Tehinse Olayinka

RESPONSE OF 7075 AND 7050 ALUMINIUM ALLOYS TO HIGH
TEMPERATURE PRE-PRECIPITATION HEAT TREATMENT
By
OLAYINKA BLESSING TEHINSE
A Thesis submitted to the Faculty of Graduate Studies of
The University of Manitoba
in partial fulfilment of the requirements of the degree of
MASTER OF SCIENCE
Department of Mechanical Engineering
University of Manitoba
Winnipeg
Copyright © 2014 by Olayinka Blessing Tehinse

ABSTRACT
Al-Zn-Mg-Cu (7xxx series) aluminium alloys are widely used for aircraft structures.
It is difficult to obtain a combination of optimal strength and stress corrosion cracking
(SCC) resistance for these alloys. It appears that SCC resistance of these alloys is
related to grain boundary precipitate morphology. One technique to control the grain
boundary precipitate morphology is to introduce a controlled cooling procedure
referred to as High Temperature Pre-precipitation (HTPP) treatment following the
solution heat treatment. There is need for a detailed study of the effect of HTPP on the
properties of commercial Al-Zn-Mg-Cu alloys using different intermediate
temperatures. In this thesis research, the results of ten HTPP processes applied to
7075 and 7050 commercial 7xxx series alloys are presented in terms of hardness,
electrical conductivity, corrosion resistance, TEM analysis of grain boundary
precipitate morphology and EDS analysis of solute concentration profile at the grain
boundary. Results indicate that subsequent to HTPP processing, the 7050 alloy can be
precipitation aged to a higher hardness compared to 7075; this result is associated
with the modification of 7050 alloy by zirconium versus chromium in 7075 alloy.
HTPP heat treatment achieves better SCC resistance compared to standard T6 temper.
However, it does not appear that HTPP can achieve a combination of hardness,
electrical conductivity and corrosion resistance superior to standard T6 and T7X
tempers.
ii
ACKNOWLEDGEMENT
I really appreciate my advisor, Dr. Jonathan Beddoes for the opportunity to work on
this research. I am grateful to him for the teaching, guidance, mentorship, personal
interest and support which has enabled me to have a great graduate study experience.
I also appreciate the support and guidance of my thesis committee, Dr. Bassuoni and
Dr. Caley.
The financial supports of Natural Science and Engineering Research Council of
Canada, Faculty of Graduate studies and Faculty of Engineering, University of
Manitoba on this research are highly appreciated. I am grateful to Mike Boswick,
Trevor Smith and Dan Rossong for their technical support. I really appreciate Dr.
Khan for the training and support on the TEM analysis used in this work.
I acknowledge the inspiring effort of my parents Mr. and Mrs. Tehinse, Mr. and Mrs.
Adetunji and the rest of my family. Their moral support, prayers and encouragement
are highly appreciated. I am thankful to my friends/colleagues: Dr. Oshoba, Dr. Ola,
Dr. Oluwasegun, Dr. Krutika, Emmanuel Ocran, Johnson Aina, Omhudhowo Oshobe,
Ebenezer Essel, Afua Adobea Ampadu-mintah, Ioannis Polyzois and others for their
help and guidance. I am thankful to my roommates Bolanle Akinwumi and Victoria
Owuobe for their love and companionship. My absolute gratitude goes to Jehovah
God for His unconditional love, mercy and grace.
