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研究生： 劉俊呈
論文名稱： NiMnInX變磁形狀記憶合金之研究
指導教授： 胡塵滌
口試委員: 胡塵滌
楊聰仁
吳錫侃
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2014
畢業學年度： 102
語文別： 中文
論文頁數： 97
中文關鍵詞： 形狀記憶合金 、變磁性效應 、相變化溫度 、微結構
相關次數： 點閱：2  下載：0 
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    • 鐵磁性記憶合金的變磁性效應為施加磁場時，合金的相變化溫度隨之改變，可導致磁場誘發逆麻田散相變化。本研究在Ni50Mn36In14中以Ni置換Mn或以Au、Fe、Co取代Ni製作三元及四元合金塊材，探討NiMnInX特性包括：相變化溫度、微結構、變磁性效應、磁致伸縮。
    將各種合金做1173K 24小時熱處理並水淬後，所得到的合金母相晶格皆為L21，麻田散相為10M或14M。
    合金中以Ni置換Mn將產生Ni3In析出相。以Au取代Ni合金母相晶格常數上升。以Fe取代Ni將產生-Fe析出。
    以Au、Fe取代Ni使相變化溫度及熱焓值下降；以Co取代Ni使相變化溫度大幅上升，且熱焓值亦上升，由變溫金相觀測得知熱焓值越高，麻田散相變化驅動力越大。
    以Fe取代Ni使居禮溫度上升，並且母相與麻田散相磁化量差異變大，有明顯之變磁性效應。以Co取代Ni，母相與麻田散相磁化量差異亦變大，有變磁性效應。磁場下相變化溫度改變量之實驗值與計算值趨勢相符。其中Ingot #5試片在50kOe磁場下相變化溫度改變量高達35K。
    從應變規量測證實Ingot #2、#3、#7與#8均有變磁性效應。磁致伸縮雖證實各合金本身磁致伸縮值不高，但以Fe取代Ni使合金磁致伸縮值上升，並且居禮溫度隨Fe比例增加而上升。

    目錄 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.......................................................................................................... 3 2-1 鐵磁性形狀記憶合金 .................................................................................... 3 2-2 傳統形狀記憶效應 ........................................................................................ 3 2-3 磁伸縮[20, 21] .................................................................................................... 5 2-4 鐵磁性形狀記憶效應 .................................................................................... 6 2-5 變磁性形狀記憶合金 .................................................................................... 8 2-6 變磁性形狀記憶效應 .................................................................................... 9 2-7 變磁性形狀記憶合金應用 .......................................................................... 10 2-8 NiMnX變磁性形狀記憶合金文獻回顧 ...................................................... 11 2-9 NiMnX合金添加第四元素文獻回顧 .......................................................... 12 2-9-1 添加Co ............................................................................................. 13 2-9-2 添加Fe .............................................................................................. 13 2-9-3 添加Cu ............................................................................................. 14 2-9-4 添加Ga ............................................................................................. 15 2-9-5 添加Ge ............................................................................................. 15 2-10 相變化溫度改變量實驗值與計算值文獻回顧 ........................................ 16 2-11 變磁性效應文獻回顧 ................................................................................ 16 第三章 實驗步驟及方法............................................................................................ 27 3-1 試片製備 ...................................................................................................... 27 3-2 合金鑄錠熔煉 .............................................................................................. 28 3-2-1 真空均質化熱處理(Homogenized Heat Treatment in vacuum) ...... 29 3-2-2 真空退火處理(Annealing in vacuum) .............................................. 29 3-3 成份分析 ...................................................................................................... 29 3-4 熱示差掃描卡量計量測(Differential Scanning Calorimetry) ..................... 29 3-5 結構分析及觀察 .......................................................................................... 30 3-5-1 室溫X-ray繞射分析........................................................................ 30 3-5-2 光學顯微鏡(Optical Microscope , OM)顯微結構觀察 ................... 31 3-6 磁性質量測 .................................................................................................. 