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論文名稱 Title |
Zr-Al-Si系三元合金800 ℃平衡相圖研究 Phase Diagram Study of Zr-Al-Si ternary system at 800 ℃ |
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系所名稱 Department |
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畢業學年期 Year, semester |
語文別 Language |
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學位類別 Degree |
頁數 Number of pages |
102 |
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研究生 Author |
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指導教授 Advisor |
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召集委員 Convenor |
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口試委員 Advisory Committee |
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口試日期 Date of Exam |
2009-06-11 |
繳交日期 Date of Submission |
2009-07-16 |
關鍵字 Keywords |
鋁、三元合金、相圖、鋯、矽 Phase Diagram, ternary system, Zr-Al-Si |
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統計 Statistics |
本論文已被瀏覽 5666 次,被下載 0 次 The thesis/dissertation has been browsed 5666 times, has been downloaded 0 times. |
中文摘要 |
本實驗主要探討Zr-Al-Si系三元合金800 ℃平衡相圖,其探討這系統的主要動機是現有的文獻資料中,有關這系統的平衡相圖相關資料文獻不多而有待開發,且文獻中多半使用Zr與Al-Si共晶合金或其重要關鍵點的三元擴散偶的研究,均質化熱處理的時效時間僅僅是2至24小時,相較於打點分析熱處理的時間360至720小時有著顯著的差異,其擴散偶合金相的平衡與元素擴散是否均勻,可從本實驗與文獻中的相圖對照比對,得知其結果,又因為文獻中只取Al-Si共晶合金做不同溫度的擴散偶,使其單一溫度三元平衡相圖中,大部分角落部份缺少相的平衡的結果。所以本實驗採用打點分析,先用文獻中的相圖為參考標準,先選出十一個點,等實驗結果出來後,再更進一步做其他點的相作確認。 因此本實驗以純Zr、Al、Si配製選定的合金成分,利用真空熔煉(Arc Melting)的方式均勻混合合金,然後將合金試片放置在高溫管狀爐800 ℃中進行維持兩週的均質化(Homogenization)熱處理,使合金試片達到相平衡。然後將熱處理後的金屬作金相前處理,包括鑲埋、研磨與拋光。再分別進行合金試片的SEM分析以及EPMA分析各相的成分與DTA熱分析後的結果,最後根據以上所有量測結果,進而完成建立起Zr-Al-Si系三元合金800 ℃相圖,希望藉由這些平衡相圖的輪廓和熱分析實驗結果,將來當做提供尋找Zr-Al-Si系三元合金成份或相關系四元或五元合金成份的參考資料。 在研究Zr-Al-Si系三元合金800 ℃平衡相圖中,研究發現在Zr-Si二元系合金系統中,有三的介金屬平衡相Zr3Si2、ZrSi以及ZrSi2的存在;研究發現在Al-Zr二元系合金系統中,有六個介金屬平衡相AlZr3、AlZr2、Al3Zr4、Al3Zr2、Al2Zr與Al3Zr的存在;且研究相圖中總共有十四個三相區和十五個兩相區的生成。研究更發現,除了文獻中所提到的三個三元化合物外,還在組成成分65 at% Zr附近,發現了第四個三元化合物 |
Abstract |
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目次 Table of Contents |
摘要····························································································································· i 總目錄······················································································································ iii 表目錄······················································································································ vi 圖目錄···················································································································· viii 壹、前言················································································································· 1 貳、研究動機與文獻回顧······················································································ 3 2.1 Zr-Al-Si 合金相圖的應用······································································ 3 2.1.1 應用於非晶質合金···································································· 3 2.1.2 應用於耐熱合金方面································································ 4 2.1.3 應用於奈米孔洞材料································································ 5 2.1.4 結論···························································································· 6 2.2 平衡相圖································································································· 