博碩士論文 89343004 詳細資訊




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姓名 張志鴻(Chih-Horng Chang)  查詢紙本館藏   畢業系所 機械工程學系
論文名稱 合金元素(銀與鎂)與熱處理對A201鋁合金應力腐蝕與熱穩定性之影響
(Alloying Elements (Silver and Magnesium) on The Stress Corrosion Cracking and Thermal Stability of A201 Aluminum Alloy)
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摘要(中) A201鋁合金(Al-4.6Cu-0.3Mg-0.6Ag)具有高強度與熱穩定性,已廣泛應用於航太與軍事工業。A201鋁合金含銀量介於0.4 wt.%至1 wt.%之間,除原有之θ′相之外,可析出具熱穩定性之強化相Ω,使合金具有極為優良的常溫與高溫(200℃以下)強度,此外在銅含量固定下鎂含量可影響析出相的種類與分布情形(Ω、S′與θ′相),故銀與鎂含量皆為影響Ω析出的重要合金元素。應用於航空設備之高強度Al-Cu鋁合金易受應力腐蝕而破壞,因此A201鋁合金之應力腐蝕敏感性極需重視,而合金的熱處理狀態則會影響應力腐蝕的性質,此外航空器材常須承受高速與空氣摩擦所引發的高溫,故合金於高溫下之熱穩定性為合金相當重要的性質。
基於合金元素與熱處理對於A201鋁合金微結構與性質上的影響,因此本研究將探討合金元素與熱處理對於合金微結構、機械強度、應力腐蝕與熱穩定性之變化與效應,以完整呈現此一高強度鋁合金之特性。
由於銀為刺激Ω相析出的重要合金元素,於本論文中首先將藉由不同銀含量(0、0.3、0.6與0.9 wt.% Ag)之合金,施以頂時效(T6)、過時效(T7)以及回復與再時效(retrogression and reaging,RRA)等不同熱處理製程來探討銀含量對於A201鑄鋁合金強化析出相、機械性質與應力腐蝕敏感性的影響;爾後,再藉由不同銅/鎂比(分別為29、19、8與4)的熱擠製Al-4.6Cu-XMg-0.6Ag合金,探討合金於107、135與155℃下1000小時之熱穩定性。
本論文透過金相、導電度(Electrical Conductivity, %IACS)、微差熱掃瞄(Differential Scanning Calorimetry)與穿透式電子顯微鏡(Transmission Electron Microscopy)等微結構之觀察與分析,配合硬度(HRB)、拉伸與應力腐蝕等合金性質上的試驗,獲得以下結論:Ω相析出量與機械強度隨銀含量增加而增加,但是銀含量高達0.9重量百分比時卻出現抑制θ′相之情形;銀含量不會影響晶界析出物,但高銀含量合金會增加富銅之強化相(Ω與θ′相)整體析出效果,導致應力腐蝕敏感性增加。相較於過時效(T7)熱處理之合金,經頂時效(T6)處理後合金無析出帶較窄,造成明顯的面積效應,導致應力腐蝕性提高,而回復與再時效(RRA)熱處理無法明顯改變晶界析出物型態或降低面積效應,故未能降低鑄造A201鋁合金應力腐蝕敏感性;高鎂含量之合金(即低銅/鎂比),產生大量之銀-鎂(Ag-Mg co-cluster)聚集,引發Ω相大量析出,故此合金擁有高強度與高熱穩定性。
摘要(英) A201 aluminum alloy (Al-4.6Cu-0.3Mg-0.6Ag) has been widely applied in the aviation and military industries due to its very high mechanical strength and thermal stability.
The silver containing, between 0.4 to 1 wt.%, is unequal characteristic of A201 alloy that change the precipitated sequence and lead to trigger precipitation of the thermal stable Ω phase along with θ′ phase of Al-Cu alloy. Due to the precipitated of Ω phase, A201 alloy possess execllent mechanical strength under 200℃. The concentration of magnesium affect the relative distribution of Ω, S′ and θ′ phases at constant copper containing that influence the thermal stability of alloy. Therefore, the concentration of silver and magnesium are both the important factor for precipitation of Ω phase. High strength Al-Cu alloy is known to be damanged by stress corrosion cracking. The heat treatment condition affect the stress corrosion cracking susceptibility of alloy. Moreover, the skin of a super sonic bear aero dynamic heating, thus, the thermal stsbility treat as an serious properties of A201 alloy.