31 3-7 磁伸縮量測 .................................................................................................. 32 3-8 溫度誘發應變量測 (Strain Gauge Method) ............................................... 34 3-9 儀器與量測原理 .......................................................................................... 34 3-9-1 X光繞射儀 (X-Ray Diffractometer) ................................................ 34 3-9-2 熱示差掃描卡量計 (Differential Scanning Calorimetry)[61] ........... 35 3-9-3 超導量子干涉儀(Superconducting Quantum Interference Devices, SQUID) ........................................................................................................ 35 3-9-4 應變規(Strain Gauge) ....................................................................... 35 第四章 結果與討論.................................................................................................... 37 4-1 試片代號介紹 .............................................................................................. 37 4-2 試片基本性質研究 ...................................................................................... 37 4-2-1 ICP-MS (Inductively Coupled Plasma Mass Spectrometry)成分分析...................................................................................................................... 37 4-2-2 室溫 X-Ray 繞射分析 .................................................................... 38 4-2-3 晶格常數討論 ................................................................................... 43 4-2-4 光學顯微鏡室溫金相觀察 ............................................................... 44 4-2-5 光學顯微鏡變溫金相觀察 ............................................................... 47 4-2-6 DSC熱分析 ....................................................................................... 54 4-2-7 無磁場相變化溫度探討 ................................................................... 61 4-3 磁性質研究 .................................................................................................. 63 4-3-1 磁場下溫度誘發應變 (Strain Gauge Method) ................................ 63 4-3-2 磁通量研究 (SQUID Method)......................................................... 68 4-3-3 磁化量對溫度循環研究 (SQUID Method)..................................... 71 4-3-4 磁致伸縮研究 ................................................................................... 79 第五章 結論................................................................................................................ 87 第六章 參考文獻........................................................................................................ 89 圖目錄 圖 2-1 形狀記憶合金之形狀記憶效應示意圖 .................................................... 18 圖 2-2 CuAlNi合金熱彈性型麻田散體經冷卻、加熱所致的成長、收縮之光學顯微鏡照片[17] ......................................................................................................... 18 圖 2-3單向&雙向形狀記憶效應示意圖 .............................................................. 19 圖 2-4 磁致伸縮現象之示意圖[21] ....................................................................... 19 圖 2-5 磁伸縮與磁化機制示意圖[21] ................................................................... 20 圖 2-6 磁伸縮量測示意圖[56] ............................................................................... 20 圖 2-7 鐵磁性形狀記憶效應示意圖[57] ............................................................... 20 圖 2-8 (a)磁伸縮與(b)鐵磁性形狀記憶效應的比較[22] ....................................... 21 圖 2-9曲線270 K與290 K呈現變磁性轉換行為[11] ......................................... 21 圖 2-10 傳統形狀記憶效應與變磁性形狀記憶效應示意圖 .............................. 22 圖 2-11 NiMnX合金施加磁場對相變化溫度的影響[58] ..................................... 22 圖 2-12 NiMnX((a)X=Sn, (b)X=In)合金之居禮溫度、麻田散相變化溫度與e/a ratio之關係示意圖[30] ............................................................................................ 23 圖 2-13 Ni-Mn基修士勒合金相變化溫度與e/a ratio關係示意圖[31] ............... 23 圖 2-14 L21結構示意圖[34] .................................................................................... 