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研究生：	甘帕格 GHANTASALA PRANAV BHARGAV
論文名稱：	以CALPHAD方法建構包含η'介穩相之 Al-Zn-Mg-Cu四元熱力學資料庫 CALPHAD Thermodynamic Modeling for Al-Zn-Mg-Cu Quaternary System with η' Metastable Phase Description
指導教授：	林士剛 Lin, Shih-Kang
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2022
畢業學年度：	110
語文別：	英文
論文頁數：	123
中文關鍵詞：	Al-Zn-Mg-Cu 四元系統、η' 介穩態析出物、SAXS 、DSC 、TEM
外文關鍵詞：	Al-Zn-Mg-Cu quaternary system, η' metastable phase, SAXS, DSC, TEM
相關次數：	點閱：63 下載：1
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鋁合金為汽車和航空產業之重要開發材料，為減少車體重量以增加汽車里程，汽車行業正在積極開發新興鋁合金材料。鋁合金部件的完整製造鏈包含精煉、鑄造、均質化、軋製/擠壓以及熱處理。而化學或熱力學驅動力、界面能、機械驅動力等是每個加工步驟的重要驅動力。因此鋁合金材料之研究與開發於化學和熱力學之理解至關重要。

鋁合金熱化學特性和相圖之研究有助於開發新的鋁合金成分和優化工藝。而CALPHAD計算熱力學方法是研究合金熱力學的最有效方法之一，透過建立完善的鋁合金熱力學資料庫有助於釐清複雜合金系統的相平衡和熱力學性質。

因此本研究聚焦於AA7075 鋁合金，通過結合實驗和熱力學計算方法來建立包含η' 介穩態析出物之 Al-Zn-Mg-Cu 四元熱力學資料庫，本研究彙整了文獻可得之Al-Cu、Al-Mg、Al-Zn、Cu-Mg、Cu-Zn、Mg-Zn、Al-Cu-Mg、Al-Zn-Mg、Al-Zn-Cu和Cu-Mg-Zn二元和三元系統。並採用不同的實驗技術分析Al-Zn-Mg三元系統中強度最高的η' 介穩態析出物，如透過TEM尋找析出物與鋁基底成分以及析出物尺寸，通過DSC差示掃描量熱法分析析出物體積分率，通過SAXS分析析出物尺寸和體積分率。並整合上述實驗結果獲得在 120℃ 等溫截面，生成了包含η'介穩態析出物之 Al-Zn-Mg-Cu 四元熱力學資料庫。

此包含介穩態析出物之 Al-Zn-Mg-Cu 四元熱力學資料庫可用於分析 AA7075鋁合金在凝固和平衡條件下的相平衡、析出物類型及其析出物體積分率。

關鍵字: Al-Zn-Mg-Cu 四元系統, η'介穩態析出物, SAXS, DSC,TEM

Aluminum alloys are prominently used in vehicle production and aviation. The automobile industry is experiencing a renaissance of aluminum research due to the necessity to increase gas mileage and mass diminution. The complete manufacturing chain of Al alloy components begins with refining, casting, homogenization, rolling/extrusion, and lastly heat treatment. Chemical or thermodynamic driving forces, interfacial energy, mechanical driving forces, and so on are the driving forces for each processing step. Thermodynamics relating to chemical processes and phase transitions is thus crucial.

The study of Al alloy thermochemical characteristics and phase diagrams are useful for developing new Al alloy compositions and optimizing processes. One of the most efficient approaches to study alloy thermodynamics is to use the CALPHAD (CALculation of PHAse Diagram) method. The phase equilibria and thermodynamic properties of complicated alloy systems can be determined using a well-developed Al alloy thermodynamic database.

The current work focuses on the construction of a thermodynamic database for the Al-Zn-Mg-Cu Quaternary system and thermodynamic modeling of η' metastable phase via a combined experimental and thermodynamic modeling method as a foundation for understanding numerous processes in Al 7075 alloys. The thermodynamic descriptions of the Al-Cu, Al-Mg, Al-Zn, Cu-Mg, Cu-Zn, Mg-Zn, Al-Cu-Mg, Al-Zn-Mg, Al-Zn-Cu, and Cu-Mg-Zn stable phase binary and ternary systems were upgraded. Different experimental techniques are used to find the most strengthening η' metastable phase in Al-Zn-Mg ternary system, such as Transmission Electron Microscopy to find precipitate, matrix composition, and precipitate size, Differential Scanning Calorimetry to find volume fraction, and small-angle X-ray Scattering to find the precipitate size and volume fraction. At an isothermal section of 120C, the thermodynamic description of the η' metastable phase description was generated. Furthermore, the binary, ternary, and metastable phase descriptions were combined with the Al-Zn-Mg-Cu Quaternary system.

