具鉭顆粒散布強化之鐵基金屬玻璃複材的合成及其性質之研究

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曾建堯(Chien-yao Tseng) 查詢紙本館藏

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材料科學與工程研究所

論文名稱

具鉭顆粒散布強化之鐵基金屬玻璃複材的合成及其性質之研究
(Synthesis and Properties Characterization of Iron Based Bulk Metallic Glass Composites with Ex-situ Tantalum Particles Dispersed Reinforcement)

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摘要(中)

由於鋼鐵材料被廣泛地使用於各個領域，鐵基非晶質合金，亦可稱之為非晶質鋼材，其數十年來一直是非晶質合金材料的研究重點之一。鐵基金屬玻璃與鋯基或鈀基非晶質合金相比之下，價格低廉的特色向來是其最具吸引力之處，但可惜的是，如此的材料卻往往因為缺乏塑性而限制了其應用範疇。為了解決鐵基金屬玻璃塑性不佳的問題，本研究成功利用真空銅模傾鑄法製作出含有外添加鉭顆粒強化的鐵基非晶質複合合金。經由壓縮試驗與硬度量測，我們發現添加13vol. %鉭顆粒塊材的塑性變形量可延展至6.43%，其破裂韌性更可增加至139.4MPa m0.5，破裂應力也高達3.18GPa，而其破裂面與施力方向的夾角為38.8度，若以未添加顆粒的非晶質合金與之相比，後者不具任何的塑性表現。根據掃描式電子顯微儀觀測分析後發現，異質相顆粒於鑄造過程中發生尺寸細化的現象，而細化後之顆粒有助於阻擋微裂隙的前進，並提升複材的機械性質。但是，鉭元素的添加會於鑄造過程中形成碳化鉭，而碳化鉭高硬度與高彈性係數的特性，最終將對材料的塑性產生危害。本研究的成果有助於瞭解使用外添加鉭顆粒對鐵基非晶質基地產生的影響與強化效果。

摘要(英)

Due to the widely used of steel, Fe-based amorphous alloy, also known as amorphous steel, is being studied by many researchers. Comparing to Zr- and Pt-based amorphous alloys, the cost of Fe-based amorphous alloy is the most attracting characteristic, especially. Unfortunately, the lack of plasticity of such material limits its application severely. According to such situation, the ex-situ method is applied in this study where the Fe-based bulk metallic glass composites Fe77Mo5P9C7.5B1.5 was casted with different amount of ex-situ Ta particles addition as the reinforcing phase by tilt mold casting in argon atmosphere. These composite alloys were examined by applying compression loading and indentation so the corresponding mechanical properties were then acquired. The BMG composite with 13vol. % Ta particles possessing a fracture toughness of 139.4 MPa m0.5 can sustain a plastic strain to failure of 6.43% at compressive fracture strength as high as 3.18GPa where the angle between the compressive shear plane and loading axis is ~38.8° while zero plasticity without reinforcing phase particles being distributed. Depending on SEM observation and analysis, the heterogeneous phase particles dispersing in the matrix decreased own sizes after casting which hold better performance to stop the propagation of micro-cracks. However, the formation of tantalum carbide which processing larger hardness and elastic modulus reduced the fraction of ductile Ta phase and thus harmed the plasticity eventually. The results of this study tended to solve the problems of fast propagation of shear bands and micro-cracks in Fe-based BMGs further providing an effective solution to improve the plasticity.

關鍵字(中)

★ 複合材料
★ 散布強化
★ 金屬玻璃

關鍵字(英)

