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研究生： 林偉恩
Lin, Wei-En
論文名稱： CoFe0.5-2.5MnTi0.5-2.5VZr與AlMgNi0.3-1.0TiZr 高熵儲氫合金之研究
Hydrogen Storage in CoFe0.5-2.5MnTi0.5-2.5VZr and AlMgNi0.3-1.0TiZr High-Entropy Alloys
指導教授： 陳瑞凱
Chen, Swe-Kai
葉均蔚
Yeh, Jien-Wei
口試委員:
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： 2009
畢業學年度： 97
語文別： 中文
論文頁數： 158
中文關鍵詞： 儲氫高熵合金 、CoFexMnTiyVZr & AlMgNiwTiZr 、非晶化抑制元素 、PCI 、C14 Laves相 、介金屬化合物
外文關鍵詞： Hydrogen-storage high-entropy alloys, CoFexMnTiyVZr &, amorphization inhibitor, PCI, C14 Laves phase, Intermetallics
相關次數： 點閱：1  下載：0 
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    • 本研究第一部份以等莫耳CoFeMnTiVZr多元高熵合金為基礎，以Fe與Ti變量 (Fex及Tiy合金) 作元素改質及溫度改變，以探討真空電弧熔煉鑄造態非等莫耳合金CoFexMnTiyVZr (簡稱E6合金) 的吸放氫行為。第二部份以創新的等莫耳含鎂AlMgNiTiZr高熵合金為基礎，以Ni變量作元素改質及溫度改變，探討輕型機械合金化AlMgNiwTiZr高熵合金 (簡稱E5合金) 的吸放氫行為。先以X光繞射儀分析晶體結構，掃描電鏡分析微結構，EDS測定合金組成，DSC量測金屬氫化物的放氫溫度，再以PCI及動力曲線，量測E5及E6合金吸放氫行為。
    重要結論如下: 鑄造態E6合金，最大儲氫量約2 wt%，平台壓集中在1 - 5 atm之間，t0.9 (達到最大儲氫量百分之九十所需的時間) 約在100秒以內，遲滯值約在1以內，晶粒大小吸氫前分布在17.1 nm - 50.3 nm，吸氫後分布在14.8 nm - 46.1 nm，體積膨脹率約在3 %以內，晶體結構主要為C14 Laves相，元素過度添加，皆有元素態析出，熱力學分析顯示，E6合金分布趨勢與AB2型合金相似。機械合金化E5合金，球磨八小時即已合金化，各元素分布均勻，最大儲氫量約1.5 wt%，動力學達飽和儲氫量時間較長、t0.9約10,000秒，平台壓分布於5 - 12 atm之間，晶體結構由數種介金屬化合物所構成，球磨時間越長以及Ni含量減少，越容易發生非晶結構，因此Ni在E5合金內為非晶化抑制元素。

    The first part of this study investigates behavior of hydrogen absorption and desorption of non-equal-molar vacuum-arc-remelted as-cast CoFexMnTiyVZr (E6 alloys) based on their equal-molar counterpart by varying x (Fex alloys) and y (Tiy alloys) contents as well as measuring temperature. The second part does the same things as the first part but only changing the alloys to mechanical-alloying (MA) light-weighted AlMgNiwTiZr (E5 alloys). Experiments include XRD, SEM, EDS, DSC, PCI, and kinetics of hydrogen absorption and desorption for determination of crystal structure, microstructure, phase composition, hydrogen desorption temperature, and behavior of hydrogen absorption and desorption of E6 and E5 alloys, respectively.
    Primary conclusions are summarized as follows: The as-cast E6 alloys possess maximal hydrogen storage capacity of 2 wt %, plateau pressure in PCIs of 1 – 5 atm, time to 90 % of maximal capacity, t0.9, of about 100 s, values of hysteresis of less than 1, grain size before and after hydrogen absorption cycle of 17.1 nm - 50.3 nm, and 14.8 nm - 46.1 nm, respectively, volume expansion mostly of less than 3 %, crystal structure of C14 Laves phase for both before and after cycle states, elemental precipitation for excessive addition of Fe and Ti, and similar distribution as the AB2 alloys in the thermodynamic ΔH vs. (H/M)max plot. MA-E5 alloys have become alloys after 8-h MA with homogeneous distribution of composition, and possess maximal hydrogen storage capacity of 1.5 wt %, plateau pressure in PCIs of 5 – 12 atm, t0.9 of about 10,000 s, crystal structure composed of several intermetallics, property of easy amorphization for prolonged MA and for alloys containing less amount of Ni. Therefore Ni is an amorphization inhibitor in E5 alloys.