24 圖 2-15 NiMnIn與NiCoMnIn合金居禮溫度與相變化溫度示意圖[34] ............. 24 圖 2-16 文獻相變化溫度改變整理([a]Ni50Mn25Ga25[55]；[b]Ni50.3Mn33.8In15.9[28]；[c]Ni45Co5Mn36.6In13.4[11]；[d]Ni45Co5Mn36.7In13.3[53]；[e]Ni51Mn33In16[54]；[f]Ni41Co9Mn39Sb11[40]；[g]Ni43Co7Mn39Sn11[37]) ................................................... 26 圖 2-17 圖 2-16各合金成分相圖(Ni41Co9Mn39Sb11與Ni43Co7Mn39Sn11重疊)26 圖 3-1實驗流程簡介 ............................................................................................. 27 圖 3-2真空電弧熔煉系統裝置示意圖 ................................................................. 28 圖 3-3 DSC200F3熱式差掃描卡量計 .................................................................. 30 圖 3-4 Shimadzu XRD-6000繞射儀[59]................................................................. 31 圖 3-5超導量子干涉儀(Superconducting Quantum Interference Device Magnetomer, SQUID)[60] ......................................................................................... 32 圖 3-6磁伸縮量測電路裝置示意圖 ..................................................................... 33 圖 3-7磁致伸縮量測載具 ..................................................................................... 33 圖 3-8溫度誘發應變量測示意圖 ......................................................................... 34 圖 3-9 應變規主要構造圖 .................................................................................... 36 圖 3-10 金屬導線受拉力後彈性應變圖[62] ......................................................... 36 圖 4-1 Ingot #1室溫X-ray繞射圖譜 ................................................................... 39 圖 4-2 Ingot #2室溫X-ray繞射圖譜 ................................................................... 40 圖 4-3 Ingot #3室溫X-ray繞射圖譜 ................................................................... 40 圖 4-4 Ingot #4室溫X-ray繞射圖譜 ................................................................... 41 圖 4-5 Ingot #5室溫X-ray繞射圖譜 ................................................................... 41 圖 4-6 Ingot #6室溫X-ray繞射圖譜 ................................................................... 42 圖 4-7 Ingot #7室溫X-ray繞射圖譜 ................................................................... 42 圖 4-8 Ingot #8室溫X-ray繞射圖譜 ................................................................... 43 圖 4-9 Ingot #1室溫金相(a：放大倍率200；b：放大倍率500) ...................... 45 圖 4-10 Ingot #2室溫金相(a：放大倍率100；b：放大倍率200) .................... 45 圖 4-11 Ingot #3室溫金相(a：放大倍率100；b：放大倍率200) .................... 45 圖 4-12 Ingot #4室溫金相(a：放大倍率100；b：放大倍率200) .................... 46 圖 4-13 Ingot #5室溫金相(a：放大倍率200；b：放大倍率500) .................... 46 圖 4-14 Ingot #6室溫金相(a：放大倍率200；b：放大倍率500) .................... 46 圖 4-15 Ingot #7室溫金相(a：放大倍率100；b：放大倍率200) .................... 47 圖 4-16 Ingot #8室溫金相(a：放大倍率100；b：放大倍率200) .................... 47 圖 4-17 光學顯微鏡下Ingot #1試片升降溫觀察(放大倍率：200) .................. 49 圖 4-18 光學顯微鏡下Ingot #2試片升降溫觀察(放大倍率：100) .................. 50 圖 4-19 光學顯微鏡下Ingot #3試片升降溫觀察(放大倍率：100) .................. 51 圖 4-20 光學顯微鏡下Ingot #7試片升降溫觀察(放大倍率：200) .................. 52 圖 4-21 光學顯微鏡下Ingot #8試片升降溫觀察(放大倍率：200) .................. 53 圖 4-22 Ingot #1 DSC熱分析圖............................................................................ 55 圖 4-23 Ingot #2 DSC熱分析圖............................................................................ 56 圖 4-24 Ingot #3 DSC熱分析圖............................................................................ 56 圖 4-25 Ingot #4 DSC熱分析圖............................................................................ 57 圖 4-26 Ingot #5 DSC熱分析圖............................................................................ 57 圖 4-27 Ingot #6 DSC熱分析圖............................................................................ 58 圖 4-28 Ingot #7 DSC熱分析圖............................................................................ 