★ Composite
★ Dispersion Strengthening
★ Metallic Glasses

論文目次

中文摘要……………………………………………………………………i
英文摘要……………………………………………………………………ii
總目錄 ……………………………………………………………………iii
表目錄 ……………………………………………………………………vii
圖目錄 ……………………………………………………………………viii
一、前言………………………………………………………………1
二、實驗原理…………………………………………………………3
2-1 塊狀非晶質合金發展簡介………………………………………3
2-2 非晶質合金之種類………………………………………………5
2-3 非晶質合金的設計與製作………………………………………6
2-3-1 實驗歸納法則……………………………………………6
2-3-2 非晶質合金相關製程介紹………………………………7
2-3-3 微量元素的添加與其影響………………………………10
2-4 塊狀非晶質合金複材的發展……………………………………11
2-5 非晶質合金之性質………………………………………………12
2-5-1 機械性質…………………………………………………12
2-5-1-1 自由體積…………………………………………….12
2-5-1-2 剪切轉換區………………………………………….13
2-5-1-3破裂行為與表現……………………………………..14
2-5-2 熱力學性質………………………………………………15
2-5-2-1熱穩定性……………………………………………..15
2-5-2-2玻璃形成能力………………………………………..16
2-5-3 耐腐蝕性質………………………………………………18
三、實驗方法………………………………………………………….20
3-1 實驗目的………………………………………………………….20
3-2 合金製作………………………………………………………….21
3-2-1 合金配置…………………………………………………21
3-2-2 合金熔煉…………………………………………………21
3-2-3 粉末添加…………………………………………………22
3-2-4 非晶質棒材製作………………………………………….22
3-3 實驗分析………………………………………………………….23
3-3-1 成份分析…………………………………………………23
3-3-1-1 成份分析試片製作………………………….…..23
3-3-1-2 成份分析量測…………………………………….23
3-3-1-2-1 能量散布光譜儀……………………………23
3-3-1-2-2 波長散布光譜儀……………………………24
3-3-2 微結構觀測分析…………………………………………24
3-3-2-1 XRD與SEM試片製作……………………………..24
3-3-2-2 X光繞射分析儀……………………………..……24
3-3-2-3 掃瞄式電子顯微鏡……………………………….25
3-3-2-3-1 二次電子(secondary electron)影像………...25
3-3-2-3-2 背向散射電子(BSE)影像…………………..25
3-3-3 機械性質分析……………………………………………26
3-3-3-1 硬度與破壞韌性量測………………………….…26
3-3-3-1-1 試片製作……………………………………26
3-3-3-1-2 維氏硬度……………………………………26
3-3-3-1-3 破壞韌性……………………………………26
3-3-3-2 抗壓強度與塑性量測……………………………27
3-3-3-2-1 試片製作……………………………………27
3-3-3-2-2 壓縮試驗……………………………………28
3-3-4 熱性質分析…………………………………………….28
3-3-4-1 試片製作…………………………………….….28
3-3-4-2 等速率升溫測試………………………………..28
四、結果與討論………………………………………………………30
4-1 Fe77Mo5P9C7.5B1.5非晶質合金性質分析……………….…….…30
4-2 添加鉭顆粒之Fe77Mo5P9C7.5B1.5非晶質合金複材性質分析……33
五、結論………………………………………………………………39
參考文獻………………………………………………………………….40
表目錄
表2-1 常見非晶質合金系統…………………………………………49
表2-2 非晶質合金的分類……………………………………………49
表2-3 非晶質合金的分類……………………………………………50
表4-1 Fe77Mo5P9C7.5B1.5 EPMA成份分析結果……………………..50
表4-2 Fe77Mo5P9C7.5B1.5 基本熱性質………………………………..50
表4-3 Fe77Mo5P9C7.5B1.5 BMGC機械性質數據……………………..51
表4-4 添加之鉭顆粒於棒材中實際分布的比例與尺寸……………51
表4-5 粒徑10μm以上之鉭顆粒尺寸與比例統計………………….52
表4-6 鉭元素與Fe77Mo5P9C7.5B1.5合金各元素混合熱一覽………..52