Due to the alloying elements and heat treatment significantly affect the microstructure and properties of A201 alloy, hence, present works attempt to discover the effect of alloying elements (silver and magnesium) and heat treatment on the stress corrosion cracking and thermal stability of A201 aluminum alloy.
For the purpose of reveal the bottom of the effect on of silver and magnesium contain on precipitation of A201 alloy, present work start with made various quantity of silver (0 to 0.9 wt.%) containing alloy, subsequencely heat treated to T6, T7 and RRA condition. Second step of this investigation was performed on the different quantity of magnesium (0.15 to 1.1 wt. %) containing hot extrusion alloys. The alloys were long-term exposed at 105, 135 and 155℃ up to 1000 hours.
Microstructural features were elucidated by optical microscopy, electron probe X-ray microanalysis, measurement of electrical conductivity and differential scanning calorimetry. The microstructure was correlated with Rockwell hardness and tensile testing. The stress corrosion cracking susceptibility of alloy was assessed by performing the slow strain rate test in air and salt solution.
The results of present works revealed that the addition of Ag at a concentration of under 0.6 mass% promoted the precipitation of the Ω and θ’’ phases and the augmentation of hardness of T7 tempered alloys. 0.9 mass% Ag caused the extensive precipitation of the Ω phase, but only mildly suppressed the precipitation of the θ’’ phase, slightly increasing the hardness. The high density of the precipitates of the Ω phase is responsible for the excellent thermal stability under 185℃ exposure for 100 hours and mechanical properties. The Ω precipitates out before the θ’’ phase, and does so more quickly, during the aging process. The continuous grain boundary precipitations and the high Ag concentration alloy that exist high density of the Ω and θ’’ phases caused susceptibility to high stress corrosion cracking. The presence of a wide precipitation-free zone and discontinuous large particles in the grain boundary precipitates caused the T7 alloy to have a low susceptibility to stress corrosion cracking. The alloys tempered to the retrogression and reaging condition cannot reduce susceptibility of the Al-Cu-Mg-Ag alloy to stress corrosion cracking. Decreasing the Cu/Mg ratio of alloy by furthermore addition of Mg leads Ω to become major strengthening phase after ageing treatment. Therefore, the hot extrusion process did not bother the precipitated of Ω phase. However, the 1.1 wt. % Mg contain alloy was too hard and brittle lad to serious cracking occurred following hot extrusion.
關鍵字(中) ★ Al-Cu-Mg-Ag合金
★ 應力腐蝕
★ 微差熱掃瞄
★ 導電度(%IACS)
★ 穿透式電子顯微鏡
關鍵字(英) ★ Stress corrosion cracking
★ Al-Cu-Mg-Ag alloy
★ Electric Conductivity (%IACS)
★ Transmission Electron Microscopy
★ Differential Scanning Calorimetry
論文目次 總 目 錄
――――――――――― 中英文摘要 ―――――――――――
中文摘要 I
英文摘要 III
―――――――――――― 誌 謝 ―――――――――――――
誌 謝 V
――――――――――――― 目錄 ―――――――――――――
總目錄 VI
表目錄 XI
圖目錄 XIII
―――――――― 第一章 研究背景與文獻回顧 ――――――――
1.1 A201合金簡介 1
1.1.1鋁合金簡介 1
(a) 鋁合金發展歷史 1
(b) 鋁合金分類 2
1.1.2 A201鋁合金發展與性質簡介 4
(a) A201鋁合金發展過程 4
(b) A201鋁合金之優、缺點與特色 6
1.2 A201鋁合金基礎理論 9
1.2.1合金凝固特性 9
1.2.2合金熱處理 11
(a) 高溫固溶處理 12
(b) 低溫淬火 13
(c) 時效處理 14
1.2.3合金強化機制與析出序列 16
(a) Al-Cu合金 16
(b) Al-Cu-Mg 合金 17
(c) Al-Cu-Mg-Ag 合金 17
1.2.4 Ω相析出機制 18
1.2.5 Cu/Mg比對於析出影響 22
1.2.6強化相熱穩定性 24
1.2.7合金相變化檢測與分析 25
(a) 儀器原理與技術 25
(b) 數值模擬分析 26
1.2.8合金加工影響 29
1.3 A201鋁合金應力腐蝕 30
1.3.1應力腐蝕簡介 30
1.3.2 A201鋁合金時效處理對應力腐蝕影響 33
1.3.3應力腐蝕的試驗方法 36
1.4 研究背景、動機與目的 37
1.4.1研究背景與動機 37
1.4.2 研究目的 40
―――――――――― 第二章 實驗方法 ――――――――――
2.1 合金準備與鑄造 41
2.1.1 不同銀含量合金之製作(合金A、B、C與D) 41
2.1.2不同銅/鎂比合金之製作 (合金E、F、G與H) 44
2.1.3 合金熱擠製 44
2.2 熱處理 44
2.2.1 標準時效處理 44
2.2.2長期時效處理 45
2.3 微結構觀察與分析 46
2.3.1 光學顯微鏡 46
2.3.2 電子微探儀 46
2.3.3掃描式電子顯微鏡 47
2.3.4導電度量測 47