6 2.3 二元系合金平衡相圖············································································· 7 2.3.1 Zr-Al 二元系合金平衡相圖······················································· 7 2.3.2 Zr-Si 二元系合金平衡相圖······················································· 8 2.3.3 Si-Al 二元系合金平衡相圖······················································· 9 2.4 Zr-Al-Si 三元系統平衡相圖·································································· 9 參、研究方法與步驟···························································································· 12 3.1 研究方法······························································································· 12 3.2 實驗步驟······························································································· 12 3.2.1 選點·························································································· 12 3.2.2 切割與秤重·············································································· 13 3.2.3 合金配置·················································································· 14 3.2.4 封管與均質化熱處理······························································ 15 3.2.5 金相前處理·············································································· 16 3.2.6 金相量測分析·········································································· 17 3.2.7 熱分析(DTA) ······································································ 18 3.2.8 平衡相圖的量測分析······························································ 19 肆、實驗結果討論································································································ 20 4.1 Zr-Al-Si 三元系合金的EPMA 量測分析··········································· 20 4.1.1 Zr2Al5Si-Al2Zr-Al3Zr 三相區···················································· 21 4.1.2 Zr4AlSi3-Al2Zr- Zr2Al5Si 三相區·············································· 21 4.1.3 Al3Zr2-Al2Zr- Zr3Si2 三相區······················································· 22 4.1.4 τ4-AlZr3-(α-Z)三相區······························································· 23 4.1.5 Zr3Si2-Al2Zr-Zr4AlSi3 三相區··················································· 24 4.1.6 Zr2Al5Si-Zr3Al4Si5-ZrSi 三相區··············································· 25 4.1.7 Al3Zr4-τ4-Al3Zr2 三相區··························································· 26 4.1.8 Al3Zr4-τ4-AlZr2 三相區···························································· 26 4.1.9 Zr3Si2-τ4-(α-Zr)三相區····························································· 27 4.1.10 Zr3Si2-ZrSi-Zr4AlSi3 三相區··················································· 28 4.1.11 ZrSi2-ZrSi-Zr3Al4Si5 三相區··················································· 29 4.2 Zr-Al-Si 三元系合金的EPMA 量測分析結果··································· 29 伍、討論··············································································································· 31 5.1 Zr-Al-Si 三元系合金平衡相圖···························································· 31 5.1.1 1 號合金試片在三元相圖中的分布情況·································· 31 5.1.2 2 號合金試片在三元相圖中的分布情況·································· 32 5.1.3 3 號合金試片在三元相圖中的分布情況·································· 32 5.1.4 5、6 號合金試片在三元相圖中的分布情況···························· 33 5.1.5 7、8 號合金試片在三元相圖中的分布情況···························· 33 5.1.6 