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論文名稱 Title |
利用摩擦攪拌製程及原位反應製造鋁基奈米複合材料 Aluminium matrix nanocomposites produced in situ by friction stir processing |
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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 |
163 |
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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 |
2011-03-18 |
繳交日期 Date of Submission |
2011-03-26 |
關鍵字 Keywords |
Al-Fe2O3系統、鋁-鐵系統、鋁-鉬系統、原位(in situ)反應、鋁基複合材料、摩擦攪拌 Al-Fe, Al-Mo, Al-Fe2O3, in-situ reaction, FSP |
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統計 Statistics |
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中文摘要 |
在本研究中利用摩擦攪拌製程已成功製造原位(in situ) 鋁基複合材料。製程 中,先藉著粉末冶金方式將鋁-鐵、鋁-鉬及鋁-氧化鐵粉末均勻混合後,再利用傳 統冷壓與燒結方式製成試棒。之後再利用多道次摩擦攪拌所提供的高溫與大量的 塑性應變來製造原位金屬基複合材料。而此概念是結合製程的摩擦熱與鋁跟過渡 金屬(TM)或鋁跟金屬氧化物(MO)之間反應放熱來製造大量的奈米強化項在鋁基 材中。 在鋁-鐵系統中,經由摩擦攪拌製程可引發鋁、鐵粉末之間原位(in situ)反應, 且生成Al-Al13Fe4化合物。而此強化項Al13Fe4顆粒大小約100奈米。在鋁-鉬系統中, 生成的介金屬化合物可均勻的散佈在基材中,而此介金屬強化項顆粒主要為 Al12Mo與少量的Al5Mo,且放熱反應會在界面產生局部Al熔融而加快反應形成。也 因摩擦攪拌所產生大量的塑性變形,可將在界面產生的介金屬顆粒有效的移走且 均勻散佈在鋁基材中。 在Al-Fe2O3 系統中, 藉由摩擦攪拌所引發的熱機反應(thermite reaction, Al+Fe2O3→Al2O3+Al13Fe4)與反應所還原出來的鐵會與多餘的鋁再進而反應產生 Al13Fe4化合物。所以在試棒中有兩種強化項Al13Fe4與Al2O3,且Al2O3顆粒約10奈米 大小且團聚成約100-200奈米之顆粒。在試棒中也因Fe2O3含量的多寡同時存在兩種 Al2O3相。在Al-2Fe2O3合金中是γ相的氧化鋁而在高含量Al-4Fe2O3合金中則是α相 的氧化鋁。而此不同則是因為不同反應熱釋放的關係,與Al-4Fe2O3系統做比較, 在Al-2Fe2O3中有較低的反應熱而在Al-4Fe2O3中則有較多釋放的反應熱。 同時,在Al-Al13Fe4/Al2O3化合物中則具有高強度且較佳的延展性。而此高強 度推測主要是由於裡面含有較小的Al2O3顆粒所造成。且其高溫的強度在五百度時 還可維持在100 MPa,因此,此化合物的高溫穩定性極佳。而高溫強度佳則是由於 小的顆粒所貢獻,尤其是氧化鋁顆粒。因氧化鋁顆粒在高溫相當穩定。 在計算摩擦攪拌溫度的演化方面,須考慮摩擦攪拌所生成的摩擦熱,再加上 反應所釋放的生成熱。而所得之最高溫度Tp與反應完的Fe或Fe2O3的比例做圖可知 Tp為反應比例的函數。由計算結果顯示最高溫度Tp可容易的到達鋁熔融溫度,尤其在Al-Fe2O3系統中。而在摩擦攪拌中的反應機制與微結構的演化也會在文章中做詳 細討論 |
Abstract |
Friction stir processing (FSP) was applied to produce aluminum based in situ composites from powder mixtures of Al-Fe, Al-Mo, and Al-Fe2O3. Billet of powder mixtures was prepared by the use of conventional pressing and sintering route. The sintered billet was then subjected to multiple passages of FSP. During FSP, the material has experienced both high temperature and very large plastic strain. The basic idea for fabricating the composites is to combine the hot working nature of friction stir processing (FSP) and the exothermic reaction between aluminum and transition metals (Al-Fe, Al-Mo) or metal oxides (Al-Fe2O3). In the Al-Fe alloy, in situ Al–Fe reaction can be induced during FSP and form Al-Al13Fe4 composite. The size of reinforcing particles formed by the in-situ reaction is ~100 nm. In Al-Mo alloys, fine Al-Mo intermetallic particles with an average size of ~200 nm were formed and uniformly dispersed in the aluminum matrix by FSP. The Al-Mo intermetallic particles were identified mainly as Al12Mo with minor amount of Al5Mo. The exothermic reaction could result in local melting of Al at the Al/TM interface, and the liquid Al may accelerate the reaction. In addition, it is suggested that the critical mechanism responsible for the rapid reaction and the formation of nanometer sized particles in FSP is the effective removal of the Al-TM intermetallic phase from the Al-TM interface, maintaining an intimate contact between TM and Al. In the Al-Fe2O3 system, the reactions taking place during FSP includes the thermite reaction (2Al +Fe2O3 → Al2O3 + 2Fe), and the reaction between the reduced Fe and Al to form Al13Fe4. In the FSPed Al-Fe2O3 specimens, there are two types of second phase particles, Al13Fe4 and Al2O3. The Al2O3 particles (about 10 nm in size) usually appear as a cluster of 100-200 nm in diameter. There are two types of Al2O3 phases existed in the Al matrix after FSP passes, depending on the content of Fe2O3. One is γ-Al2O3 in Al-2Fe2O3 specimens, and the other is α-Al2O3 in Al-4Fe2O3 specimens. It is suggested that the formation of different type of Al2O3 particles in the Al-Fe2O3 composites may be attributed to different heat release in each system. The lower heat release in Al-2Fe2O3 sample favors the formation of the while the higher heat release in Al-4Fe2O3 sample results in the α-Al2O3. The Al-Al13Fe4/Al2O3 composite produced by FSP exhibits both high strength and good tensile ductility. The higher strength in Al-Fe2O3 specimen may be due to the presence of fine Al2O3 particles. The flow stress of the Al-4Fe2O3 composite can maintain at 100 MPa even at 773 K. The good thermal stability and high temperature strength of Al-Al13Fe4/Al2O3 composites could be attributed to the fine dispersion of second phase particles in the aluminum matrix, especially the nanometric Al2O3 particles. These Al2O3 particles are very stable at elevated temperatures, even after long time exposure at 873 K. The temperature excursion in FSP is determined by both the FSP parameters and the exothermic reaction involved. The peak temperature in Al-Fe or Al-Fe2O3 system during FSP was calculated as a function of the fraction of Fe or Fe2O3 reacted. Based on calculated results, it is noted that with the in situ reaction, the value of can easily reach the melting point of Al, especially for the Al-Fe2O3 system. The reaction mechanism and microstructure evolution during FSP are discussed. |
目次 Table of Contents |
論文審定書................................................................................................................................ I 誌謝............................................................................................................................................ II 中文摘要.................................................................................................................................... IV Abstract....................................................................................................................................... VI CONTENTS ...............................................................................................................................VIII List of Table................................................................................................................................ XI List of Figure Captions................................................................................................................XII Chapter 1 Introduction.............................................................................................................. 1 Chapter 2 Literature review...................................................................................................... 5 2-1 Metal matrix composites ............................................................................................ 5 2-1-1 In-situ metal matrix composites...................................................................... 