輥軋變形對7075-T73鋁合金的微結構影響與陽極行為和皮膜性質的探討

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周俊宏(CHUN-HUNG CHOU) 查詢紙本館藏

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機械工程學系

論文名稱

輥軋變形對7075-T73鋁合金的微結構影響與陽極行為和皮膜性質的探討
(The effect of rolling deformation on the microstructure evolution and Anodic Aluminum Oxide behavior formed on 7075-T73 aluminum Alloy)

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摘要(中)

本實驗主要研究7075鋁合金退火、變形(低溫輥軋, CR & 常溫輥軋, RR)及人工時效處理(T73)對微結構的影響。使用維克氏硬度試驗(Hv)，光學顯微鏡（OM），穿透式電子顯微鏡（TEM）對7075-T73的微結構與析出型態進行分析。7075鋁合金使用15oC/hr的退火速率能夠獲得均勻的微結構組織與小的硬度變異值；T73處理後CRST73試片基地上擁有最高的硬度值、最低的硬度變異值與最少的顆粒數量分佈與均勻的析出強化相(η-MgZn2)分佈。
7075鋁合金表面處理陽極使用15 wt% 硫酸，硬化陽極使用22 wt% 硫酸、1.85 wt% 草酸、0.1 wt% 硫酸鋁的混合酸。V-t曲線是用來計算陽極與硬化陽極所消耗的能量。使用掃描式電子顯微鏡(SEM)觀察陽極氧化膜(AAO films)上的孔洞行態，X射線光電子能譜儀(XPS)分析陽極氧化膜表面的成分分佈。經過變形的試片(CRST73&RRST73)在陽極與硬化陽極處理時比ST73消耗的能量要少。在XPS的分析結果中可以從O/Al比去確定氧化膜的成分組成，在一般陽極處理(MA)後表面氧化膜的成分偏向Al(OH)3，硬化陽極處理(HA)後表面氧化膜成分偏向AlOOH，而陽極與硬化陽極氧化膜與基材界面處的成分偏向Al-O-H。使用電化學的方式來分析計算氧化鋁膜的耐腐蝕性，腐蝕試驗後得到CRST73比RRST73與ST73擁有更好的耐腐蝕性。
CIE L* a* b*色差和光學常數（吸收值（k）、折射率（n）、反射率（R））被應用於氧化鋁薄膜的光學性質進行分析。結果我們發現氧化膜厚度增加L值會降低，表面粗糙度增加折射率（n）和反射率（R）會降低，吸收值(k)會增加。

摘要(英)

In this study, the 7075 aluminum alloy were subjected to annealing, deformation (Cryo-rolling, CR & Room temperature Rolling, RR) following artificial aging treatment (T73). The microstructure and precipitation morphology of 7075-T73 aluminum alloy which subjected to varied deformed process were analyzed by Vicker’s hardness (Hv), optical microscope (OM), transmission electro microscope (TEM). The 7075 aluminum alloy with 15oC/hr annealing rate that obtained an uniform microstructure and smaller hardness variation; after T73 treatment, the CRST73 sample owns a highest micro hardness lowest hardness variation and lowest particles distribution in the matrix and uniform precipitation of strengthening phase (η-MgZn2) distribution.
The surface treatment of 7075 aluminum alloy was subject to 15 wt% H2SO4 for anodic treatment (MA) and mixed with 22 wt% H2SO4, and 1.85 wt% H2C2O4, and 0.1 wt% (AlH4)2SO4 for hard anodic treatment (HA). The V-t curve was used to record the anodic and hard anodic treatments and calculated energy consumption during anodic treatment.. The scanning electrical microscope (SEM) was applied to observation the pore population of anodic alumina oxide (AAO) film, and X-ray photoelectron spectrum (XPS) analysis was used to obtain the surface composition of AAO films. The deformed samples (CRST73 and RRST73) were following anodic and hard anodic treatment that obtained lower energy consumption than the without deformed samples (ST73). In the XPS analysis results, according to O/Al ratio, we can determine the surface composition of the AAO film. The Al(OH)3 phase are favored form after MA treatment, the and AlOOH phase form after HA treatment. The other hand, the AlOOH phase and Al-O-H phase were found at matrix/oxide interface. The electrochemical analyses were applied to measure the corrosion resistance of AAO film. After corrosion test, the CRST73 sample owns a better corrosion resistance than the RRST73 and ST73.
The CIE L * a * b * color difference and optical constant (absorption values (k), the refractive index (n), reflectance (R)) were applied to analyze the optical properties of AAO films. As the results, we found the increasing thickness of the oxide film with reduced the L values of AAO films, and increases surface roughness with decreasing refractive index (n) and reflectance (R) but increasing the adsorption value.