    頁次 摘要 --------------------------------------------------------------------------------------------I Abstract ----------------------------------------------------------------------------------------II 目錄 -------------------------------------------------------------------------------------------III 圖目錄 ---------------------------------------------------------------------------------------VI 表目錄 -------------------------------------------------------------------------------------XIII Chapter 1: 前言 1 1-1 簡介---------------------------------------------------------------------------------------1 Chapter 2: 文獻回顧與基礎理論 5 2-1 儲氫合金的簡史與應用 -------------------------------------------------------5 2-2 各種儲氫材料的簡介 -----------------------------------------------------------8 2-2-1 金屬氫化物 -------------------------------------------------------------11 2-2-2 複合氫化物 -------------------------------------------------------------14 2-2-3 有基金屬骨架 (MOFs) -----------------------------------------------16 2-2-4 奈米管與碳材 ---------------------------------------------------------20 2-2-5 儲氫金屬氫化物薄膜 ----------------------------------------------21 2-3 各種儲氫合金簡介 ------------------------------------------------------------ 22 2-3-1 AB5 Type -------------------------------------------------------------------22 2-3-2 AB2 Type -------------------------------------------------------------------23 2-3-3 AB Type ---------------------------------------------------------------------25 2-3-4 A2B Type -------------------------------------------------------------------26 2-3-5 AB3 Type -------------------------------------------------------------------27 2-3-6 Other Type -----------------------------------------------------------------29 2-4 表面活化 --------------------------------------------------------------------------- 32 2-5 動力學曲線 ----------------------------------------------------------------------- 35 2-6 PCI曲線 --------------------------------------------------------------------------------38 2-7 van’t Hoff plot -------------------------------------------------------------------- 40 2-8 遲滯效應 --------------------------------------------------------------------------- 41 2-9 Laves phase 特性 ------------------------------------------------------------------43 2-10 Mg型儲氫材料及複合型儲氫材料的特性 ------------------------ 45 2-11 高熵合金 ---------------------------------------------------------------------------48 2-12 機械合金法 -----------------------------------------------------------------------52 Chapter 3: 實驗步驟與方法 54 3-1 過渡金屬型合金設計 -------------------------------------------------------- 54 3-2 輕型合金設計 ------------------------------------------------------------------- 54 3-3 過渡金屬型合金製備 -------------------------------------------------------- 55 3-4 過渡金屬型合金粉末製備 ------------------------------------------------- 56 3-5 輕型合金粉末製備 ------------------------------------------------------------ 56 3-6 試片活化、動力學曲線與PCI曲線 --------------------------------------56 3-6-1 試片活化 --------------------------------------------------------------- 57 3-6-2 動力曲線 -----------------------------------------------------------------59 3-6-3 PCI曲線 ------------------------------------------------------------------- 