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論文名稱 Title |
經高比率擠型AZ31鎂合金之低溫高速超塑性研發與變形機構之分析 Development and Analysis of Low Temperature and High Strain Rate Superplasticity in High-Ratio Extruded AZ31 Mg Alloys |
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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 |
224 |
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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 |
2005-04-26 |
繳交日期 Date of Submission |
2005-06-17 |
關鍵字 Keywords |
超塑性、織構、鎂合金、等徑轉角擠形 Texture, Superplasticity, ECAP, Magnesium alloy |
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統計 Statistics |
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中文摘要 |
本研究將商用AZ31鎂合金經簡易擠型加工後,可使該合金呈現低溫及高速超塑性。經擠型後的晶粒可細化至1-4 μm。加工後的鎂板可得到50%優異的室溫伸長量,在高速超塑性測試條件下也獲得1000%的伸長量。同時鎂合金也利用等徑轉角擠製法(ECAP)來達到合金內部晶粒細化。在125及150oC低溫條件下可達到200%和461%的伸長量,該測試溫度分別為0.43與0.46鎂合金熔點溫度。結果顯示經由加工後的鎂合金可以達到低溫超塑性。 利用x-ray繞射圖形,背向散射電子繞射(EBSD)以及穿透式電子顯微鏡(TEM)選區繞射的方法,針對擠型及等徑轉角擠製後的材料,研究其織構行為及高角度晶界之比率。經一系列實驗分析,從結果可觀察到擠型棒材的主要織構為<10-10>平行擠型方向,等徑轉角擠製後的織構為<-2-576>平行擠型方向。至於擠型板材,主要織構則為{0002}基面平行擠型方向。 本實驗透過不同的拉伸溫度測試,觀察不同溫度區間的變形機構。在150 ~ 200oC,變形機構以差排滑移為主,計算後之活化能所對應機構為熱活化差排滑移。在250 ~ 300oC之測試區間,變形機構則以晶界滑移為主,控制速率之主要擴散步驟為晶界擴散。 |
Abstract |
There have been numerous efforts in processing metallic alloys into fine-grained materials, so as to exhibit high strain rate superplasticity (HSRSP) and/or low temperature superplasticity (LTSP). The current study is to apply the most simple and feasible one-step extrusion method on the commercial AZ31 magnesium billet to result in low temperature and high strain rate superplasticity (LT&HSRSP). The one-step extrusion was undertaken using a high extrusion ratio at 250-350oC, and the grain size after one-step extrusion became ~1-4 mm. The processed AZ31 plate exhibited high room temperature tensile elongation up to 50%, as well as superior LTSP and/or HSRSP up to 1000%. Meanwhile, the AZ31 alloy was also conducted by equal-channel angular pressing (ECAP). It is demonstrated that an elongation of 461% may be attained at a temperature of 150oC, equivalent to 0.46 Tm where Tm is the absolute melting temperature. This result clearly demonstrates the potential for achieving low temperature superplasticity. A detailed investigation, using x-ray diffraction (XRD), electron back scattering diffraction (EBSD), and transmission electron microscopy / selected area diffraction (TEM/SAD), revealed different textures in the as-extruded and as-ECAP bars. These dominant textures were characteristic of <10 0>//ED in the extruded bars and < 76>//ED in the ECAP condition, where ED is the extrusion direction. The results show that the basal planes tend to lie parallel to the extrusion axis in the extruded bars but there is a rearrangement during ECAP and the basal planes become reasonably aligned with the theoretical shearing plane. As to the extruded plates, the {0002} planes tended to lie on the plane that contains the extrusion axis. At different tensile temperatures, different deformation mechanisms would be dominant. Over the lower loading temperatures within 150-200oC, the true strain rate sensitivity, mt, after extracting the threshold stress is determined to be 0.28, suggesting that power-law dislocation creep but the Qt value is not related to any creep mechanism. It should be partly due to thermal activated dislocation slip mechanism. However, more data need to be tested systematically this part in the future study in order to define the correct deformation mechanism. As to the loading temperatures over 250-300oC, the mt value and the true activation energy for the extruded specimens are calculated to be ~0.4-0.5 and ~90-100 kJ/mol, implying that the major deformation mechanism is grain boundary sliding plus minor solute drag creep, with the rate controlling diffusion step being the magnesium grain boundary diffusion. |