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TABLE OF CONTENTS
ABSTRACT ..................................................................................................................ii
ACKNOWLEDGEMENT ..........................................................................................iii
LIST OF TABLES .....................................................................................................vii
LIST OF FIGURES ..................................................................................................viii
LIST OF COPYRIGHTED MATERIAL FOR WHICH PERMISSION WAS
OBTAINED ................................................................................................................xii
CHAPTER ONE: INTRODUCTION ........................................................................ 1
1.1 Historical development of Al-Zn-Mg-Cu alloys for airframe structures ........ 1
1.2 Motivation and Objectives of this Thesis Research ...................................... 10
CHAPTER TWO: Al-Zn-Mg-Cu ALLOYS............................................................ 12
2.1 Alloying elements ......................................................................................... 12
2.2 7xxx versus 2xxx series aluminium alloys for aircraft structures ................. 14
2.3 Precipitation hardening in 7xxx alloys .......................................................... 16
2.4 Introduction to physical metallurgy of 7xxx alloys ...................................... 19
2.5 Mechanism of precipitation hardening in 7xxx alloys .................................. 21
2.6 Important microstructural features ................................................................ 22
2.6.1 Quench sensitivity.................................................................................. 25
2.6.2 Electrical conductivity ........................................................................... 28
CHAPTER THREE: LOCALISED CORROSION IN Al-Zn-Mg-Cu
ALLOYS ..................................................................................................................... 30
3.1 Intergranular Corrosion ................................................................................. 30
iv
3.2 Exfoliation Corrosion .................................................................................... 31
3.3 Stress Corrosion Cracking............................................................................. 32
3.3.1 Mechanism of Stress Corrosion Cracking ............................................. 33
3.4 Effect of slip character on SCC in Al-Zn-Mg-Cu alloys .............................. 35
3.5 Influence of grain boundary precipitate structure on SCC ............................ 37
3.6 Influence of magnesium and copper content................................................. 38
3.7 Crack initiation versus propagation and damage tolerance design
requirement ................................................................................................... 39
CHAPTER FOUR: EFFECT OF HEAT TREATMENT ON SCC RESISTANCE
OF Al-Zn-Mg-Cu ALLOYS ...................................................................................... 42
4.1 Overaging ...................................................................................................... 42
4.2 Retrogression and reaging ............................................................................. 43
4.3 High Temperature Pre-precipitation heat treatment ...................................... 46
4.4 Effect of heat treatment on grain boundary segregation…………………… 50
CHAPTER FIVE: EXPERIMENTAL PROCEDURE .......................................... 52
5.1 Experimental materials .................................................................................. 52
5.2 Heat treatment procedure .............................................................................. 52
5.3 Electrical conductivity testing ....................................................................... 57
5.4 Hardness testing ............................................................................................ 58
5.5 Corrosion tests ............................................................................................... 59
5.5.1 Exfoliation corrosion testing .................................................................. 59
5.5.2 Stress corrosion test (Double beam test) ................................................ 61
v
5.6 Microstructural Analysis ............................................................................... 64
CHAPTER SIX: EXPERIMENTAL RESULTS .................................................... 67
6.1 Electrical conductivity results ....................................................................... 67
6.2 Hardness results............................................................................................ 70
6.3 Corrosion test results .................................................................................... 75
6.3.1 Exfoliation corrosion result.................................................................... 75
6.3.2 Stress Corrosion Cracking results .......................................................... 83
6.4 Results of microstructural analysis ............................................................... 98
6.5 Microstructural analysis of unaged samples using TEM ............................ 100
6.6 Microstructural analysis of aged samples using TEM ................................ 103
6.7 Energy Dispersive X-ray Spectrometry (EDS) analysis…………………... 106
CHAPTER SEVEN: DISCUSSION OF RESULTS ............................................. 110
7.1 Effect of heat treatment on EC of 7075 and 7050 alloys ............................ 110
7.2 Effect of heat treatment on hardness of 7050 and 7075 alloys ................... 111
7.3 Exfoliation Corrosion (EXCO) versus EC of 7075 and 7050 alloy ............ 114
7.4 Effect of HTPP on Stress corrosion cracking of 7075 and 7050 alloy ....... 115
7.5 Grain boundary precipitate versus SCC resistance ..................................... 118
7.6 Effect of HTPP on microstructure ............................................................... 119
CHAPTER EIGHT: CONCLUSIONS .................................................................. 122
8.1 Recommendations for future work .............................................................. 123
REFERENCES ......................................................................................................... 124
vi
LIST OF TABLES
Tables Page