5 2-1-2 Fabrication of metal matrix composites via powder metallurgy route ........... 8 2-1-3 The strengthening mechanisms in metal matrix composites .......................... 9 2-2 Friction stir processing............................................................................................... 12 2-2-1 Fundamental principles................................................................................... 12 2-2-2 Thermal history............................................................................................... 13 2-2-3 Tool tilt angle.................................................................................................. 14 2-2-4 Defect formation ............................................................................................. 15 2-2-5 Applications .................................................................................................... 16 2-3 Al-TM systems........................................................................................................... 17 2-3-1 Al-Fe alloys..................................................................................................... 17 2-3-2 Al-Mo alloys ................................................................................................... 19 2-4 Al-Fe2O3 systems ....................................................................................................... 21 2-4-1 Al-Fe-O phase diagram................................................................................... 21 2-4-2 Al/Fe2O3 reaction and applications................................................................. 21 2-4-3 Al2O3 ............................................................................................................... 24 2-5 Alloys for high temperature applications ................................................................... 24 Chapter 3 Experimental procedures and materials ................................................................... 26 3-1 Materials..................................................................................................................... 26 3-2 Fabrication of billets for friction stir processing........................................................ 26 3-2-1 Powder mixing................................................................................................ 26 3-2-2 Cold compaction ............................................................................................. 27 3-3 Friction stir processing (FSP)..................................................................................... 27 3-4 Microstructure Analysis ............................................................................................. 27 3-4-1 Microscopic observation................................................................................. 27 3-4-2 X-ray diffraction (XRD) ................................................................................. 28 3-4-3 Differential scanning calorimetry (DSC) analysis.......................................... 28 3-4-4 Transmission electron microscopy (TEM) ..................................................... 28 3-5 Mechanical properties ................................................................................................ 28 3-5-1 Microhardness measurement .......................................................................... 28 3-5-2 Tensile and compressive tests at ambient temperature ................................... 29 3-5-3 Elevated temperature compressive tests ......................................................... 29 Chapter 4 Results...................................................................................................................... 30 4-1 Al-Fe system .............................................................................................................. 30 4-1-1 Microstructure evolution................................................................................. 30 4-1-2 Mechanical properties of Al-Al13Fe4 composites ........................................... 34 4.2 Al-Mo system............................................................................................................. 35 4-2-1 Microstructure of the Al-Mo specimens ......................................................... 35 4-2-2 Influence of tool traversing speed and post-FSP heat treatment..................... 36 4-2-3 Mechanism of Al-Mo reaction during FSP..................................................... 38 4-2-4 Mechanical properties..................................................................................... 39 4-3 Al-Fe2O3 alloys .......................................................................................................... 40 4-3-1 Microstructure of Al-2Fe2O3 alloy processed by FSP .................................... 41 4-3-2 Microstructure of Al-4Fe2O3 alloy processed by FSP .................................... 43 4-3-3 Mechanical properties..................................................................................... 45 4-3-4 Strength at elevated temperature..................................................................... 46 Chapter 5 Discussions .............................................................................................................. 48 5-1 The temperature excursion with in situ reaction during FSP..................................... 48 5-2 Reactions and microstructure development during FSP ............................................ 53 5-2-1 Reactions in Al-TM systems during FSP........................................................ 53 5-2-2 Reactions in Al-Fe2O3 systems during FSP.................................................... 55 5-3 The Al13Fe4 particles formed in Al-Fe and Al-Fe2O3 systems................................... 57 5-4 The strengthening due to Al2O3 nanoparticles ........................................................... 58 5-5 Young’s modulus of Al-10Fe and Al-Fe2O3 composites produced by FSP............... 59 Chapter 6 Conclusions.............................................................................................................. 62 Tables.......................................................................................................................................... 65 Figures ........................................................................................................................................ 71 Reference .................................................................................................................................... 132 |
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