60 3-7 XRD分析 ------------------------------------------------------------------------------61 3-8 SEM分析 ------------------------------------------------------------------------------61 3-9 DSC分析 ------------------------------------------------------------------------------61 Chapter 4: 結果與討論 62 4-1 CoFeMnTiyVZr 與 CoFexMnTiVZr 合金SEM、EDS與Mapping分-----62 4-2 CoFeMnTiyVZr 與 CoFexMnTiVZr 合金動力學曲線分析 ------------83 4-3 CoFeMnTiyVZr 與 CoFexMnTiVZr 合金PCI曲線分析 -------------------91 4-4 CoFeMnTiyVZr 與 CoFexMnTiVZr 合金XRD晶體結構分析 --------100 4-5 CoFeMnTiyVZr 與 CoFexMnTiVZr 合金DSC熱性質分析 ------------117 4-6 AlMgNiwTiZr 合金SEM / EDS 分析 ----------------------------------------120 4-7 AlMgNiwTiZr 合金動力學曲線分析 -------------------------------------128 4-8 AlMgNiwTiZr 合金PCI曲線分析 --------------------------------------------131 4-9 AlMgNiwTiZr 合金XRD晶體結構分析 ---------------------------------- 133 4-10 AlMgNiwTiZr 合金DSC熱性質分析 ------------------------------------ 137 4-11 CoFeMnTiyVZr、CoFexMnTiVZr與AlMgNiwTiZr 合金熱力學分--140 Chapter 5: 結論 -----------------------------------------------------------------------149 Chapter 6: References -----------------------------------------------------------------154 圖目錄 頁次 圖1-1 儲氫材料發展趨勢 -----------------------------------------------------------3 圖2-1 裝同樣四公斤的氫氣所需不同儲氫材料的體積相對於汽車示意圖 ------------------------------------------------------------------------------------7 圖2-2 元素及其氫化物資料表 (含儲氫量 wt%)----------------------------8 圖2-3 各種金屬氫化物的van’t Hoff line -------------------------------------9 圖2-4 儲氫材料家族譜 ------------------------------------------------------------ 11 圖2-5 氫原子在四面體與八面體格隙位置圖 ---------------------------12 圖2-6 儲氫合金形成示意圖 -----------------------------------------------------12 圖2-7 金屬氫化物ΔH比較圖 ----------------------------------------------------13 圖2-8 多種複合氫化物儲氫量比較圖 ------------------------------------- 14 圖2-9 NaAlH4系列的van’t Hoff plot ------------------------------------------ 15 圖2-10 多種孔隙型材料儲氫量與表面積示意圖 ----------------------17 圖2-11 MOF-5 結構圖 ----------------------------------------------------------------17 圖2-12 MOF-5於78 K儲氫示意圖 ------------------------------------------------18 圖2-13 MOF-5於室溫下儲氫示意圖 -------------------------------------------18 圖2-14 MOF-5於78 K儲氮示意圖 ------------------------------------------------19 圖2-15 多種製程奈米碳管動力學比較圖 ---------------------------------21 圖2-16 LaNi5與LaNi5H6結構圖-----------------------------------------------------22 圖2-17 AB5型儲氫合金的van’t‭ ‬Hoff plot -----------------------------------23 圖2-18 C14與C15 Laves phase ------------------------------------------------------24 圖2-19 AB2型儲氫合金的van’t Hoff plot -----------------------------------25 圖2-20 TiFe與TiFeH2結構圖 ---------------------------------------------------------26 圖2-21 Mg2Ni與Mg2NiD3.9吸放氫前後結構圖 ----------------------------27 圖2-22 PuNi3 AB3型合金晶體結構 ---------------------------------------------28 圖2-23 M. Martin利用吸氫動力曲線所推算的儲氫機制 ------------36 圖2-24 K. C. Chou預測動力曲線的模型 -------------------------------------36 圖2-25 反應分率F (The reacted fraction) 與Hydrogen absorption rate關係圖 ------------------------------------------------------------------------------------------37 圖2-26 合金在不同材質Chamber下的吸氫量與速率常數關係圖37 圖2-27 實際PCI曲線與簡單合金吸放氫像變化流程圖 --------------38 