Ni3Ag1與Ni1Ag3奈米粒子則與Ni@Ag奈米粒子相似，皆展現雙頻電磁波吸收特性。Ni3Ag1奈米粒子之最大反射損失於7.1與36.5GHz處出現，而Ni1Ag3奈米粒子則於7.7與30.3GHz處發生。推測NiAg合金奈米粒子中之Ni與Ag原子並未均勻分佈，可能有富鎳或富銀之微相分散於粒子內部，形成類似核殼型的微結構。因此在電磁場下，該微相結構之晶界會因極化滯緩現象而產生介電損失，故呈現雙頻電磁波吸收之特性。至於Ni1Ag1奈米粒子，可能因兩成份之比例相近，粒子內部可能較少有富鎳或富銀之微相產生，故僅有單頻吸收特性。
此外，CoAg與CoNi奈米粒子皆呈現單頻電磁波吸收特性，但吸收頻率則隨組成改變而不同。最大反射損失發生之頻率，Co3Ag1、Co1Ag1、Co1Ag3 、Co3Ni1、Co1Ni1、與Co1Ni3分別為8.7、16.2、12.1、12.1、15.8、與15.2GHz。推測CoAg與CoNi奈米粒子內部可能具有較佳的組成均勻性，故未如Ni1Ag3與Ni3Ag1奈米粒子般展現雙頻電磁波吸收特性。值得注意的，CoNiAg奈米粒子亦於12.2與30.7GHz呈現雙頻電磁波吸收之特性，顯示當Ni與Ag同時存在時，有較大的機會出現雙頻電磁波吸收現象。
據此可知，金屬奈米粒子之電磁波吸收頻率可藉由金屬種類及其合金組成的改變或核殼結構的建立加以調整，甚至可因微相結構的存在而展現雙頻吸收的特性。

This dissertation concerns the polyol synthesis of monodisperse Ni, Ag, Co, and their core-shell and alloy nanoparticles. Also, their electromagnetic (EM) wave absorption properties while embedded in a polymer matrix were studied.
For the synthesis of metal nanoparticles, they were synthesized in ethylene glycol with hydrazine and PEI as the reducing agent and protective agent, respectively. Fourteen kinds of metal nanoparticles were obtained, including Ni, Ag, Co, Ni@Ag, Ni3Ag1, Ni1Ag1, Ni1Ag3, Co3Ag1, Co1Ag1, Co1Ag3, Co3Ni1, Co1Ni1, Co1Ni3, and CoNiAg. They were all very small and monodisperse with a face-centered cubic (fcc) structure. Except Ag, they were nearly superparamagnetic.
For the study on the EM wave absorption properties, the reflection loss (RL) and the corresponding permittivity and permeability of the above metal nanoparticles in the frequency ranges of 2-18 GHz and 18-40 GHz were investigated. It was found that no significant EM wave absorption was observed for Ag nanoparticles in two frequency ranges examined. Co and Ni nanoparticles showed the maximum RL at 22.3 and 31.8 GHz, respectively. However, Ni@Ag nanoparticles not only remained a significant absorption at 31.5 GHz but also showed an additional absorption at 10.8 GHz, exhibiting a dual-frequency EM wave absorption property. The additional absorption of Ni@Ag nanoparticles at 10.8 GHz might be due to the lags of polarization between the core/shell interfaces as the frequency was varied, which contributed to the dielectric loss. Furthermore, both Ni3Ag1 and Ni1Ag3 nanoparticles exhibited a dual-frequency EM wave absorption property with the maximum RL at 7.1 and 36.5 GHz for Ni3Ag1 and 7.7 and 30.3 GHz for Ni1Ag3. It was suggested that the distribution of Ni and Ag atoms in the bulk phase of Ni3Ag1 and Ni1Ag3 nanoparticles might be inhomogeneous. Ni- and Ag-rich micro-domains might be formed, leading to the appearance of the second absorption due to the lags of polarization at the interfaces as the frequency was varied. As for the Ni1Ag1 nanoparticles, a single-frequency EM wave absorption was observed, probably due to the absence of Ni- and Ag-rich domains when Ag and Ni contents were similar.
In addition, CoAg and CoNi nanoparticles all exhibited a single-frequency EM wave absorption. The absorption frequency varied with the composition. The frequencies where the maximum RL occurred were 8.7, 16.2, 12.1, 12.1, 15.8, and 15.2 GHz for Co3Ag1, Co1Ag1, Co1Ag3 , Co3Ni1, Co1Ni1, and Co1Ni3, respectively. It was suggested that the compositions of CoAg and CoNi nanoparticles in the bulk phase were homogeneous. It was noted that CoNiAg nanoparticles also exhibited a dual-frequency EM wave absorption property at 12.2 and 30.7 GHz, revealing the simultaneous presence of Ni and Ag easily led to the dual-frequency EM wave absorption.
Accordingly, it could be concluded that the EM wave absorption frequency of metal nanoparticles could be tuned by changing the kind of metal nanoparticles and their alloy composition or core-shell structure. The presence of micro-phases might lead to the dual-frequency EM wave absorption.