關鍵字(中)

★ 陽極
★ 過時效處理
★ 退火
★ 7075
★ 硬化陽極

關鍵字(英)

★ hard anodic
★ anodic
★ 7075
★ annealing
★ over aging treatment

論文目次

目錄
中文摘要 i
Abstract ii
目錄 iv
圖目錄 vi
第二章 vi
表目錄 x
第二章 x
第一章前言 1
第二章理論探討與文獻回顧 2
2-2 鋁合金熱處理 2
2-3 7000系列鋁合金微結構 3
2-3-1 高強度7000系列鋁合金析出強化機制[2~7] 3
2-3-2 7000系列合金兩階段時效探討 10
2-3-3 銅、氫元素對7xxx鋁合金影響 12
2-3-4 7000系列輥軋介紹 15
2-3-5 比較T6及T73時效 18
2-3-6 7000系列鋁合金析出物(TEM&SEM)外形分析 21
2-4 鋁合金陽極與硬化陽極處理 23
2-4-1 陽極膜種類與成長機制 24
2-4-2 陽極氧化膜生成的電壓-時間曲線(V-t curve) 26
2-4-3 硬化陽極與電流、電壓的關係 30
2-4-4 7000系鋁合金對硬化陽極影響 33
2-5 光學檢測 35
2-6 腐蝕 37
2-6-1 腐蝕的定義[46] 37
2-6-2 腐蝕型態 37
2-6-3 氯離子腐蝕理論 38
第三章實驗方法與步驟 40
3-1 實驗材料及試片準備 40
3-2 實驗步驟 40
第四章結果與討論 46
4-1 熱處理與輥軋變形的微結構分析 46
4-1-1 鋁合金熱處理條件選用 46
4-1-2 變形差異對微結構影響分析 50
4-2 陽極與硬化陽極氧化膜性質分析 61
4-2-1 陽極與硬化陽極成長階段能量消耗分析 61
4-2-2 陽極與硬化陽極氧化膜孔洞型態 65
4-3 陽極與硬化陽極XPS成份分析 72
4-4 陽極與硬化陽極腐蝕阻抗能力分析 76
4-5 陽極與硬化陽極處理氧化膜色澤變化與光學性質 81
4-5-1 國際照明規範CIE L*a*b*成色標準 81
4-5-2 光學性質 82
第五章結論 92
參考文獻 94
附錄一 102
附錄二 104
圖目錄
第二章
Fig. 2-1 7075鋁合金固溶處理及固溶處理後自然時效10天後的量熱曲線[6]。 4
Fig. 2-2 Al-Zn-Mg-Cu alloy 時效16小時120℃ HRTEM圖[2]。 5
Fig.2-3 7075鋁合金施以低溫輥軋後低溫時效HRTEM圖[3]。 5
Fig. 2-4 Al-Zn-Mg-Cu 四元460℃等溫相圖[7]。 6
Fig. 2-5 Al-Zn 二元相圖[8]。 7
Fig. 2-6 Al-Mg 二元相圖[8]。 7
Fig. 2-7 Al-Cu 二元相圖[8]。 8
Fig. 2-8 Al-Mg-Zn 三元相圖[8]。 9
Fig. 2-9 材料在不同參數下二階段時效的應力應變曲線[9]。 11
Fig. 2-10 AA7xxx-T6 鋁合金隨著Cu含量增加硬度也跟著增加[10]。 12
Fig. 2-11 TEM下的微結構 (A)7004, (B)7039, (C)7029, (D)7075, (E)7050鋁合金[10]。 13
Fig. 2-12 7075-T6鋁合金以極化電位-725mVSCE在除氣的0.5M的NaCl中預先通電的電流曲線，時間(a)0h,(b)6h,(c)12h,(d)24h[11]。 14
Fig. 2-13 7075-T6鋁合金以極化電位-725mVSCE在除氣的0.5M的NaCl中預先通電後的材料表面狀態，時間(a)0h,(b)6h,(c)12h,(d)24h[11]。 14
Fig. 2-14 7075合金在低溫輥軋及常溫輥軋不同應變下的取向分布差異柱狀圖(a)固溶材料(b)低溫輥軋下真應變2.3(c)常溫輥軋下真應變2.3(d)低溫輥軋下真應3.4(e)常溫輥軋下真應變3.4[12]。 16
Fig. 2-15 XRD分析7075合金CR、RTR及ST受時效處理前後[13]。 17
Fig. 2-16 TEM比較7075合金晶粒內微結構(a)T6, (b)T73[14]。 19
Fig. 2-17 7075鋁合金T6及T7量熱曲線[6]。 20
Fig. 2-18 TEM下7075鋁合金微結構(a)T6,(b)T7[6]。 20