目次 Table of Contents |
Table of Content i List of Tables v List of Figures vii Abstract xiii 中文提要 xv 誌謝 xvi Chapter 1 Introduction 1 1.1 The basic character of superplastic materials 1 1.2 Types of superplasticity 3 1.2.1 Fine structure superplasticity (FSS) 3 1.2.2 Internal stress superplasticity (ISS) 4 1.2.3 High strain rate superplasticity (HSRSP) or low temperature superplasticity (LTSP) 5 1.2.4 Coarse grained superplasticity (CGSP) 5 1.2.5 Other mechanisms 7 1.3 The development and application of magnesium alloys 7 1.4 Properties of magnesium alloys 9 1.4.1 The classification of magnesium alloys 9 1.4.2 Grain size 10 1.4.3 Solute content in magnesium alloys 10 1.4.4 Grain refining processes 12 1.4.4.1 Rapid solidification (RS) 12 1.4.4.2 Powder metallurgy (PM) 13 1.4.4.3 Rolling 14 1.4.4.4 Equal channel angular pressing (ECAP) 14 1.4.4.5 Forging 17 1.4.4.6 Extrusion 17 1.4.4.7 Double extrusion and cyclic (reciprocal) extrusion 18 1.4.4.8 A two-step processing route 19 1.4.5 Room temperature tensile properties 20 1.5 Superplastic behavior in magnesium alloys 20 1.5.1 HSRSP in magnesium alloys 21 1.5.2 LTSP in magnesium alloys 22 1.5.3 Deformation mechanisms 22 1.6 Cavitation 23 1.7 Crystal orientation and overview of techniques for microtexture determination 24 1.7.1 Overview of techniques for microtexture determination 25 1.7.2 The basic principles and setup of typical EBSD system 25 1.7.3 The study of texture in magnesium alloy 26 1.8 Motive of the research 27 Chapter 2 Experimental Methods 29 2.1 Materials 29 2.2 Grain refining processes 30 2.2.1 Extrusion 30 2.2.2 Processing route of equal-channel-angular pressing 31 2.3 Evaluation of superplasticity behavior 32 2.3.1 Tensile tests 32 2.3.2 Strain uniformity 32 2.3.3 Strain rate sensitivity (m-value) 33 2.4 Microstructure observations 33 2.4.1 Grain size and cavitation 33 2.4.2 TEM 34 2.4.3 Thermal stability 34 2.4.4 Fractography examinations 35 2.5 Microhardness measurements 35 2.6 Texture characterization 35 2.6.1 X-ray diffraction 35 2.6.2 EBSD 36 2.6.3 TEM 36 Chapter 3 Experimental Results and Discussions 37 3.1 Microstructure characterization 37 3.1.1 Grain size evolution 37 3.1.2 Influence of annealing temperature and time 38 3.1.3 Microstructures in specimens subject to different superplastic strains and temperatures 39 3.2 Microhardness 40 3.3 Tensile properties 41 3.3.1 Room temperature tensile properties 41 3.3.2 Superplastic behavior over 150-300oC and 10-4-10-1 s-1 43 3.3.2.1 Comparison of LTSP in the E1 and E1B specimens 43 3.3.2.2 Comparison of the E1 and E2 specimens processed to different extrusion ratios 45 3.3.2.3 Comparison of the E2 and the E2B specimens processed into different geometric shapes 45 3.3.2.4 Comparison of the E2B and E3 specimens processed to different extrusion ratios 47 3.3.2.5 Comparison of the E3 and E3B specimens to different plate thicknesses 47 3.3.3 Plastic anisotropy 49 3.3.4 Fractography after tensile testing 50 3.4 Texture characterization 52 3.4.1 Texture determined by X-ray diffraction patterns 52 3.4.2 Texture evolution during static annealing 53 3.4.3 Texture determined by X-ray pole figures 