中文摘要……………………………………………………………. I
英文摘要……………………………………………………………. III
誌謝…………………………………………………………………. V
總目錄………………………………………………………………. VI
表目錄………………………………………………………………. IX
圖目錄………………………………………………………………. X
符號…………………………………………………………………. XV

第一章 緒論………………………………………………………... 1
1.1 奈米材料與奈米技術………………………………………….. 1
1.1.1 奈米材料之定義與範疇………………………………….. 1
1.1.2 奈米材料之特性…………………………………………... 1
1.1.3 奈米材料之應用領域……………………………………... 11
1.1.4 奈米材料之製備…………………………………………... 13
1.1.4.1 奈米材料之製法簡介………………………………… 13
1.1.4.2 複合奈米粒子之製備………………………………… 17
1.2 電磁波抑制材料……………………………………………….. 23
1.2.1 前言………………………………………………………... 23
1.2.2 能量場的特性……………………………………………... 24
1.2.3 電磁波干擾/放射頻率干擾之簡介………………………. 27
1.2.3.1 產生來源與分類……………………………………… 27
1.2.3.2 電磁波干擾的管理法規……………………………… 32
1.2.4 遮蔽材與吸收材之特性…………………………………... 34
1.3 電磁波吸收材之製作與設計………………………………….. 39
1.4 導電性高分子塑膠之製備技術……………………………….. 41
1.5 研究動機……………………………………………………….. 42

第二章 理論部分…………………………………………………... 44
2.1 電磁波干擾/放射頻率干擾之遮蔽理論……………………… 44
2.2 微波吸收材之吸收原理……………………………………….. 51
2.3 微波反射損失之量測理論…………………………………….. 54
2.4 多元醇法……………………………………………………….. 57

第三章 實驗部分…………………………………………………... 59
3.1 藥品、儀器與材料…………………………………………….. 59
3.1.1 藥品………………………………………………………... 59
3.1.2 儀器………………………………………………………... 60
3.1.3 材料………………………………………………………... 61
3.2 多元醇法製備Ni@Ag複合奈米粒子之方法………………… 62
3.2.1 低濃度Ni@Ag複合奈米粒子……………………………. 62
3.2.2 高濃度Ni@Ag複合奈米粒子……………………………. 62
3.3 多元醇法製備合金奈米粒子之方法………………………….. 63
3.4 製備金屬奈米粒子複合膜之方法…………………………….. 65
3.5 特性分析……………………………………………………….. 66

第四章 結果與討論………………………………………………... 69
4.1 Ni@Ag奈米粒子之合成與電磁波吸收特性…………………. 69
4.1.1 鎳奈米粒子之基本物性…………………………………... 69
4.1.2 Ni@Ag奈米粒子之基本物性…………………………….. 71
4.1.3 Ni@Ag奈米粒子複合膜之電磁波吸收特性…………….. 86
4.2 NiAg合金奈米粒子之合成與電磁波吸收特性………………. 93
4.2.1 NiAg合金奈米粒子之基本物性………………………….. 93
4.2.2 NiAg奈米粒子複合膜之電磁波吸收特性………………. 101
4.3 CoAg合金奈米粒子之合成與電磁波吸收特性……………… 110
4.3.1 CoAg合金奈米粒子之基本物性…………………………. 110
4.3.2 CoAg奈米粒子複合膜之電磁波吸收特性………………. 118
4.4 CoNi合金奈米粒子之合成與電磁波吸收特性………………. 127
4.4.1 CoNi合金奈米粒子之基本物性………………………….. 127
4.4.2 CoNi奈米粒子複合膜之電磁波吸收特性………………. 134
4.5 CoNiAg合金奈米粒子之合成與電磁波吸收特性…………… 142
4.5.1 CoNiAg合金奈米粒子之基本物性………………………. 142
4.5.2 CoNiAg奈米粒子複合膜之電磁波吸收特性……………. 146

第五章 結論………………………………………………………... 152

參考文獻……………………………………………………………. 156

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