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研究生： 黃東平
Dong-ping Huang
論文名稱： 鐵鉻合金與鎳-釔安定化氧化鋯陶金之界面反應及接合之研究
Study on Interfacial Reactions between Iron-Chromium Alloy and Nickel-Yttria Stabilized Zirconia Cermet,and Joint Behavior
指導教授： 顏怡文
Yee-wen Yen
口試委員: 李嘉平
Chiapyng Lee
陳志銘
Chih-ming Chen
學位類別： 碩士
Master
系所名稱： 工程學院 - 材料科學與工程系
Department of Materials Science and Engineering
論文出版年： 2006
畢業學年度： 94
語文別： 中文
論文頁數： 186
中文關鍵詞： 界面反應 、鎳-釔安定化氧化鋯陶金 、不鏽鋼 、硬銲
外文關鍵詞： interfacial reaction, Ni-YSZ cerment, stainless steel, brazing
相關次數： 點閱：247  下載：9 
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    • 固態氧化物燃料電池的系統中，不鏽鋼材料是近年來熱門的雙極板材料，主要元素為Fe-Cr-Ni；陽極材料為鎳-釔安定化氧化鋯陶金。本研究主要著重在探討4種Fe-Cr合金與Ni界面反應關係，並以真空硬銲方式，使用Ag-Cu與商用Ag基活性填料，接合商用430不鏽鋼與Ni-YSZ陶金。
    Fe-Cr/Ni界面反應，當Fe-Cr合金組成為Fe-16、25wt%Cr時，界面可以觀察到γ與α+α’的兩相混合區；當Fe-Cr合金組成為Fe -80、94wt%Cr時，界面則可以觀察到γ+α’的兩相混合區。隨著反應時間及溫度的增加，合金含Cr量的減少，反應層厚度隨之變厚，總厚度與時間平方根成正比關係，符合拋物線定律，反應為擴散控制。
    商用430不鏽鋼與陽極Ni-YSZ之接合，採用Ag-Cu與商用Ag基活性填料，以真空硬銲方式進行，將系統簡化為Ni、YSZ、430不鏽鋼與Ni-YSZ與填料反應。在Ag-Cu/Ni的液固反應中，Ni基材界面會隨填料含Cu量，逐漸生成(Cu,Ni)固溶體。穩定(Cu,Ni)固溶體生成，會減緩Cu原子往Ni基材擴散之趨勢。探討Ag-Cu/電鍍 Ni/ 430不鏽鋼的液固反應，含Cu量低的填料，界面越平整，反應層為γ(Fe,Ni)；含Cu量高的填料，界面越粗糙，反應層為(Cu,Ni)．γ(Fe,Ni)。
    使用商用Silver ABA填料接合YSZ/430不鏽鋼，在YSZ界面上可以觀察到TiO/Cu2(Ti,Al)4O生成，隨著溫度與時間增加，生成相轉為TiO, Al2O3/Cu2(Ti,Al)4O，Cu2(Ti,Al)4O 會逐漸被TiO取代且其形態也會轉為島嶼狀。430不鏽鋼界面上生成物短時間為過飽和固溶Ti的AlCu2Ti/Ti-rich，長時間下轉為Ti-rich；使用商用Cusil ABA填料，在YSZ界面上則可以觀察到TiO/ Cu3Ti3O/Cu2Ti4O生成，隨著溫度與時間增加，Cu2Ti4O會逐漸溶解而消失，430不鏽鋼界面上生成物無論時間長短，均為Cu-Ti化合物；使用商用Ag50Cu48Ti2填料，在YSZ界面上則可以觀察到TiO/Cu3Ti3O生成，隨著溫度與時間增加，Cu3Ti3O會逐漸剝離至填料中，430不鏽鋼界面上生成物無論時間長短，均為Cu-Ti化合物。
    使用商用Silver ABA填料接合Ni/430不鏽鋼，在Ni界面處短時間下共有三反應層AlNi3/TiNi3/AlNi2Ti，長時間持溫下最終只有AlNi3穩定存在，430不鏽鋼界面上生成物無論時間長短，均為Ti-rich。使用商用Cusil ABA填料，在Ni界面處生成(Cu,Ni)固溶體，填料區為固化後之常溫組織，在831℃以下，主要由Ag-rich、針狀TiNi3及島嶼狀(Cu,Ni)固溶體組成，溫度861℃以上，島嶼狀(Cu,Ni)固溶體會轉為層狀並固溶2.4at.%Ti，在430不鏽鋼界面上並無明顯生成物。使用商用Ag50Cu48Ti2填料，在Ni界面處生成(Cu,Ni)固溶體，填料區為固化後之常溫組織，在838℃以下，主要由Ag-rich、針狀TiNi3、島嶼狀(Cu,Ni)固溶體及大團塊Cu-rich組成，溫度為868℃時，大團塊Cu-rich轉為島嶼狀(Cu,Ni)固溶體，在430不鏽鋼界面上並無明顯生成物。