圖2-28 PCI曲線與van’t Hoff plot ------------------------------------------------40 圖2-29 C14與C15 AB2 Laves phase結構圖 ----------------------------------- 43 圖2-30 ZrMn2合金吸放氫前後XRD圖 ---------------------------------------- 44 圖2-31 MgH2及Mg2NiH4放氫DSC圖 ------------------------------------------- 45 圖2-32 不同晶粒大小Mg動力學曲線比較 ------------------------------- 46 圖2-33 Pd催化劑對Mg吸氫動力曲線影響 ---------------------------------46 圖2-34 Mg球磨的有無於350oC PCI 比較 ------------------------------------47 圖2-35 NaAlH4催化劑的有無對放氫動力學的影響 -------------------47 圖2-36 高熵合金熱力學分析圖 ------------------------------------------------50 圖2-37 緩慢擴散示意圖 -----------------------------------------------------------50 圖2-38 高熵合金與傳統合金導熱度比較示意圖 ----------------------51 圖2-39 機械合金法原理: A: 脆裂 B: 冷焊 ---------------------------------53 圖2-40 機械合金粉末粒徑與球磨時間關係圖 --------------------------53 圖3-1 本研究實驗流程圖 -------------------------------------------------------- 54 圖3-2 真空電弧熔煉爐 ------------------------------------------------------------ 55 圖3-3 活化條件與流程 ------------------------------------------------------------ 58 圖3-4 上: 試片腔體說明圖 下: 儲氫設備示意圖 ----------------------59 圖4-1 CoFeMnTi0.5VZr 粉末的500倍金相與EDS分析 --------------------65 圖4-2 CoFeMnTi0.5VZr 塊材的500倍金相與EDS分析 --------------------66 圖4-3 CoFeMnTiVZr 粉末的500倍金相與EDS分析 -------------------------66 圖4-4 CoFeMnTiVZr 塊材的500倍金相與EDS分析 -------------------------67 圖4-5 CoFeMnTi1.5VZr 粉末的500倍金相與EDS分析 --------------------67 圖4-6 CoFeMnTi1.5VZr 塊材的500倍金相與EDS分析 --------------------68 圖4-7 CoFeMnTi2VZr 粉末的500倍金相與EDS分析 -----------------------68 圖4-8 CoFeMnTi2VZr 塊材的500倍金相與EDS分析 -----------------------69 圖4-9 CoFeMnTi2.5VZr 粉末的500倍金相與EDS分析 --------------------69 圖4-10 CoFeMnTi2.5VZr 塊材的500倍金相與EDS分析 ----------------- 70 圖4-11 CoFeMnTi0.5VZr 塊材的500倍Mapping ------------------------------70 圖4-12 CoFeMnTiVZr 塊材的500倍Mapping ---------------------------------- 71 圖4-13 CoFeMnTi1.5VZr 塊材的500倍Mapping -------------------------------71 圖4-14 CoFeMnTi2VZr 塊材的500倍Mapping ---------------------------------72 圖4-15 CoFeMnTi2.5VZr 塊材的500倍Mapping -------------------------------72 圖4-16 CoFe0.5MnTiVZr 粉末的500倍金相與EDS分析 -------------------74 圖4-17 CoFe0.5MnTiVZr 塊材的500倍金相與EDS分析 -------------------74 圖4-18 CoFe1.25MnTiVZr 粉末的500倍金相與EDS分析 -----------------75 圖4-19 CoFe1.25MnTiVZr 塊材的500倍金相與EDS分析 -----------------75 圖4-20 CoFe1.5MnTiVZr 粉末的500倍金相與EDS分析 -------------------76 圖4-21 CoFe1.5MnTiVZr 塊材的500倍金相與EDS分析 -------------------76 圖4-22 CoFe2MnTiVZr 粉末的500倍金相與EDS分析 ---------------------77 圖4-23 CoFe2MnTiVZr 塊材的500倍金相與EDS分析 ---------------------77 圖4-24 CoFe2.5MnTiVZr 粉末的500倍金相與EDS分析 -------------------78 圖4-25 CoFe0.5MnTiVZr 塊材的500倍Mapping -------------------------------78 圖4-26 CoFe1.25MnTiVZr 塊材的500倍Mapping -----------------------------79 圖4-27 CoFe1.5MnTiVZr 塊材的500倍Mapping -------------------------------79 圖4-28 CoFe2MnTiVZr 塊材的500倍Mapping -------------------------------- 80 圖4-29 Tiy合金室溫的動力學曲線圖 -----------------------------------------84 圖4-30 Tiy合金室溫短時間的動力學曲線圖 -----------------------------84 圖4-31 Fex合金室溫的動力學曲線圖 ----------------------------------------85 圖4-32 Fex合金室溫短時間的動力學曲線圖 -----------------------------85 圖4-33 Tiy合金80oC的動力學曲線圖 -----------------------------------------87 