Fig. 2-19 繞射環下7075鋁合金T6處理析出物的分佈量[6]。 21
Fig. 2-20 多孔陽極氧化鋁膜示意圖[33]。 23
Fig. 2-21 鋁合金氧化膜形成示意圖(a)初始電場分佈(b)穿透路徑形成(c)局部電場集中[34]。 25
Fig. 2-22 鋁合金氧化膜孔洞形成之穩定成長[35]。 25
Fig. 2-23 鋁合金陽極氧化膜隨陽極時間(0~49s)增加而變厚[37]。 26
Fig. 2-24 陽極過程電壓-時間關係圖[41]。 27
Fig. 2-25 不同陽極時間下的陽極膜SEM表面型態 (a)0, (b)2, (c)4, (d)5, (e)6, (f)10, (g)12, (h)20 sec[41]。 28
Fig. 2-26 TEM下觀察不同陽極時間的陽極膜表面型態 (a)3, (b)12, (c)20 sec[42]。 29
Fig. 2-27 陽極時間與膜上孔洞的關係(a)孔的大小與樹料的關係 (b)陽極時間對孔的大小關係[40]。 29
Fig. 2-28 硬化陽極在Type I (1 oC、1.8 M H2SO4溶液、電流密度j=120 mA cm-2)，把鋁基材腐蝕剩下膜的部分，使用離子減薄(ion milling)把膜的底部除去露出陽極孔洞，分別在 (a) 27 V, (b) 32 V, (c) 40 V 三種電壓[44]。 31
Fig. 2-29 硬化陽極在Type I(1 oC、1.8 M H2SO4溶液、電流密度j=120 mA cm-2)，硬化陽極膜側面孔壁生長狀態，分別在 (a) 27 V, (b) 32 V, (c) 40 V 三種電壓[44]。 32
Fig. 2-30 7075鋁合金硬化陽極處理電壓與時間關係圖[27]。 33
Fig. 2-31 7075鋁合金硬化陽極膜斷面SEM圖(a) alloy 1, (b) alloy 2[27]。 34
Fig. 2-32 L*a*b色彩圖。 35
Fig. 2- 33 金屬在氯化鈉溶液裡的腐蝕行為[47]。 39
第三章
Fig. 3-1 實驗流程。 44
第四章
Fig. 4-1 OM 50X下觀察AA7075-O不同退火速率對微結構影響。 48
Fig. 4-2 SEM觀察AA7075-O用15oC/hr退火速率所得材料表面的析出顆粒外型。 48
Fig. 4-3 OM下觀察AA7075鋁合金在熱處理前的金相結構 (a)倍率50X (b)倍率100X。 54
Fig. 4-4 OM下觀察AA7075鋁合金在 ST73的金相結構 (a)倍率50X (b)倍率100X。 54
Fig. 4-5 OM下觀察AA7075鋁合金在 CRST73的金相結構 (a)倍率50X (b)倍率100X。 55
Fig. 4-6 OM下觀察AA7075鋁合金在 RRST73的金相結構 (a)倍率50X (b)倍率100X。 55
Fig. 4-7 SEM與EDS觀察AA7075-ST73顆粒外型與成分。 56
Fig. 4-8 TEM下AA7075鋁合金ST73微結構。 57
Fig. 4-9 TEM下AA7075鋁合金CRST73微結構。 58
Fig. 4-10 TEM下AA7075鋁合金RRST73微結構。 59
Fig. 4-11 TEM下AA7075鋁合金CRST73晶界上的連續析出物及EDS成份分析。 60
Fig. 4-12 TEM下AA7075鋁合金CRST73基地上的棒狀析出物及EDS成份分析。 60
Fig. 4-13 相同電流密度下一般陽極與硬化陽極的電壓-時間曲線及微分曲線圖，分別： (a)A ST73； (b)A CRST73； (c)A RRST73； (d)HA ST73； (e)HA CRST73； (f)HA RRST73。 63
Fig. 4-14 SEM下觀察A-ST73陽極表面狀態 (a)6 s, (b)30 s, (c)300 s, (d)17.5 min。 66
Fig. 4-15 SEM下觀察A-CRST73陽極表面狀態 (a)6 s, (b)30 s, (c)300 s, (d)17.5 min。 67
Fig. 4-16 SEM下觀察A-RRST73陽極表面狀態 (a)6 s, (b)30 s, (c)300 s, (d)17.5 min。 68