    The stainless steels are one of the popular interconnect materials in the SOFC systems recently. The anode material is Nickel-Yttria Stabilized Zirconia cermet (Ni-YSZ). In this study, interfacial reactions between Fe-Cr alloys and Ni-YSZ were experimentally investigated at specific temperatures and the vacuum brazing of Ni-YSZ to stainless steel was carried out using Ag-Cu and Ag-based alloys as active fillers.
    In Fe-Cr/Ni reaction couples, Cr in 16 or 25 wt%, the reaction layer were γ and α+α’ at 750℃; When the temperature is 850℃, α+α’ will turn to γ+α’. As Cr is in 80 or 94wt%, the reaction layer were γ+α’ two phase region at 750、850℃. The thickness of reaction layers increased with low Cr%, long time and higher temperature, and the growth mechanism can be described by using parabolic law.
    In Ag-Cu/Ni reaction couples, (Cu,Ni) solid solution formed gradually which increased with reaction time and Cu%. It seems that (Cu,Ni) solid solution is the diffusion barrier in Ag-Cu/Ni reaction couples.
    In Ag-Cu/EP Ni/430SS reaction couples, the filler of content of low Cu, the morphology is smooth and the reaction layer was γ(Fe,Ni). On the contrary, high content of Cu, the reaction layer was (Cu,Ni)．γ(Fe,Ni).
    Joining of 8YSZ to 430SS has been carried out using Silver ABA filler. Interface microstructure found between filler and YSZ were TiO and Cu2(Ti,Al)4O; Increased with time and temperature the reaction products were Al2O3-TiO/Cu2(Ti,Al)4O phases. The Cu2(Ti,Al)4O will be replaced by TiO and the morphology turn to island gradually. At braze/430SS interface a discontinuous layer identified as Ti-rich formed.
    Joining of 8YSZ to 430SS has been carried out using Cusil ABA filler. The microstructure at the interface, three reaction products TiO、Cu3Ti3O and Cu2Ti4O phases formed between filler and YSZ; Increased with time and temperature, the Cu2Ti4O will dissolve into filler and disappear gradually. At braze/430SS interface a discontinuous layer identified as Cu-Ti formed.
    Joining of 8YSZ to 430SS has been carried out using Ag50Cu48Ti2 filler. The reaction layers at the interface between filler and YSZ were TiO and Cu3Ti3O phases; Increased with time and temperature the reaction layer Cu3Ti3O spalling into filler gradually. At braze/430SS interface a discontinuous layer identified as Cu-Ti formed.
    Joining of Ni to 430SS has been carried out using Silver ABA filler. Three types reaction layers formed at the interface between filler and Ni were AlNi3/TiNi3/AlNi2Ti phases; Increased with time and temperature，only AlNi3 can stabilize the existence. At braze/430SS interface a discontinuous layer identified as Ti-rich formed.
    Joining of 8YSZ to 430SS has been carried out using Cusil ABA filler. The microstructure at the interface between filler and Ni were (Cu,Ni) solid solution; In the filler matrix, spread a lot of acicular TiNi3 and form (Cu,Ni) in island; At braze/430SS interface have not observed reaction layers clearly.
    Joining of 8YSZ to 430SS has been carried out using Ag50Cu48Ti2 filler, have similar results with Cusil ABA filler.

    第一章 前言..........................................................1 第二章 文獻回顧與理論基礎............................................3 2-1 固態氧化物燃料電池簡介......................................3 2-2 固態氧化物燃料電池雙極板材料相關研究.......................12 2-3 固態氧化物燃料電池密封材料相關研究.........................14 2-4 相平衡圖...................................................16 2-4.1 Fe-Cr二元相平衡圖..........................................17 2-4.2 Ni-Cr二元相平衡圖..........................................18 2-4.3 Fe-Ni二元相平衡圖..........................................19 2-4.4 Fe-Cr-Ni三元相平衡圖.......................................20 2-5 擴散機制與界面反應.........................................23 2-6 金屬與陶瓷的接合技術.......................................27 2-6.1 擴散接合...................................................28 2-6.2 真空硬銲...................................................29 2-6.3 不鏽鋼與氧化物陶瓷接合相關研究文獻.........................31 第三章 實驗方法.....................................................39 3-1 合金製備...................................................39 3-2 反應偶製備.................................................43 3-3 YSZ塊材製備................................................44 3-4 Ni-YSZ cermet塊材製備......................................45 3-5 電鍍.......................................................48 3-6 真空硬銲...................................................50 3-7 試片分析...................................................53 第四章 結果與討論...................................................56 4-1 Fe-Cr合金/Ni基材界面反應...................................56 4-2 Ag-Cu填料系統..............................................77 4-2.1 Ag-Cu填料/Ni基材液固反應...................................77 4-2.2 430SS/EP Ni固固反應........................................94 4-2.3 430SS/EP Ni/Ag-Cu液固反應..................................96 4-3 Ag基活性填料系統..........................................101 4-3.1 430SS/商用Silver ABA填料/8YSZ基材液固反應.................101 4-3.2 430SS/商用Cusil ABA填料/8YSZ基材液固反應..................117 4-3.3 430SS/商用Ag50Cu48Ti2填料/8YSZ基材液固反應................129 4-3.4 430SS/商用Silver ABA填料/Ni基材液固反應...................146 4-3.5 430SS/商用Cusil ABA填料/Ni基材液固反應....................157 4-3.6 430SS/商用Ag50Cu48Ti2填料/Ni基材液固反應..................168 第五章 結論........................................................177 第六章 參考文獻....................................................180

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