9、10、11 號合金試片在三元相圖中的分布情況·················· 34 5.1.7 12 號合金試片在三元相圖中的分布情況································ 34 5.1.8 13 號合金試片在三元相圖中的分布情況································ 35 5.1.9 14 號合金試片在三元相圖中的分布情況································ 35 5.1.10 15 號合金試片在三元相圖中的分布情況······························ 35 5.1.11 16 號合金試片在三元相圖中的分布情況······························ 36 5.2 本實驗800 ℃相圖與文獻中Jain 和Gupta 900 ℃相圖的比較······· 36 5.2.1 1 號試片位置800 ℃相圖與文獻900 ℃相圖比較················ 37 5.2.2 2 號試片位置800 ℃相圖與文獻900 ℃相圖比較················ 37 5.2.3 3 號試片位置800 ℃相圖與文獻900 ℃相圖比較················ 38 5.2.4 5、6 號試片位置800 ℃相圖與文獻900 ℃相圖比較·········· 38 5.2.5 7、8 號試片位置800 ℃相圖與文獻900 ℃相圖比較·········· 38 5.2.6 9、10、11 號試片位置800 ℃相圖與文獻900 ℃相圖比較· 39 5.2.7 12 號試片位置800 ℃相圖與文獻900 ℃相圖比較·············· 39 5.2.8 13 號試片位置800 ℃相圖與文獻900 ℃相圖比較·············· 40 5.2.9 13 號試片位置800 ℃相圖與文獻900 ℃相圖比較·············· 40 5.2.10 15 號試片位置800 ℃相圖與文獻900 ℃相圖比較············ 40 5.2.11 16 號試片位置800 ℃相圖與文獻900 ℃相圖比較············· 41 陸、結論··············································································································· 42 柒、參考文獻········································································································ 45 表2-1 非晶質合金的性質與應用························49 表4-1 Zr-Al-Si三元系合金1號試片Zr29Al68Si3的成分分析與平衡圖(一)························50 表4-1 Zr-Al-Si三元系合金2號試片Zr34Al53Si13的成分分析與平衡圖(二)························51 表4-1 Zr-Al-Si三元系合金3號試片Zr44Al47Si9的成分分析與平衡圖(三)························52 表4-1 Zr-Al-Si三元系合金4號試片Zr51Al40.5Si8.5的成分分析與平衡圖(四)························53 表4-1 Zr-Al-Si三元系合金5號試片Zr70Al20Si10的成分分析與平衡圖(五)························54 表4-1 Zr-Al-Si三元系合金6號試片Zr70Al10Si20的成分分析與平衡圖(六)························55 表4-1 Zr-Al-Si三元系合金7號試片Zr57.5Al6Si36.5的成分分析與平衡圖(七)························56 表4-1 Zr-Al-Si三元系合金8號試片Zr53.5Al13Si33.5的成分分析與平衡圖(八)························57 表4-1 Zr-Al-Si三元系合金9號試片Zr43.5Al16.5Si40的成分分析與平衡圖(九)························58 表4-1 Zr-Al-Si三元系合金10號試片Zr37.5Al22.5Si40的成分分析與平衡圖(十)························59 表4-1 Zr-Al-Si三元系合金11號試片Zr31.8Al22.2Si46的成分分析與平衡圖(十一)························60 表4-1 Zr-Al-Si三元系合金12號試片Zr58Al22Si20的成份分析與平衡相(十二)························61 表4-1 Zr-Al-Si三元系合金13號試片Zr60Al30Si10的成份分析與平衡相(十三)························62 表4-1 Zr-Al-Si三元系合金14號試片Zr67Al3Si30的成份分析與平衡相(十四)························63 表4-1 Zr-Al-Si三元系合金15號試片Zr53Al5Si42的成份分析與平衡相(十五)························64 表4-1 Zr-Al-Si三元系合金16號試片Zr38Al7Si55的成份分析與平衡相(十六)························65 表4-2 Zr-Al-Si三元系合金的三相區(一)························66 表4-2 Zr-Al-Si三元系合金的三相區(二)························67 表5-1 Zr-Al-Si三元系合金8號試片900 ℃Zr53.5Al13Si33.5的成份分析與平衡相(一) ························68 表5-1 Zr-Al-Si三元系合金10號試片900 ℃Zr37.5Al22.5Si40的成份分析與平衡相(二) ························69 圖2-2 Zr-Al二元系平衡相圖························70 圖2-3 Zr-Si二元系平衡相圖························71 圖2-4 Al-Si二元系平衡相圖························72 圖2-5 Zr-Al-Si900 ℃平衡相圖研究························73 圖2-6 Zr-Al-Si1000 ℃平衡相圖研究························73 圖3-1 三元系合金平衡相圖的架構圖························74 圖3-2 實驗流程圖························74 圖3-3 合金選點圖························75 圖3-4 真空電弧熔煉爐的結構圖························75 圖4-1 合金試片1號的顯微組織照片························76 圖4-2 合金試片2號的顯微組織照片························76 圖4-3 合金試片3號的顯微組織照片························77 圖4-4 