The generated thermodynamic database with η' the metastable phase was used to analyze phase equilibrium, types of precipitations, and their amounts under both solidification and equilibrium circumstances for the Al7075 series alloys.

Keywords: Al-Zn-Mg-Cu quaternary system, η' metastable phase, SAXS, DSC, TEM.

CONTENTS 

摘要	ii
ABSTRACT	iii
ACKNOWLEDGMENT	iv
CONTENTS	v
LIST OF TABLES	viii
LIST OF FIGURES	ix
CHAPTER 1 INTRODUCTION	12
1.1 Preface	12
1.2 CALPHAD Modeling	13
1.3 Methodology	17
CHAPTER 2 LITERATURE REVIEW	18
2.1  Thermodynamic assessment of AL-Zn-Mg-Cu stable phases quaternary system	18
2.1.1 Aluminum – Copper  Binary System	18
2.1.2 Aluminum-Magnesium  Binary System	20
2.1.3 Aluminum – Zinc Binary System	22
2.1.4 Copper – Zinc Binary System	24
2.1.5 Copper – Magnesium  Binary System	26
2.1.6 Magnesium – Zinc Binary System	28
2.1.7 Aluminium – Copper – Magnesium Ternary System	30
2.1.8 Aluminium – Magnesium – Zinc Ternary system	32
2.1.9 Aluminium – Copper – Zinc Ternary system	34
2.1.10 Copper – Magnesium – Zinc Ternary system	36
2.1.11 Al – Zn – Mg – Cu Quaternary system	38
2.2 Description of 7xxx alloys	44
2.3 Metastable Phases	45
2.3.1 Compilation of composition data	48
2.3.2 Homogeneous precipitation	49
CHAPTER 3 EXPERIMENTAL PROCEDURE	50
3.1 Introduction	50
3.1.1 Composition	50
3.2 Alloy preparation	53
3.3 Experimental techniques	54
3.3.1 Optical Microscopy	54
3.3.2 Scanning Electron Microscopy	54
3.3.3 X-Ray Diffraction	55
3.3.4 Micro-Hardness	55
3.3.5 Differential Scanning Calorimetry (DSC)	56
3.3.6 Transmission Electron Microscopy (TEM)	57
3.3.7 Small-Angle X-ray Scattering (SAXS)	58
CHAPTER 4 RESULTS AND DISCUSSION	66
4.1 Introduction	66
4.2 Microstructure characterization	66
4.2.1 As-Cast Condition	66
4.2.2 Heat Treatment	66
4.3 X-Ray Diffraction analysis	70
4.4 Microhardness	72
4.5 TEM Analysis	74
4.6 DSC Investigation	77
4.7 Quantitative characterization by SAXS measurements	80
4.7.1 Interpretation of SAXS measurements	80
4.7.2 Guinier Radius	80
4.7.3 Integrated intensity	81
4.7.4 SAXS measurements are used to estimate volume fraction.	82
4.7.5 MgZn2 assumption	83
4.7.6 Al8Zn6Mg4 assumption	83
4.8 Optimization of Eta prime Metastable phase.	86
4.9 Summary	89
4.10 Future Work	92
REFERENCES	93
APPENDIX A The input files used in PANDAT	101
A.1 Al – Zn – Mg – Cu Quaternary System	101


LIST OF TABLES 
Table 2.1 Al-Cu-Mg-Zn phase nomenclature	41
Table 2.2 Reported  composition, Experiment Condition, and Phase fraction.	48
Table 3.1 The chemical composition of the alloys studied (in percentages).	50
Table 4.1 Estimation of the area under the dissolution peak yielded a quantification of η' - particles.	79
Table 4.2 Guinier radius (Rg) obtained for  T6 initial states.	80
Table 4.3 shows how to calculate the total integrated intensity by combining the three variables.	81
Table 4.4 summarizes the calculated integrated intensity Q0, which was generated by adding the three terms determined in Table.	82
Table 4.5 The volume fraction must be determined using atomic scattering factors and atomic volumes.	83
Table 4.6 provides the volume fraction results for Alloy Al84 based on the assumptions.	84
Table 4.7 Summary of the SAXS Results	85
Table.8 Summary of the experimental Results	91


