本研究旨在藉由摩擦攪拌製程(Friction stir process)誘發原位反應(In-situ reaction)以製造原位鋁基複合材料。透過調控摩擦攪拌製程參數(轉速、走速、道次)釐清反應量與參數間的關係，以及原位反應機制的研究，並進一步改良合金設計，提升反應量與強化效果。由摩擦攪拌製程所引進的大量塑性變形可提供細化微結構的效果，增加反應物間的接觸；而製程所引入的摩擦熱可進一步觸發置換反應(Displacement reaction)產生氧化鋁並釋出大量的反應熱。各系統之粉體(鋁與氧化矽；鋁與氧化銅；鋁、鎂與氧化銅)均勻混合以冷壓製成試棒，其中，鋁與氧化矽及鋁與氧化銅之試棒透過燒結提升試棒強度以利於摩擦攪拌製程進行。
在鋁與氧化矽系統中，摩擦攪拌製程成功的誘發鋁與氧化矽間的反應，生成穩定相氧化鋁(α-Al2O3)及矽，同時散佈於極細晶(1 μm)的基材中。在固定走速的條件下，反應量係與轉速及道次成正相關。降低走速可提高製程時間進而增加反應量。微結構觀察顯示，主要的強化相是奈米氧化鋁顆粒(20 nm)，生成於鋁與氧化矽界面，經由摩擦攪拌製程散佈至基材中，普遍以氧化鋁團簇(Cluster)的型態存在。該強化相可有效的阻礙差排滑移，進而以Orowan strengthening提升強化效果。此外，熱處理(873 K/1hr)後可達完全反應，蓋因氧化鋁未完全包覆氧化矽使得氧化矽與鋁間仍保有接觸。機械性質方面，鋁與氧化矽試棒經FSP-500-15-4後，抗拉強度可達319 MPa，延展性為0.13。
在鋁與氧化銅系統中，散佈於基材中的氧化鋁是為鋁與氧化銅反應所生成，而銅與鋁反應後，則形成介金屬化合物(θ-Al2Cu)。此複材主要的強化相為奈米尺寸的氧化鋁，該氧化鋁為非晶質，經電子束照射後，相變態為γ-Al2O3。此外，殘餘的氧化銅具有核殼結構(Core-shell structure)，核心由氧化銅及氧化亞銅組成，殼層則由非晶質氧化鋁構成。試棒經摩擦攪拌製程後，輔以熱處理未能有效的提升反應量，歸因於非晶質氧化鋁形成阻障層致使反應無法被熱處理引發。
鎂添加於鋁氧化銅系統中，藉由鎂與氧化銅反應取代鋁與氧化銅反應，獲得提升反應量的結果。鎂與氧化銅反應後，生成奈米尺寸的氧化鎂顆粒(10 nm)，常以團簇(Cluster)型態存在與基材中，是為主要的強化相。鋁與銅之介金屬化合物(θ-Al2Cu)尺寸約為 200 nm。經摩擦攪拌製程後，鋁晶粒細化至0.6 μm。機械性質顯示，複材(Al-10Mg-10CuO)楊氏係數達88 GPa，相較鋁與氧化銅系統之複材，展現優異的機械性質，顯示鎂添加於鋁-氧化銅系統中，可有效的提升反應量及機械性質。

Aluminum matrix composites reinforced with nanometer-sized particles were produced from powder mixture of Al and oxides by using friction stir processing (FSP). This approach combined the hot working nature of FSP and exothermic reactions between Al and oxides. In this study, composites synthesized from Al-SiO2, Al-CuO and Al-Mg-CuO were investigated, and the microstructure and mechanical properties of the composites were characterized.
In the Al-SiO2 composites, Al2O3 particles were produced in situ by oxide-aluminum displacement reactions. The Al2O3 particles were formed at the Al/SiO2 interface, and dispersed in the aluminum matrix by the stirring action of the rotating tool during FSP. Microstructural examinations revealed the Al2O3 particles present mainly in the form of clusters of nano-sized (approximately 20 nm) particles, which were identified as α-Al2O3. Because of the fine dispersion of nano-sized particles in an ultrafine-grained aluminum matrix, the composites exhibit superior tensile strength and ductility. Quantitative phase analysis indicated that the extent of the Al-SiO2 reaction increased in conjunction with an increasing tool rotation rate and a decreasing tool traverse speed in FSP.
In the Al-CuO composite, the in situ formed reinforcements include nanometer-sized Al2O3 and Al2Cu particles. These Al2O3 nano-particles were identified as amorphous in the as-FSPed condition. The average Al grain size in the FSPed composite was approximately 1 μm. The composite exhibited enhanced strength. The major contributions to the high strength of the composite are the ultrafine grained structure of aluminum matrix and the fine dispersion of nanometer-size reinforcing particles inside aluminum grains.
Aluminum based in situ composite was synthesized from powder mixture of Al/Mg/CuO by using friction stir processing (FSP). Microstructure characterization indicates that in situ formed MgO and Al2Cu nano-particles are uniformly distrubuted in submicron-grained aluminum matrix. Because of the large amount of nanometer-size reinforcements in a submicron-grained matrix, the composite exhibits superior Young’s modulus and strength. The reaction mechanism responsible for the in situ formation of MgO and Al2Cu particles in FSP is discussed. This work has demonstrated the beneficial effect of utilizing the Mg/metal-oxide displacement reaction in the synthesis of aluminum based in situ composite.

中文摘要 I
Abstract III
Contents V
List of Table VII
List of Figure Captions VIII
Chapter 1 Introduction 1
Chapter 2 Literature review 5
2.1 Friction stir process (FSP) 5
2.1.1 Fundamentals of FSW/FSP 5
2.1.2 Application of FSP for microstructure refinement 7
2.1.3 Fabrication of composites by using FSP 8
2.2 Strengthening mechanisms in particle reinforced metal matrix composites 9
2.3 In situ Al-TM composites produced by FSP 11
2.4 In situ composites synthesized by thermite reaction 15
2.5 In situ aluminum composites produced by combining thermite reaction and FSP 19
Chapter 3 Experimental procedures 22
3.1 Materials 22
3.2 Friction stir processing (FSP) 22
3.3 Microstructure characterization 23
3.4 Mechanical tests 23
3.5 Thermal analysis 24
Chapter 4 Results 25
4.1 Al-SiO2 system 25
4.1.1 Microstructure 25
4.1.2 Effect of FSP parameters 27
4.1.3 Mechanical properties 28
4.1.4 Effect of post-FSP heat treatment 29
4.2 Al-CuO system 31
4.2.1 Microstructure 31
4.2.2 Mechanical properties 33
4.2.3 Effect of post-FSP heat treatment 34
4.2.4 Effect of CuO content on the mechanical properties of FSPed Al-xCuO samples 35
4.3 Al-Mg-CuO system 38
4.3.1 Microstructure 38
4.3.2 Mechanical properties 39
4.3.3 Effect of chemical composition on the mechanical properties of FSPed Al-Mg-CuO 40
Chapter 5 Discussions 43
5.1 The effect of FSP parameters on the in situ Al-SiO2 reaction 43
5.2 I In-situ reactions in Al-SiO2 and Al-CuO during FSP 44
5.2.1 Al-SiO2 system 45
5.2.2 Al-CuO system 47
5.2.3 Polymorphs of Al2O3 resulted from thermite reactions 49
5.3 Effect of Mg on the in situ reaction in Al-CuO system 50
5.4 Tension-compression asymmetry 52
Chapter 6 Conclusion 54
Tables 56
Figures 62
Reference 91

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