合金試片4號的顯微組織照片························77 圖4-5 合金試片5號的顯微組織照片························78 圖4-6 合金試片6號的顯微組織照片························78 圖4-7 合金試片7號的顯微組織照片························79 圖4-8 合金試片8號的顯微組織照片························79 圖4-9 合金試片9號的顯微組織照片························80 圖4-10 合金試片10號的顯微組織照片························80 圖4-11 合金試片11號的顯微組織照片························81 圖4-12 合金試片12號的BEI顯微組織照片························81 圖4-13 合金試片13號的BEI顯微組織照片························82 圖4-14 合金試片14號的BEI顯微組織照片························82 圖4-15 合金試片15號的BEI顯微組織照片························83 圖4-16 合金試片16號的BEI顯微組織照片························83 圖5-1 1號合金試片在三元相圖at%中的分布情況························84 圖5-2 2號合金試片在三元相圖at%中的分布情況························84 圖5-3 3號合金試片在三元相圖at%中的分布情況························85 圖5-4 5、6號合金試片在三元相圖at%中的分布情況························85 圖5-5 7、8號合金試片在三元相圖at%中的分布情況························86 圖5-6 9、10、11號合金試片在三元相圖at%中的分布情況························86 圖5-7 12號合金試片在三元相圖at%中的分布情況························87 圖5-8 13號合金試片在三元相圖at%中的分布情況························87 圖5-9 14號合金試片在三元相圖at%中的分布情況························88 圖5-10 15號合金試片在三元相圖at%中的分布情況························88 圖5-11 16號合金試片在三元相圖at%中的分布情況························89 圖5-12 Zr-Al-Si三元系合金800 ℃平衡相圖························89 圖5-13 合金試片8號900 ℃的BEI顯微組織照片························90 圖5-14 合金試片10號900 ℃的BEI顯微組織照片························90 |
參考文獻 References |
1. A. Peruzzi, “ Reinvestigation of the Zr-rich end of the Zr-Al equilibrium phase diagram ” , Journal of Nuclear Materials, vol. 186, pp. 89-99, 1992 2. N. Bertolino and U. Anselmi-Tamburini, “ Combustion synthesis of Zr-Si intermetallic compounds ” , Journal of Alloys and Compounds, vol. 288, pp. 238-248, 1999 3. 李俊霖, “ Al-Au-Cu和Al-Au-Pt擴散偶相圖研究 ” , 國立中山大學, 碩士論文, 2008 4. V.G. Kuznetsov and V.I. Ravezova, “ Structure of the Compound AlAu4 ” , Dokl. Akad. Nauk. , SSSR, 81. pp. 51-54, 1951, in Russian 5. E. Philofsky, “ Intermetallic Formation in Gold-Aluminum System ” , Solid State Electronics, vol. 13, pp. 1391-1399, 1970 6. 賴加瀚, “ Al-Cr-Ta-Ti-Zr-N多元氮化物薄膜之製備與性質研究 ” ,清華大學, 博士論文,2007 7. 施志雄, “ 鈦鋯銅鎳四元系800 ℃相圖測定 ” , 國立中山大學, 碩士論文, 1995 8. A. Inoue, “ Stabilization of metallic supercooled liquid and bulk amorphous alloys ” , Acta Materialia, vol. 48, pp. 279-306, 2000 9. W. H. Wang, “ Roles of minor additions in formation and properties of bulk metallic glasses ” , Prog. Mater. Sci. , vol. 52, pp. 540-596, 2007 10. A. Inoue, “ Bulk glassy and nonequilibrium crystalline alloys by stabilization of supercooled liquid: fabrication, functional properties and applications ” , Proc. Japan Acad. , B81, pp. 156-171, 2005 11. A.I. Salimon, M.F. Ashby, Y. Brecher and A.L. Greer, “ Bulk metallic glasses: what are they good for? ” , Mater. Sci. Eng. , A375-377, pp. 358-388, 2004 12. 蔣偉仁, “ 鋯基非晶質合金及平衡相圖研究 ” , 國立中山大學, 博士論文, 2007 13. 洪子翔, “ 添加硼與矽對鋯鋁銅鎳非晶質合金結晶之熱性質研究 ” , 國立中山大學, 碩士論文, 2003 14. J. Stringer and I.G. Wright, “ Current limitations of high-temperature alloys in practical applications ” , Oxidation of Metals, vol. 44, p. 265, 1995 15. P. Elliott, “ Materials performance in high-temperature waste combustion systems ” , Materials Performance, p. 88, Feb. 1993 16. 