58 圖 4-29 Ingot #8 DSC熱分析圖............................................................................ 59 圖 4-30 相變化起始溫度(Ms)對應合金成分3D投影圖 .................................... 59 圖 4-31 相變化溫度與價電子體積密度n(nm-3)關係圖 ..................................... 62 圖 4-32 Ingot #2 應變對應溫度關係圖 ............................................................... 64 圖 4-33 Ingot #3 應變對應溫度關係圖 ............................................................... 64 圖 4-34 Ingot #7 應變對應溫度關係圖 ............................................................... 65 圖 4-35 Ingot #8 應變對應溫度關係圖 ............................................................... 65 圖 4-36 Ingot #2 0.5kOe、2kOe、4kOe、10kOe之磁化量對溫度曲線 ............ 66 圖 4-37 Ingot #3 0.5kOe、2kOe、4kOe、10kOe之磁化量對溫度曲線 ............ 66 圖 4-38 Ingot #8 0.5kOe、2kOe、4kOe、10kOe之磁化量對溫度曲線 ............ 67 圖 4-39 應變規量測之相變化溫度改變量實驗值與計算值比較 (a：Ingot #2，b：Ingot #3，c：Ingot #7，d：Ingot #8) ..................................... 67 圖 4-40 Ingot #1 275K磁通量對磁場變化曲線圖(As=276.6K) .......................... 69 圖 4-41 Ingot #2 295K磁通量對磁場變化曲線圖(As=295.1K) .......................... 69 圖 4-42 Ingot #3 285K磁通量對磁場變化曲線圖(As=287.9K) .......................... 70 圖 4-43 Ingot #5 200K磁通量對磁場變化曲線圖(As=197.7K) .......................... 70 圖 4-44 Ingot #8 340K磁通量對磁場變化曲線圖(As=340.1K) .......................... 71 圖 4-45 Ingot #1 0.5kOe、10kOe、50kOe之磁化量對溫度曲線 ...................... 74 圖 4-46 Ingot #2 0.5kOe、10kOe、50kOe之磁化量對溫度曲線 ...................... 74 圖 4-47 Ingot #3 0.5kOe、10kOe、50kOe之磁化量對溫度曲線 ...................... 75 圖 4-48 Ingot #5 0.5kOe、10kOe、50kOe之磁化量對溫度曲線 ...................... 75 圖 4-49 Ingot #6 0.5kOe、10kOe之磁化量對溫度曲線 ..................................... 76 圖 4-50 Ingot #7 0.5kOe、50kOe之磁化量對溫度曲線 ..................................... 76 圖 4-51 Ingot #8 0.5kOe、10kOe、50kOe之磁化量對溫度曲線 (小圖為高溫區域放大圖) ...................................................................................... 77 圖 4-52 SQUID量測之相變化溫度改變量實驗值與計算值比較(a：Ingot #1，b：Ingot #2，c：Ingot #3，d：Ingot #5，e：Ingot #8) ............................................ 78 圖 4-53 Ingot #1~#3、#5、#8相變化溫度改變量與文獻數值比較3D投影圖([a]Ni50.3Mn33.8In15.9[28]；[b]Ni45Co5Mn36.7In13.3[53]；[c]Ni51Mn33In16[54]) ............. 79 圖 4-54 (a)磁場沿不同方向施加示意圖；(b)特製夾具示意圖 .......................... 81 圖 4-55 Ingot #1試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 82 圖 4-56 Ingot #2試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 82 圖 4-57 Ingot #3試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 83 圖 4-58 Ingot #4試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 83 圖 4-59 Ingot #5試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 84 圖 4-60 Ingot #6試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係 與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 84 圖 4-61 Ingot #7試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 85 圖 4-62 Ingot #8試片室溫下(a)~(c)x、y、z方向磁致伸縮值對外加磁場關係圖與 (d)飽和磁致伸縮值對外加磁場關係圖 .................................................... 85 圖 4-63 Ni50Mn25+xIn25-x合金溫度(T)對應價電子原子濃度(e/a)關係圖，圖中列出母相與麻田散相之居禮溫度及合金相變化溫度(Ms)[66] ................................. 86 表目錄 表 2-1 NiMnX合金M、S、相變化溫度改變量計算值與實驗值比較 ......... 25 表 4-1 試片 ICP-MS 成分分析結果 .................................................................. 38 表 4-2 試片之母相晶格常數(a0)、母相單位晶格體積(V) ................................ 44 表 4-3 DSC量測之試片相變化溫度、熱焓值及居禮溫度 ................................ 55 表 4-4 不同檢定方法之相變化溫度比較 ............................................................ 60 表 4-5 試片之母相晶格常數(a0)、母相單位晶格體積(V)、相變化溫度(Ms, Mf, As, Af)、價電子原子濃度比(e/a)及價電子體積密度n(nm-3) .............................. 62 表 4-6 M-T曲線 (0.5kOe) 量測之試片相變化溫度(Ms、Mf、As、Af)、 、 ................................................................................................................................. 77

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