LIST OF FIGURES 
Figure 1.1 CALPHAD Method Symbolic Representation [7].	14
Figure 1.2 Methodology flow chart.	17
Figure 2.1 The Al-Cu binary system's experimental phase diagram by Song-Mao Liang.[14]	19
Figure 2.2 The Al-Mg binary system's experimental phase diagram by H.-L Lukas [22]	21
Figure 2.3 The Al-Zn binary system's experimental phase diagram by S.A Mey [25].	23
Figure 2.4 The Cu-Zn binary system's experimental phase diagram by Song-Mao Liang [31].	25
Figure 2.5 The Cu-Mg binary system's experimental phase diagram by Coughanowr et al [36]	27
Figure 2.6 The Mg-Zn binary system's experimental phase diagram by Agarwal et al [40].	29
Figure 2.7 The Al-Cu-Mg ternary system's experimental phase diagram at 400℃  by T. Buhler [49].	31
Figure 2.8 The Al-Mg-Zn ternary system's experimental phase diagram at 400℃  by P. Liang[41].	33
Figure 2.9 The Al-Cu-Zn ternary system's experimental phase diagram at 400℃  by song-Mao Liang [58].	35
Figure 2.10 The Cu-Mg-Zn ternary system's experimental phase diagram at 400℃  by P. Linag [62].	37
Figure 2.11 The Al-Zn-Mg-Cu quaternary system experimental phase diagram at 120℃ .	43
Figure 2.12 The ternary Al-Zn-Mg phase diagram a. Portion at 200°C (M= η =MgZn2; T=Al2Mg3Zn3) at the Al-rich sector. [65]	44
Figure 2.13 Analysis of the η'-structure [66]	47
Figure 3.1 At 120°C and 490°C, the ternary Al-Mg-Zn phase diagram in the Al-rich corner.	51
Figure 3.2  The Experiment Process Flow chart	52
Figure 3.3 The heat treatment for T6 tempering is depicted schematically in this diagram.	52
Figure 3.4 Boron Nitrite (BN) sprayed silica tube.	53
Figure 3.5 shows the SAXS spectra acquired by the CCD camera.	62
Figure 3.6 The integrated intensity Q0 and the Guinier radius Rg are used to interpret SAXS data. On a T6 material, an example of a SAXS spectrum.	64
Figure 4.1 (a) Typical OM micrographs of the as-cast Al-Zn-Mg alloy (showing dendritic microstructure), (b) SEM micrographs of the as-cast Al-Zn-Mg alloy (showing dendritic morphology).	67
Figure 4.2 SEM micrographs of the as-cast Al-Zn-Mg alloy and EDS spectrum.	67
Figure 4.3 At 400°C, the Al-Mg – Zn phase diagram shows the alloy compositions at various stages.	68
Figure 4.4 Typical SEM micrograph and EDS spectrum of the Solution treatment of Al-Mg-Zn alloy at 490℃  for 3h.	68
Figure 4.5 Heat-Treated Al-Zn-Mg alloy SEM-BSE micrographs after 24 hours at 120°C.	69
Figure 4.6 Al-Zn-Mg X-ray diffraction curves under As-Cast conditions.	70
Figure 4.7 Al-Zn-Mg X-ray diffraction curves after 3 hours of solution treatment at 490°C.	70
Figure 4.8 The age-hardness curves of the alloys during isothermal aging at 120℃ 	72
Figure 4.9 (a) EBSD mapping of Alloy Al84 (b) EBSD micrograph of alloy Al84 representing the {111}Al plane (c) TEM micrograph of alloy Al84 representing the eta prime metastable phase.	74
Figure 4.10 (a) TEM micrograph indicating the Eta prime precipitates (b) TEM micrograph indicating the Al Matrix.	75
Figure 4.11 From the raw image to the image analysis to find the precipitate size. (a) Maximum Precipitate size (b) Minimum precipitate Size.	76
Figure 4.12 DSC scans of GP Zone, η'  and η phases.	77
Figure 4.13 DSC thermograph of Alloy Al84 representing the eta prime Dissolution peak.	78
Figure 4.14 SAXS Results obtained from T6 Temper, Different Plots used in the interpretation are presented.	80
Figure 4.15 For big q-values, the Iq4 vs q 4 plot can be used to derive the constant K-values.	81
Figure 4.16 The K constant is determined in the Iq4 against q 4 plot. Laue denotes the slope of the Porod's behavior, and K denotes the origins ordinates. In this example of T6's beginning condition, Porod's law is demonstrated.	81
Figure 4.17 phase fraction of assumed conditions and fitting conditions.	85
Figure 4.18 Experimental phase diagram of the Al-Zn-Mg ternary system at 120℃  with Eta prime metastable phase.	86
Figure 4.19 At 120℃  the experimental phase diagram of the Al-Zn-Mg-Cu quaternary system with the eta prime metastable phase.	88
                                    

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