表4-7 α相鐵於非晶質合金複材中的比例………………………….52
圖目錄
圖2-1 splat-quenching示意圖………………………………………...53
圖2-2 活塞壓擊急冷設備……………………………………………..53
圖2-3 原子簇堆疊方式………………………………………………..54
圖2-4 非晶質合金的機械性質………………………………………..54
圖2-5 非晶質合金抗壓與抗拉時的差異……………………………..55
圖3-1 實驗流程圖……………………………………………………..55
圖3-2 真空氬焊機……………………………………………………..56
圖3-3 慢速切割機……………………………………………………..56
圖3-4 金相研磨機……………………………………………………..57
圖3-5 場發射雙束型聚焦離子束顯微鏡……………………………..57
圖3-6 電子微探儀……………………………………………………..58
圖3-7 X光繞射分析儀………………………………………………..58
圖3-8 維式硬度儀……………………………………………………..59
圖3-9 抗壓試驗夾具…………………………………………………..59
圖3-10 萬能試驗機……………………………………………………..60
圖3-11 熱差掃瞄分析儀………………………………………………..60
圖3-12 維式壓痕與破裂韌性量測……………………………………..61
圖4-1 Fe77Mo5P9C7.5B1.5非晶質合金薄帶於不同升溫速率下之熱差分析曲線………………………………………………………………….…62
圖4-2 Fe77Mo5P9C7.5B1.5 非晶質合金薄帶高溫熱差分析曲線……………………………………………...…………………..63
圖4-3 Fe77Mo5P9C7.5B1.5 非晶質合金塊材與薄帶於相同升溫速率下熱性質差異………………..…………………………………………….63
圖4-4 Fe77Mo5P9C7.5B1.5 基材X光繞射圖形……………………………...64
圖4-5 Fe77Mo5P9C7.5B1.5 基材背向散射電子影像………………………64
圖4-6 銅模鑄造Fe77Mo5P9C7.5B1.5非晶質複合棒材………………...65
圖4-7 不同鉭顆粒添加比例Fe77Mo5P9C7.5B1.5 BMGC抗壓試驗結果一覽…………………………………………………………………65
圖4-8 Fe77Mo5P9C7.5B1.5 + 0 vol. %Ta 荷重50Kg壓痕SEM影像…….66
圖4-9 Fe77Mo5P9C7.5B1.5 + 7.5 vol. %Ta 荷重50Kg壓痕SEM影像…..66
圖4-10 Fe77Mo5P9C7.5B1.5 + 10 vol. %Ta 荷重50Kg壓痕SEM影像……67
圖4-11 Fe77Mo5P9C7.5B1.5 + 13 vol. %Ta 荷重50Kg壓痕SEM影像……67
圖4-12 Fe77Mo5P9C7.5B1.5 + 15 vol. %Ta 荷重50Kg壓痕SEM影像……68
圖4-13 Fe77Mo5P9C7.5B1.5 + 7.5 vol. %Ta背向散射電子影像…………68
圖4-14 Fe77Mo5P9C7.5B1.5 + 10 vol. %Ta背向散射電子影像………….69
圖4-15 Fe77Mo5P9C7.5B1.5 + 13 vol. %Ta背向散射電子影像………….69
圖4-16 Fe77Mo5P9C7.5B1.5 + 15 vol. %Ta背向散射電子影像………….70
圖4-17 不同鉭顆粒添加比例之Fe77Mo5P9C7.5B1.5 BMGC板材熱性質差異………………………………………………………………..71
圖4-18 不同顆粒添加比例之Fe77Mo5P9C7.5B1.5 BMGC棒材之XRD圖形………………………………………………………………..72
圖4-19 Fe77Mo5P9C7.5B1.5 + 7.5 vol. %Ta背向散射電子影像…………73
圖4-20 Fe77Mo5P9C7.5B1.5 + 10 vol. %Ta背向散射電子影像………….73
圖4-21 Fe77Mo5P9C7.5B1.5 + 13 vol. %Ta背向散射電子影像………….74
圖4-22 Fe77Mo5P9C7.5B1.5 + 15 vol. %Ta背向散射電子影像………….74
圖4-23 不同顆粒添加比例之Fe77Mo5P9C7.5B1.5 BMGC板材之XRD圖形………………………………………………………………..75
圖4-24 棒材碎片比較，左方為基材，右方為具有13vol. %鉭顆粒添加………………………………………………………………..75
圖4-25 具13vol. %顆粒添加之棒材破斷面(側面)……………………76
圖4-26 具13vol. %顆粒添加之棒材破斷面(側緣)……………………76
圖4-27 具13vol. %顆粒添加之棒材破斷面，棒材邊緣破裂起始處……..77
圖4-28 具13vol. %顆粒添加之棒材破斷面，棒材中心……………..77

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指導教授

鄭憲清(Jason Shian-ching Jang)

審核日期

2012-7-23

推文