2.3.5熱差掃瞄分析 47
2.3.6穿透式電子顯微鏡 48
2.4機械性質試驗 49
2.4.1 硬度試驗 49
2.4.2 拉伸試驗 49
2.4.3 慢應變速率拉伸: 應力腐蝕評估 50
―――――――――― 第三章 結果與討論 ――――――――――
3.1銀含量與熱處對析出相、機械性質與應力腐蝕影響 影響 52
3.1.1 微結構分析 53
(a) 光學顯微鏡觀察與電子微探儀分析 53
(b) 導電度量測 59
(c) 熱差掃瞄分析 62
(d) 穿透式電子顯微鏡觀察 72
3.1.2 機械性質試驗 79
(a) 硬度試驗 79
(b) 拉伸試驗 84
3.1.3應力腐蝕試驗 89
3.1.4結論 94
3.2銅/鎂比對熱擠製Al - 4.6%Cu – XMg - 0.6Ag合金熱穩定性影響 96
3.2.1 微結構分析 96
(a) 光學顯微鏡金相觀察 96
(b) 導電度量測 101
(c) 熱差掃瞄分析 104
(d) 穿透式電子顯微鏡觀察 112
3.2.2機械性質試驗 - 拉伸試驗 117
3.2.3熱穩定試驗 120
3.2.4熱擠製影響 124
3.2.5結論 125
――――――――― 第四章 總結論 ―――――――――
總結論 127
――――――― 第五章 未來研究方向 ―――――――
未來研究方向 130
―――――――――― References ――――――――――
References 133
表 目 錄 Table List
Table 1.1 Wrought aluminum alloy series number and their major chemical compositions. 3
Table 1.2 Foundry aluminum alloy series number and their major chemical compositions. 4
Table 1.3 Chemical composition of some selected aluminum alloys. 5
Table 1.4 Tensile properties of some selected aluminum alloys at various temperatures. 7
Table 1.5 Reactions during solidification of A201 casting alloy. 10
Table 1.6 The basic heat treatment designations of aluminum alloys. 12
Table 1.7 The lattice structure and parameter of primary precipitations of A201 alloy. 20
Table 1.8 The electrode potential of solid solution and intermetallic compound of Al-Cu alloys. 35
Table 2.1 Chemical compositions of Al-4.6Cu-0.3Mg-Ag alloys (mass %). 42
Table 3.1 Weight percentage (wt.%) of elements containing of aluminum matrix, net shape and spherical shape phase of as-cast alloys. 55
Table 3.2 The electric conductivity (%IACS) of various silver containing alloys heat treated to several conditions. 60
Table 3.3 The DSC simulation results of heat of precipitation of Ω and θ′ phase for alloys A, B, C and D. 69
Table 3.4 The hardness (HRB) of various silver containing alloys heat treated to several conditions. 80
Table 3.5 The UTS, YS and EL% of the four different Ag-containing alloys tempered to T6, T7 and RRA conditions. 85
Table 3.6 The loss of ductility (%) for the T6, T7 and RRA alloys. 89
Table 3.7 Electrical conductivity (%IACS) of Al-4.6%Cu-Mg-Ag alloys under as-cast, as-quenched, 24-hour natural aging and T7 treatment conditions, and their relative electrical conductivity variations. 101
Table 3.8 The electrical conductivity (%IACS) and relative electrical conductivity variation of Al-4.6%Cu-Mg-Ag alloys which were further exposed in air for times up to 1000hr each at 107℃, 135℃ and 155℃ after T7 tempering. 103
Table 3.9 Heat of precipitation for Ω and θ′ phases under as-quenched and T7 treatment conditions. 105
Table 3.10 Heat of precipitation for the θ′ phases of alloy E, F and G further exposed in air up to 1000hr each at 107℃, 135℃ and 155℃ after T7 treated. 110
Table 3.11 The UTS, YS and EL% of the three different Mg-containing alloys under T7 heat treatment conditions. 118
Table 3.12 Hardness (HRB) of hot-extrusion Al-4.6%Cu-XMg-0.6Ag alloys under as-quenched, one-day natural aging, T7 treatment and exposure in air several times up to 100hr and 1000hr each at 107℃, 135℃ and 155℃ after T7 treatment. 121
圖 目 錄 Figure List
Fig. 1.1 The aluminum end of the aluminum-copper equilibrium diagram. 9
Fig. 1.2 3DAP elemental map of Ag, Mg, Cu and Al in an Al-4.3Cu-0.26Mg-0.7Ag alloy (a) aged for 15 s at temperature of 180℃ after a solution heat treatment, and (b) for Ω phase, an 10 h aged at 180℃. 21
Fig. 1.3 The progress of stress corrosion cracking. 31
Fig. 1.4 The temper verse resistance to stress corrosion cracking of heat treatable aluminum alloys. 35
Fig. 2.1 (a) The metal permanent mold and (b) Casting ingot of 125×100×25 mm3 43
Fig. 2.2 The standard round tension test specimen of ASTM B557M specification. 43
Fig 2.3 The slow strain rate test round bar was immersed in the salt water of 3.5% NaCl solution (pH 6.7) for SCC susceptibility assessment.