圖4-34 Tiy合金80oC短時間的動力學曲線圖 ------------------------------88 圖4-35 Fex合金80oC的動力學曲線圖 --------------------------------------- 88 圖4-36 Fex合金80oC短時間的動力學曲線圖 ---------------------------- 89 圖4-37 t0.9 vs. x變量分佈圖 ------------------------------------------------------90 圖4-38 t0.9 vs. x變量短時間分佈圖 -------------------------------------------90 圖4-39 Tiy合金室溫下 PCI曲線圖 -----------------------------------------------92 圖4-40 Fex合金室溫下 PCI曲線圖 -------------------------------------------- 93 圖4-41 Tiy合金室溫最大儲氫量比較圖 -------------------------------------94 圖4-42 Fex合金室溫最大儲氫量比較圖 ----------------------------------- 94 圖4-43 四系列合金平台壓與成份變量比較圖 --------------------------95 圖4-44 四系列合金平台壓與成份變量 (低壓部份) 比較圖 ------95 圖4-45 四系列合金遲滯效應與成份變量比較圖 ----------------------96 圖4-46 Tiy合金80oC PCI曲線圖 ---------------------------------------------------97 圖4-47 Fex合金80oC PCI曲線圖 ------------------------------------------------- 98 圖4-48 Tiy合金80oC最大儲氫量比較圖 -------------------------------------99 圖4-49 Fex合金80oC最大儲氫量比較圖 ----------------------------------- 99 圖4-50 Ti1的吸氫前後XRD比較圖 ---------------------------------------------101 圖4-51 Ti0.5的吸氫前後XRD比較圖 ------------------------------------------101 圖4-52 Ti1.5的吸氫前後XRD比較圖 ------------------------------------------102 圖4-53 Ti2的吸氫前後XRD比較圖 ---------------------------------------------102 圖4-54 Ti2.5的吸氫前後XRD比較圖 ----------------------------------------- 103 圖4-55 Tiy合金吸氫前的XRD比較圖 -----------------------------------------103 圖4-56 Tiy合金吸氫後的XRD比較圖 -----------------------------------------104 圖4-57 Fe0.5的吸氫前後XRD比較圖 -----------------------------------------104 圖4-58 Fe1.25的吸氫前後XRD比較圖 ---------------------------------------105 圖4-59 Fe1.5的吸氫前後XRD比較圖 -----------------------------------------105 圖4-60 Fex合金吸氫前的XRD比較圖 --------------------------------------- 106 圖4-61 Fex合金吸氫後的XRD比較圖 --------------------------------------- 106 圖4-62 Ti1.5合金置於大氣下一天內與一周後XRD比較圖 --------107 圖4-63 Ti0.5吸放氫前後粉末500倍的金相 -------------------------------111 圖4-64 Ti1吸放氫前後粉末500倍的金相 ----------------------------------111 圖4-65 Ti1.5吸放氫前後粉末500倍的金相 -------------------------------111 圖4-66 Ti2吸放氫前後粉末500倍的金相 ---------------------------------112 圖4-67 Ti2.5吸放氫前後粉末500倍的金相 -------------------------------112 圖4-68 Fe0.5吸放氫前後粉末500倍的金相 ------------------------------112 圖4-69 Fe1.25吸放氫前後粉末500倍的金相 ----------------------------113 圖4-70 Fe1.5吸放氫前後粉末500倍的金相 ------------------------------113 圖4-71 Tiy合金的吸氫前DSC圖 ----------------------------------------------- 118 圖4-72 Ti1吸氫前後DSC對照圖 ----------------------------------------------- 118 圖4-73 Tiy合金的吸氫後DSC圖 -----------------------------------------------119 圖4-74 Fex合金的吸氫後DSC圖 ------------------------------------------------119 圖4-75 L - 1 - 8 粉末的500倍金相與EDS分析 -------------------------- 122 圖4-76 L - 1 - 12 粉末的500倍金相與EDS分析 ------------------------ 122圖4-77 L - 1 - 16 粉末的500倍金相與EDS分析 -------------------------123 圖4-78 L - 1 - 24 粉末的500倍金相與EDS分析 -------------------------123 圖4-79 L - 0.5 - 8 粉末的500倍金相與EDS分析 ------------------------124 圖4-80 L - 0.5 - 12 粉末的500倍金相與EDS分析 --------------------- 124 圖4-81 L - 0.5 - 16 粉末的500倍金相與EDS分析 -----------------------125 圖4-82 L - 0.5 - 24 粉末的500倍金相與EDS分析 -----------------------125 圖4-84 L - 0.3 - 12 粉末的500倍金相與EDS分析 -----------------------126 圖4-84 AlMgNiTiZr等莫耳較高溫度動力曲線圖 ------------------------126 圖4-85 L - 0.3 - 16 粉末的500倍金相與EDS分析 -----------------------127 圖4-86 L - 0.3 - 24 粉末的500倍金相與EDS分析 -----------------------127 圖4-87 AlMgNiTiZr等莫耳室溫動力曲線圖 -------------------------------129 圖4-88 AlMgNiTiZr等莫耳較高溫度動力曲線圖 ------------------------129 圖4-89 AlMgNiTiZr等莫耳室溫下PCI曲線圖 -------------------------------132 圖4-90 AlMgNiwTiZr 400oC下PCI曲線圖 -------------------------------------132 圖4-91 AlMgNiTiZr 吸氫後XRD圖 -----------------------------------------------134 圖4-92 AlMgNi0.5TiZr 吸氫後XRD圖 -------------------------------------------135 圖4-93 AlMgNi0.3TiZr 吸氫後XRD圖 -------------------------------------------135 圖4-94 AlMgNiwTiZr同球磨時間下 (8 h) 吸氫後XRD對照圖--------136 圖4-95 AlMgNixTiZr同球磨時間下 (16 h) 吸氫後XRD對照圖 ------136 圖4-96 AlMgNiTiZr合金的吸氫後DSC圖 -------------------------------------138 圖4-97 AlMgNi0.5TiZr系列的吸氫後DSC圖 -------------------------------- 138 圖4-98 AlMgNi0.3TiZr系列的吸氫後DSC圖 -------------------------------- 139 圖4-99 ΔHcal與儲氫量wt%的關係圖 ---------------------------------------146 圖4-100 ΔHcal與儲氫量 (H / atom) 的關係圖 --------------------------147 圖4-101 ΔHcal與儲氫量 (H / atom) 的關係圖 --------------------------147 圖4-102 三種常用ΔH計算法之比較圖 ----------------------------------148 表目錄 頁次 表1-1 各種氫化物性質 ---------------------------------------------------------------4 表2-1 氫與金屬元素關係圖 -------------------------------------------------------9 表2-2 常見複合氫化物與理論儲氫量 ------------------------------------- 14 表2-3 有關奈米碳管儲氫特性研究成果 ---------------------------------- 20 表2-4 部份二元AB3型合金儲氫量 --------------------------------------------29 表2-5 各種儲氫合金吸放氫前後結構比較 -------------------------------29 表2-6 儲氫合金工程優缺點對照 ----------------------------------------------30 表2-7 儲氫合金工作溫度壓力對照 ------------------------------------------31 表2-8 TiFe合金表面的氧化物 ----------------------------------------------------32 表2-9 各類金屬氫化物活化條件表 ------------------------------------------34 表4-1 非等莫耳Tiy、Fex合金成份列表 --------------------------------------63 表4-2 各金屬元素與氫結合焓 (ΔH) -----------------------------------------63 表4-3 金屬原子半徑表 -------------------------------------------------------------81 表4-4 Tiy與Fex合金室溫動力曲線資訊統整 ------------------------------86 表4-5 相關文獻儲氫動力學資料 [107, 108, 109] -----------------------86 表4-6 Tiy與Fex合金80oC動力曲線資訊統整 -------------------------------89 表4-7 Tiy與Fex合金室溫PCI曲線資料 -----------------------------------------93 表4-8 Tiy與Fex合金80oC PCI曲線資料 ----------------------------------------98 表4-9 Tiy、Fex合金吸氫前的晶格常數對照表 -------------------------107 表4-10 Tiy、Fex合金吸氫後的晶格常數對照表 ---------------------- 108 表4-11 Tiy、Fex合金吸氫後的體積膨脹率 (%) 對照表 -------------108 表4-12 Tiy合金吸放氫前後晶粒大小與顆粒大小資料 -------------114 表4-13 Fex合金吸放氫前後晶粒大小與顆粒大小資料 ------------114 表4-14 許臻豪成份CoFeMnTiVxZry 吸放氫前後晶粒大小資料 --115 表4-15 四系列合金晶粒大小範圍資料 -----------------------------------116 表4-16 常見HCP金屬c/a ratio資料表 ----------------------------------------116 表4-17 AlMgNiwTiZr合金成份配置表 ----------------------------------------120 表4-18 金屬原子半徑表 -------------------------------------------------------- 130 表4-19 Tiy與Fex合金氫化物的結合焓 ------------------------------------- 142 表4-20 輕型含鎂合金氫化物的結合焓 ---------------------------------- 143

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