卓靜玟, “ 耐熱合金之高溫氧化速率研究 ”, 國立成功大學, 碩士論文, 1995 17. F.H. Stott, G.C. Wood and J. Stringer, “ The influence of alloying elements on the development and maintenance of protective scales ” , Oxidation of Metals, vol. 44, p.113, 1995 18. M.G. Fontana, “ Corrosion Engineering ” , McGraw-Hill Book Company, Singapore, 1987 19. F.H. Stott and F.I. Wei, “ Comparison of the effects of small additions of silicon or aluminum on the oxidation of iron chromium-alloys ” , Oxidation of Metals, vol. 31, p.369, 1989 20. R. Prescott and M.J. Graham, “ The oxidation of iron aluminum-alloys ” , Oxidation of Metals, vol. 38, p.73, 1992 21. Y.C. Hsu, Y.T. Hsu, H.Y. Hsu, C.M. Yang, “ Facile Synthesis of Mesoporous Silica SBA-15 with Additional Intra-Particle Porosities ” , Chemistry of Materials, vol. 19, pp. 1120, 2007 22. 曹世明, “ 矽酸鋁及矽酸鋯鋁奈米孔洞材料SBA-15之水熱穩定性及反應活性 ” , 中原大學, 碩士論文, 2007 23. F.N. Rhines, “ Phase Diagram in Metallurgy ” , McGraw-Hill Book Company, New York, pp. 5-8, 1956 24. W.L. Fink, L.A. Willey, “ Al-Zr phase diagram ” , metals handbook. Metal Park (OH):American Society for Metal, pp. 1168, 1948 25. D.J. McPherson and M. Hansen, Trans. Am. Soc. Met, vol. 46, pp. 354, 1954 26. T.B. Massalsk, “ binary alloy phase diagram second edition ” , 1990 27. C.B. Alcock, K.T. Jacob, S. Zador, O. von Goldbeck, H. Nowotny, K. Seiffert, O. Kubaschewski, “ Atomic energy review ” , Special Issue No. 6, I. A. E. A. Vienna(Austria), 1976 28. H. Schachner, H. Nowotny, R. Machenschalk, Monatsch Chem. , vol. 84, pp. 677-685, 1953 29. H. Okamto, Bull Alloy Phase Diagram, vol. 11, pp. 513-519, 1990 30. S.A. Kori, B.S. Murty, M. Chakraborty, “ Development of an efficient grain refiner for Al-7Si alloy and its modification with strontium ” , Material Science and Engineering A283, pp. 94-104, 2000 31. Hansen and Loper, “ effect of antimony the phase equilibrium of binary Al-Si alloys ” , 2000 32. M.E. Drits, E.S. Kadaner, V.I. Kuzmina, “ Solubility of Si and Zr in Al ” , Russ Metal, vol. 1, pp. 170-5, 1968 33. H. Nowotny, H. Huschka, “ Studies of the partial system Al-TiSi2, Al-ZrSi2, Al-MoSi2. Al-WSi2 ” , Monatsch Chem. , vol. 88, pp. 494-501, 1957 34. A. Raman, K. Schubert, “ On the Contribution of Some Alloy Series Related to TiAl3. II. Investigations in Some Ti-Al-Si and T4-6-In Systems” , Z. Metallkd. , vol. 56, pp. 44-52, 1965 35. J.K. Jain, S.P. Gupta, “ Intermatallic compound formation in the Zr-Al-Si ternary system ” , Material Characterization, vol. 49, pp. 139-148, 2003 36. O. Schob, H. Nowotny, F. Benesovsky, “ Structure determination of certain phases in the Al-Si-Zr and Al-Hf-Si systems ” , Monatsch Chem. , vol. 92, pp. 1218-26, 1961 37. O. Schob, H. Nowotny, F. Benesovsky, “ The ternary system formed by Ti, Zr and Hf with Al and Si ” , Planseeber Pulvermetal, vol. 10, pp. 65-71, 1962 38. K. Schubert, F. Frank, R. Gohle, A. Maldonado, H.G. Meissner, A. Raman, “ Structural data on metallic phases VIII ” , Naturwissenschaften, vol. 50, pp. 41, 1963 39. M. Hamelin, K. Girgis, A. Prince, “ Al-Si-Zr ternary diagram ” , In: Petzow G, Effenberg G, editor, Ternary Alloys, New York: VCH Publication, vol. 8, pp. 354-8, 1993 40. J.L. Murray, A.J. McLister, “ The Al-Si system ” , Bull Alloy Phase Diagram, vol. 5, pp. 77-84, 1984 |
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