Fig. 3.1 The optical microscopic images of (a) Ag-free as-cast alloy A , (b) 0.3 wt.% Ag-containing alloy B, (c) 0.6 wt.% Ag-containing alloy C and (d) 0.9 wt.% Ag-containing alloy D (arrow 1: eutectic CuAl2, 2: S phase). 54
Fig. 3.2 (a) Scanning electron microscopy SEI image of net shape segregation of alloy D, (b) corresponding X-ray map revealing segregation of Cu, (c) SEI image of spherical shape segregation, and corresponding X-ray map of (d) Cu, (e) Mg and (f) Ag. 57
Fig. 3.3 The optical microscopic images of (a) Ag-free as-cast alloy A , (b) 0.3 mass% Ag-containing alloy B, (c) 0.6 mass% Ag-containing alloy C and (d) 0.9 mass% Ag-containing alloy D (arrow : remains of eutectic CuAl2). 58
Fig. 3.4 DSC profiles of as-quenched (after solid solution treatment) alloys A, B, C and D. (The precipitation peak around 213℃ indicated the precipitation of Ω phase, I: precipitation of GP (I), II: precipitation of GP (II), III: dissolution of GP (I) and (II), IV: precipitation of θ´, V: precipitation of θ, and VI: dissolution of θ´and θ). 63
Fig. 3.5 DSC profiles of as-quenched (after solid solution treatment) alloys A, B, C and D. ( I: precipitation of Ω phase; II: precipitation of S' and θ' phases.) 65
Fig. 3.6 Decomposition of the DSC profile of alloy A into four normal distribution functions. 66
Fig. 3.7 Decomposition of the DSC profile of alloy C into six normal distribution functions. 67
Fig. 3.8 The numerically fitted DSC profiles and the values of heat of the precipitation for as-quenched alloys A, B, C and D; (a) precipitation of the Ω phase, and (b) precipitation of the θ' phase. 68
Fig. 3.9 DSC profiles of as-quenched alloy C aging at 185℃ for various periods, indicating that aging slows the precipitation of the Ω and θ' phases. 71
Fig. 3.10 Schematic diffraction patterns for zone axis = , all the expected diffraction spots resulting from regular diffraction are indicated for Al matrix and for the different orientations of possible precipitations such as Ω and θ' phase. 73
Fig. 3.11 The TEM micrograph of (a) diffraction pattern and (b) bright field image for alloy C quenched at 210 ℃ revealing tiny Ω phase; zone axis =〈011〉α. 73
Fig. 3.12 Diffraction patterns showing the various intensity of spots and streaks from the Ω and θ' phases of (a) alloy A, (b) alloy B, (c) alloy C and (d) alloy D under the T7 condition; zone axis =〈011〉α. 75
Fig. 3.13 TEM bright field images showing the Ω and θ' phases (arrows) of (a) alloy A, (b) alloy B, (c) alloy C and (d) alloy D tempered to T7 condition; zone axis = 〈011〉α. 76
Fig. 3.14 TEM bright field images and corresponding diffraction patterns from T6 alloy C: (a) diffraction patterns, (c) bright field image, and from RRA alloy C: (b) diffraction patterns, (d) bright field image; zone axis = 〈011〉α. 78
Fig. 3.15 Hardness versus time for prolonged aging at 185℃of various silver containing alloy A, B, C and D. 83
Fig. 3.16 Scanning Electron Microscopy secondary electron image of the fracture surface of tensile specimens for (a) Alloy A, (b) Alloy B, (c) Alloy C and (d) Alloy D tempered to T6 condition. 86