Fig. 4-17 SEM下觀察HA-ST73硬化陽極表面狀態 (a)15min, (b)75 min, (c)135 min。 69
Fig. 4-18 SEM下觀察HA-CRST73硬化陽極表面狀態 (a)15min, (b)75 min, (c)135 min。 70
Fig. 4-19 SEM下觀察HA-RRST73硬化陽極表面狀態 (a)15min, (b)75 min, (c)135 min。 71
Fig. 4-20 陽極處理封孔前後比較極化曲線。 79
Fig. 4-21 硬化陽極處理封孔前後比較極化曲線。 80
Fig. 4-22 陽極與硬化陽極封孔前後L值與氧化膜厚度關係。 86
Fig. 4-23 不同製程試片在陽極處理後約10 µm厚度的光學性質 (a)k， (b)n， (c)R。 87
Fig. 4-24 不同製程試片在硬化陽極處理後約10 µm厚度的光學性質 (a)k， (b)n， (c)R。 88
Fig. 4-25 不同製程試片在硬化陽極處理後約100 µm厚度的光學性質 (a)k， (b)n， (c)R。 89
Fig. 4-26 陽極處理氧化膜厚度約10µm的光學性質與膜厚、粗糙度關係， (a) O/Al對能量、 (b) 光學性質對膜厚、 (c) 光學性質對粗糙度。 90
Fig. 4-27 硬化陽極處理氧化膜厚度約10µm的光學性質與膜厚、粗糙度關係， (a)O/Al對能量、 (b)光學性質對膜厚、 (c)光學性質對粗糙度。 91
表目錄
第二章
Table 2-1 7000 系鋁合金析出特性 10
Table 2-2 二階段時效熱處條件及實驗數據 11
Table 2-3 7075合金在不同條件下的拉伸數據 17
Table 2-4 7075合金T6及T73機械性質與晶間腐蝕敏感性比較 18
Table 2-5 分析7000系列鋁合金晶粒內顆粒及析出物的長寬比。 21
Table 2-6 分析7000系列鋁合金晶粒內顆粒及析出物的周長面積比。 21
Table 2-7 分析7000系列鋁合金晶粒內顆粒及析出物的種類、大小、外型。 22
第三章
Table 3-1 本實驗所使用材料合金成分。 40
Table 3-2 XPS在O 1s、Al 2p、Si 2p、Mg 2p、Zn 2p3、Cu 2p3分析各種成分的鍵結能[50]。 45
第四章
Table 4-1 AA7075-O不同退火速率的硬度及變異值。 48
Table 4-2 EDS觀察AA7075-O用15oC/hr退火速率所得材料表面的析出顆粒成分。 49
Table 4-3 AA7075鋁合金熱處理後硬度及變異值。 51
Table 4-4 AA7075鋁合金不同熱處理後的晶粒平均尺寸。 51
Table 4-5 AA7075在倍率100X下觀察的顆粒數量及尺寸分佈。 51
Table 4-6 AA7075鋁合金不同製程試片在一般陽極與硬化陽極各階段時間與能量消耗量測表。 64
Table 4-7 AA7075鋁合金不同製程試片的導電率 (IACS%)。 65
Table 4-8 SEM觀察AA7075在陽極與硬化陽極下孔洞狀態。 65
Table 4-9 約10µm膜厚下陽極表面與界面XPS分析(At%)。 75
Table 4-10 約10µm膜厚下硬化陽極表面與界面XPS分析(At%)。 75
Table 4-11 陽極與硬化陽極封孔前後極化曲線Ecorr與Epit電壓比較。 78
Table 4-12 不同製程試片在陽極處理後的膜厚及色澤變化表。 84
Table 4-13 不同製程試片在硬化陽極處理後的膜厚及色澤變化表。 84
Table 4-14 不同製程試片在陽極與硬化陽極處理後的表面粗糙度(Ra)。 85
Table 4-15 不同製程試片在陽極與硬化陽極處理後在可見光的波長範圍(400~700nm)內的光學性質：吸收值(k)、折射率(n)、反射率(R)。 85

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指導教授

施登士(Teng-Shih Shih)

審核日期

2012-7-27

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