54 3.4.4 Texture determined by EBSD 55 3.4.5 Texture determined by TEM 56 3.4.6 Grain misorientation distributions 57 Chapter 4 Analyses of deformation Mechanisms 61 4.1 Temperature dependence of elastic modulus 61 4.2 Analysis of deformation mechanisms 61 4.2.1 Apparent strain rate sensitivity, ma 63 4.2.2 Threshold stress (sth) and true stain rate sensitivity (mt) 66 4.2.3 True activation energy, Qt 67 4.3 Comparison for specimens processed by ECAP 69 4.4 Comparison between extruded AZ31 and AZ91 alloys 70 4.5 Texture evolution during thermomechanical treatments 70 4.6 Design for continuous industry processing line 72 Chapter 5 Conclusions 74 References 77 Tables 84 Figures 117 LIST OF TABLES Table 1-1 Summarizes the typical HSRSP materials 84 Table 1-2 List the reports on LTSP 85 Table 1-3 Some characters compared among magnesium, steels, cast irons, copper, aluminum alloys and engineering plastics 86 Table 1-4 The physical or mechanical characters in magnesium 87 Table 1-5 The standard four-part ASTM alloy designations system and temper for the magnesium alloys 88 Table 1-6 The relationship between grain size and mechanical properties of AZ91 89 Table 1-7 The effect of separate solute additions of elements on the mechanical properties 90 Table 1-8 Summary of ECAP applications for Mg alloys 92 Table 1-9 Evidence for superplasticity at low temperature after ECAP 94 Table 1-10 Room temperature tensile properties after ECAP 95 Table 1-11 Comparison of superplastic properties in commercial AZ and ZK series Mg alloys without ECAP 96 Table 1-12 Summary of tensile elongation of Mg based materials at room temperature 98 Table 1-13 HSRSP and LTSP in the Magnesium alloys 99 Table 1-14 Summary of superplastic behaviors, deformation mechanisms, and activation energy of Mg based materials 100 Table 2-1 Chemical composition of the AZ31 (in wt%) 101 Table 2-2 The AZ31 specimens in this study 102 Table 3-1 Grain size and room temperature tensile properties of the AZ31 billet, extruded and ECAP specimens 103 Table 3-2 The variation of grain size for the E3 specimens after static annealing .104 Table 3-3 Room temperature tensile properties at 1x10-3 s-1 for the E3 specimens after extrusion and post-annealing 105 Table 3-4 Room temperature tensile properties at 1x10-3 s-1 for the E3B specimens after extrusion and post-annealing 106 Table 3-5 Comparison of the mechanical properties of the E1 and E1B AZ31 specimens with and without ECAP 107 Table 3-6 Comparison of the mechanical properties of the E1 and the E2 specimens processed to different extrusion ratios 108 Table 3-7 Comparison of the mechanical properties of the E2 and the E2B specimens processed into different geometric shapes 109 Table 3-8 Comparison of the mechanical properties of the E2B and the E3 specimens processed to different extrusion ratios 110 Table 3-9 Comparison of the E3 and the E3B specimens to different thicknesses 111 Table 3-10 Summary of the measured grain size and X-ray peak intensity ratio for the (0002) reflection over the (10 1) and (10 3) reflections for the E3 specimens 112 Table 3-11 Schmid factors calculated for E1 and E1B specimens 113 Table 4-1 The measured apparent strain rate sensitivity ma values based on the true stress-strain curves over strain rate of 1x10-1-1x10-4 s-1 114 Table 4-2 The measured strain rate sensitivity m-value for the E2B samples based on the jump strain rate tests 115 Table 4-3 Comparison of AZ31B and AZ91D Mg alloys processed by high-ratio (HR) extrusion and ECAP 116 LIST OF FIGURES Figure 1-1 High temperature deformation behavior of fine-grained materials 117 Figure 1-2 Changes in hardness after heating at various temperatures for 2 hours, (a) P/M, (b) I/M materials 118 Figure 1-3 Tensile strength and elongation of the P/M and I/M materials at different test temperatures 119 Figure 1-4 Schematic drawing of equal channel angular pressing. 