Fig. 3.17 Scanning Electron Microscopy secondary electron image of the fracture surface of tensile specimens for (a) Alloy A, (b) Alloy B, (c) Alloy C and (d) Alloy D tempered to T7 condition. 87
Fig. 3.18 Scanning Electron Microscopy secondary electron image of the fracture surface of tensile specimens for (a) Alloy A, (b) Alloy B, (c) Alloy C and (d) Alloy D tempered to RRA condition. 88
Fig. 3.19 TEM bright field grain boundary images of (a) Alloy A, (b) Alloy B, (c) Alloy C and (d) Alloy D tempered to T7 condition, showing a PFZ width of around 100 nm and grain boundary precipitations. 91
Fig. 3.20 TEM bright field grain boundary images of (a) T6 and (b) RRA alloy C, showing a PFZ width of approximately 50 nm, and the grain boundary precipitations. 92
Fig. 3.21 Optical micrographs of as-cast alloy (a) A (Cu/Mg = 29), (b) B (Cu/Mg = 19), (c) C (Cu/Mg = 8) and (d) D (Cu/Mg = 4); (arrow 1: eutectic CuAl2, 2: S phase). 97
Fig. 3.22 Optical micrographs of homogenization alloy (a) A (Cu/Mg = 29), (b) B (Cu/Mg = 19), (c) C (Cu/Mg = 8) and (d) D (Cu/Mg = 4); (arrow: remains of eutectic CuAl2). 98
Fig. 3.23 Optical micrographs of hot-extrusion alloy (a) A (Cu/Mg = 29), (b) B (Cu/Mg = 19), (c) C (Cu/Mg = 8) and (d) D (Cu/Mg = 4); (arrow: remains of eutectic CuAl2). 99
Fig. 3.24 Optical micrographs of solid solution treated alloy (a) A (Cu/Mg = 29), (b) B (Cu/Mg = 19), (c) C (Cu/Mg = 8) and (d) D (Cu/Mg = 4). 100
Fig. 3.25 DSC profiles of Al-4.6%Cu-Mg-Ag alloy at as-quenched and T7 condition. 105
Fig. 3.26 DSC profiles of alloy E (0.16wt.%Mg,Cu/Mg = 29) further exposed in air several times up to 1000hr each at (a) 107℃, (b) 135℃ and (c) 155℃ after T7 heat treatment. 107
Fig. 3.27 DSC profiles of alloy F (0.25wt.%Mg,Cu/Mg = 19) further exposed in air several times up to 1000hr each at (a) 107℃, (b) 135℃ and (c) 155℃ after T7 heat treatment. 108
Fig. 3.28 DSC profiles of alloy G (0.56wt.%Mg,Cu/Mg = 8) further exposed in air several times up to 1000hr each at (a) 107℃, (b) 135℃ and (c) 155℃ after T7 heat treatment. 109
Fig.3.29 Diffraction patterns and bright field image for alloy E, zone axis =〈011〉α, (a) T7, and exposed in air several times up to 1000hr each at (b)107℃, (c)135℃ and (d)155℃ after T7 tempering. 113
Fig.3.30 Diffraction patterns and bright field image for alloy F, zone axis =〈011〉α, (a) T7, and exposed in air several times up to 1000hr each at (b)107℃, (c)135℃ and (d)155℃ after T7 tempering. 114
Fig.3.31 Diffraction patterns and bright field image for alloy G, zone axis =〈011〉α , (a) T7, and exposed in air several times up to 1000hr each at (b)107℃, (c)135℃ and (d)155℃ after T7 tempering. 115
Fig. 3.32 SEM SE images of fracture surface of T7-tempering hot-extrusion (a) alloy E (0.56wt.%Mg,Cu/Mg = 8), (b) alloy F (0.56wt.%Mg,Cu/Mg = 8) and (c) alloy G. (0.56wt.%Mg,Cu/Mg = 8). 119
Fig.3.33 Hardness versus exposure time response of alloy E, F and G exposed in air several times up to 1000hr each at 107℃ (△line), 135℃ (○line) and 155℃ (□line) after T7 tempering. The first points at beginning of the curve were the hardness of alloys tempered to T7 condition. 122
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指導教授 李勝隆(Sheng-Long Lee) 審核日期 2005-7-19
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