120 Figure 1-5 Illustration of the principle of an EBSD system 121 Figure 1-6 Illustration of the set-up of an EBSD system 121 Figure 1-7 Schematic Euler angles (j1, f, j 2), which would specify an orientation 122 Figure 1-8 Schematic illustration of the misorientation angle between two grains 122 Figure 2-1 Processing routes for this research 123 Figure 2-2 Specimen configurations of (a) extruded rod with a gauge length of 8.3 mm and (b) extruded sheet with a gauge length of 5.5 mm 124 Figure 2-3 Schematic illustration of the jump-strain-rate test 125 Figure 2-4 Schematic illustration of the procedure used for taking the microhardness measurements on the transverse-sectional plane 126 Figure 3-1 The appearances of samples after extrusion and ECAP 127 Figure 3-2 The OM micrographs of the as-received AZ31 billet seen from the cross-sectional plane 128 Figure 3-3 The OM micrographs of the extruded (a) E1, (b) E1B, (c) E2, (d) E2B and (e) E3B specimens 129 Figure 3-4 The OM micrographs of the E3 specimens from the extrusion (a) flat, (b) longitudinal and (c) cross-sectional planes 131 Figure 3-5 Grain structure micrographs of the AZ31 alloy after (a) extrusion to 42:1 at 300oC (OM micrograph, E1 specimen), and (b) further ECAP at 200oC (TEM micrograph, E1B specimen) 132 Figure 3-6 Grain size versus annealing temperature after static annealing holding for 1 h in the extruded E1 and ECAP E1B samples 133 Figure 3-7 Variation of grain size as a function of temperature in the E3 specimen after holding for 1 h in the furnace 134 Figure 3-8 Variation of grain size as a function of time in the E3 specimen at 300oC 134 Figure 3-9 The typical surface topography SEM micrographs taken from the E2B specimens tensile-loaded at 200oC and 6x10-4 s-1 to different strains: (a) 0.29, (b) 0.71, (c) 1.12, and (d) 1.39 135 Figure 3-10 The typical surface topography SEM micrographs taken from the E2B specimens tensile-loaded at 300oC and 6x10-4 s-1 to different strains: (a) 0.24, (b) 0.71, (c) 1.28, (d) 1.80, and (e) 2.03 136 Figure 3-11 OM micrographs of the E3 specimens tensile-loaded at 300oC and at 1x10-3 s-1 to different strains: (a) 0.25, (b) 0.47, (c) 0.93, and (d) 1.23 137 Figure 3-12 The microhardness results taken from the transverse-sectional of samples processed by extrusion E1 (upper), and ECAP E1B (lower) specimens 138 Figure 3-13 Microhardness of the AZ31 alloy as a function of grain size 139 Figure 3-14 Typical stress-strain curves for the billet, E1 and E1B specimens tensile-loaded at room temperature and 1´10-3 s-1 140 Figure 3-15 Variation of the yield and ultimate tensile stresses of the E3 extruded plate as a function of d-1/2 in accordance with the Hall-Petch relationship 141 Figure 3-16 The macroscopic fracture morphology of the E1 and E1B specimens 142 Figure 3-17 The engineering stress versus engineering strain curves tensile-loaded at RT and the appearance of the E3B specimen after tensile testing 143 Figure 3-18 The true stress versus true strain curves for the E1 (a)(b) and E1B (c)(d) samples tensile-loaded at 150 and 200oC 144 Figure 3-19 Tensile specimens of E1 and E1B before test and tested at 1x10-4 s-1 and 150oC 146 Figure 3-20 Tensile elongation versus strain rate at 150 to 250°C for the (a) E1 and (b) E1B specimens 147 Figure 3-21 The true stress versus true strain curves and the appearance of the E1B specimen after static annealing at 125oC for 7 h tensile-loaded at 125oC and 1x10-4 s-1 148 Figure 3-22 The variation of elongation to failure as a function of test temperature 149 Figure 3-23 The variation of elongation to failure as a function of strain rate 149 Figure 3-24 The UTS versus tensile temperatures for the E2 and E2B specimens 150 Figure 3-25 The variation of elongation to failure as a function of test temperature for E2 and E2B 151 Figure 3-26 Tensile specimens of the AZ31 E2 extruded rods: (a) fixed strain rate at 1x10-3 s-1 and (b) fixed tensile temperature at 300oC 152 Figure 3-27 Tensile specimens of the AZ31 E2B extruded plates fixed strain rate at 1x10-3 s-1 153 Figure 3-28 Typical true stress and strain curves for the E3 specimens recorded from tensile tests at different initial strain rates for the loading temperatures of 150-300oC 154 Figure 3-29 The UTS versus tensile temperatures for the E2B and E3 specimens 156 Figure 3-30 Typical true stress and strain curves for the E3B specimens recorded from tensile tests at different initial strain rates for the loading temperatures of (a) 150oC, (b) 200oC, (c) 250oC, (d) 280oC and (e) 300oC 157 Figure 3-31 Variation of the tensile elongation as a function of test strain rate for the AZ31 (a) E3 and (b) E3B specimens 159 Figure 3-32 Representative tensile specimens of the AZ31 E3 extruded plates: (a) 250oC and 1x10-4 s-1, (b) 250oC and 8x10-3 s-1, (c) 280oC and 1x10-4 s-1, (d) 280oC and 8x10-3 s-1, (e) 300oC and 1x10-4 s-1, (f) 300oC and 8x10-3 s-1 160 Figure 3-33 Tensile specimens of the AZ31 E3B extruded plates fixed strain rate at 1x10-3 s-1 161 Figure 3-34 Variation of the tensile elongation as a function of test temperature for the E3 and E3B specimens at a strain rate of 1x10-3 s-1 162 Figure 3-35 Variation of cross-sectional area for the E3 specimens deformed at 300oC and 1x10-3 s-1 to tensile strains of 0.25, 0.47, 0.93, and 1.23 163 Figure 3-36 Variation of R for the E3 specimens deformed at 300oC and 1x10-3 s-1 to different tensile strains 163 Figure 3-37 Variation of cross-sectional area for the E2B specimens that deformed during tensile conditions: (a) 200oC, 6x10-4 s-1, (b) 300oC, 6x10-4 s-1, (c) 300oC, 1x10-2 s-1 164 Figure 3-38 Variation of R for the E2B specimens to different elongations 165 Figure 3-39 SEM micrographs of fractures observed in the (a) billet and (b) E3B specimens after tensile test at room temperature 166 Figure 3-40 SEM micrographs of fractures observed in the (a) E1 and (b) E1B specimens after tensile test at room temperature 167 Figure 3-41 The fracture surface of the E1B specimen after tensile testing at 150oC and different strain rates of (a) 1x10-2, and (b) 1x10-4 s-1 168 Figure 3-42 The fracture surfaces of the E3 specimens tensile-loaded at 300oC and (a) 1x10-3, (b) 8x10-3, and (c) 1x10-1 s-1 169 Figure 3-43 The fracture surfaces of the E3B specimens tensile-loaded at 150oC and (a) 1x10-4, (b) 1x10-3, (c) 2x10-3 and (d) 8x10-3 s-1 170 Figure 3-44 The fracture surfaces of the E3B specimens tensile-loaded at 1x10-3 s-1 and (a) 150, (b) 250, (c) 280 and (d) 300oC 171 Figure 3-45 X-ray diffraction patterns of the AZ31 Mg alloy showing the apparent change in texture after severe extrusion: (a) complete random Mg powders, (b) the cross-sectional plane of the as-received billet processed by semi-continuous casting, and (c) the flat plane of the E3 extruded plate 172 Figure 3-46 X-ray diffraction patterns taken from the E1 sample processed with extrusion ratio of 42:1 at 300oC : (a) longitudinal plane and (b) transverse cross-sectional plane 173 Figure 3-47 X-ray diffraction patterns taken from the E1B sample processed after ECAP for 8 passes at 200oC : (a) longitudinal plane and (b) transverse cross-sectional plane 174 Figure 3-48 X-ray diffraction patterns taken from the severely extruded E3 specimen after further annealing for 10 h at (a) 150oC, (b) 250oC, (c) 300oC, and (d) 350oC 175 Figure 3-49 X-ray diffraction patterns taken from the severely extruded E3 specimen after further annealing for 1 h at (a) 150oC, (b) 250oC, (c) 300oC, and (d) 350oC 176 Figure 3-50 The XRD (0002), (10 0) and (10 1) pole figures of the E1 and E1B specimens 177 Figure 3-51 The XRD (0002) pole figures of the E2B and E3 plate specimens 178 Figure 3-52 The EBSD (0002), (10 0) and (10 1) pole figures for the extruded E1 and ECAP E1B conditions 179 Figure 3-53 The TEM bright field images and diffraction patterns taken from the extruded E1 condition 180 Figure 3-54 The TEM bright field images and diffraction patterns taken from the ECAP E1B condition 182 Figure 3-55 The TEM bright field images and diffraction patterns taken from the extruded E2 specimen 184 Figure 3-56 The TEM bright field images and diffraction patterns taken from the extruded E3 specimen 186 Figure 3-57 The inverse pole figures determined by TEM diffraction pattern analysis: (a) E1 and (b) E1B specimens 187 Figure 3-58 The inverse pole figures determined by TEM diffraction pattern analysis in the E2 specimen 188 Figure 3-59 Schematic illustration of the dominant textures in the extruded E1 and ECAP E1B conditions 189 Figure 3-60 Examples of the SAD patterns taken from various adjacent grains in E1 190 Figure 3-61 Examples of the SAD patterns taken from various adjacent grains in the E1B specimen 191 Figure 3-62 Two representative misorientation distributions determined by TEM for the (a) E1 and (b) E1B specimens 192 Figure 3-63 The representative misorientation distributions determined by TEM for the E2 specimen 193 Figure 3-64 Two representative misorientation distributions determined by EBSD for the (a) E1 and (b) E1B specimens 194 Figure 4-1 The flow stress against strain rate curves at 150 to 200oC for the E1B specimen 195 Figure 4-2 The flow stress at e=0.3 against strain rate curves at 150 to 200oC for the E1, E2 and E3 specimens 196 Figure 4-3 The flow stress at e~0.3 versus strain rate for the E2 and E3 specimens at various temperatures 197 Figure 4-4 The E2 specimen tested at 6x10-4 ~ 1x10-3 s-1 198 Figure 4-5 Threshold stress for the E3 specimen 199 Figure 4-6 Threshold stress for the E1B specimen 200 Figure 4-7 The mt–value could be extracted from the slope of the double logarithm plot of the flow stress versus the strain rate 201 Figure 4-8 True activation energy for the E3 specimen using the true stress exponent nt of 2.5 202 Figure 4-9 True activation energy for the E3 specimen using the true stress exponent nt of 2 203 Figure 4-10 True activation energy for the E1B specimen 204 Figure 4-11 Design of the continuous press forming using heated oil or water bath 205 Figure 4-12 Illustration of continuous industrial system 206 Figure 4-13 Detailed design of the forming machine 207 |
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