1.1 Composition (wt.%) of some aluminium alloys used in aircraft ...................... 6
1.2 Typical mechanical properties of aluminium alloys ......................................... 7
5.1. Nominal and actual composition of 7075 and 7050 alloys…………………..53
5.2. Analysis of heat treatment procedure .............................................................. 54
5.3. Exfoliation corrosion rating ............................................................................. 60
6.1. Electrical conductivity results of 7075 alloy before and after aging ............... 68
6.2. Electrical conductivity results of 7050 alloy before and after aging ............... 69
6.3. Hardness result of 7075 alloy before aging ..................................................... 71
6.4. Hardness result of 7075 alloy after aging ........................................................ 72
6.5. Hardness result of 7050 alloy before aging ..................................................... 72
6.6. Hardness result of 7050 alloy after aging ........................................................ 73
6.7. Exfoliation corrosion (EXCO) rating of heat treated samples ......................... 76
6.8. Summary of results obtained from 7075 alloy double beam samples ............. 84
6.9. Summary of results obtained from 7050 alloy double beam samples ............. 84
vii
LIST OF FIGURES
Figures Page
1.1. Typical applications of aluminium alloys and tempers in aircraft
structures ............................................................................................................ 2
1.2. Materials used for upper wing skin from 1919-1994......................................... 4
1.3. Variation of SCC resistance and strength due to aging .................................... 8
1.4. Changes in hardness during RRA heat treatment ............................................. 9
2.1. Fracture toughness versus yield strength relationship for 2xxx and 7xxx
series alloys ..................................................................................................... 15
2.2. Phase diagram of a typical precipitation hardenable alloy ............................. 17
2.3. Heat treatment process for precipitation hardening in 7xxx alloys ................. 17
2.4. The Al-MgZn2 equilibrium diagram for Al-Zn-Mg alloys .............................. 21
2.5. Effect of particle size and CRSS on dislocation-precipitate interaction .......... 23
2.6. Distribution of precipitates within the matrix in T6 and T7 temper ............... 24
2.7. Continuous and discontinuous distribution of precipitates along grain
boundary in T6 and T7 temper......................................................................... 26
2.8. Dispersoid particles of Al12Mg2Cr in alloy 7075 ............................................ 26
2.9. Effect of quenching cooling rate on strength of aluminium alloys .................. 27
3.1. Exfoliation corrosion causing delamination .................................................... 31
3.2. Stress corrosion cracking in a 7075-T6 wing lock........................................... 33
3.3. TEM micrograph showing planar dislocation slip .......................................... 36
3.4. TEM micrograph showing dislocations in wavy slip ...................................... 36
3.5. Stages of SCC showing KIC and KISCC ............................................................ 40
4.1. Schematic showing retrogression and reaging heat treatment procedure ........ 43
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4.2. Effect of heat treatment on SCC resistance in 7075 alloy heat treated to T6,
T73 and RRA .................................................................................................. 44
4.3. Discontinuous grain boundary precipitates in 7075 alloy RRA ...................... 46
4.4. High temperature pre-precipitation heat treatment procedure ......................... 47
4.5. Micrographs of (a) fine and (b) coarse precipitates in the grains of
HTPP temper .................................................................................................... 49
4.6. Discontinuous precipitates at the grain boundary region of HTPP temper ..... 50
4.7. Concentration profile of Zn, Mg and Cu across the grain boundary
of (a) T651 (b) T73 (c) RRA tempers of 7150 alloy ....................................... 51
5.1. Box furnace used for HTPP treatment ............................................................. 55
5.2. Fisher Scientific silicon oil bath used for aging treatment .............................. 55
5.3. Heat treatment procedure for HTPP ................................................................ 56
5.4. EE0021 digital electrical conductivity tester ................................................... 57
5.5. Versitron Rockwell hardness tester ................................................................. 58
5.6. Polished plate prepared for exfoliation corrosion test .................................... 60
5.7. A loaded double beam sample ......................................................................... 63
5.8. Travelling microscope ..................................................................................... 63
5.9. Stress intensity vs crack length as shown in equation 1 .................................. 64
5.10. Stages of preparation of TEM sample….…………………………………... 66
6.1. Effect of heat treatment on electrical conductivity of 7075 and 7050 alloy .... 70
6.2. Effect of HTPP heat treatment on hardness of 7075 alloy............................... 74
6.3. Effect of HTPP heat treatment on hardness of 7050 alloy............................... 74
6.4. EXCO behaviour of 7075 alloy ...................................................................... 77
6.5. EXCO behaviour of 7050 alloy ...................................................................... 80
ix
6.6. Optical micrograph of a section of an exfoliated sample showing
intergranular corrosion ..................................................................................... 83
6.7. Comparism of crack length with time in two SCC samples for each of
HTPP condition TF/Q = 455 and 370 oC ............................................................ 85
6.8. Average crack length with time of 7075 double beam samples ...................... 87
6.9. Average crack length with time of 7050 double beam samples ...................... 88
6.10. Crack growth velocity vs stress intensity of 7075 samples ............................ 88
6.11. Crack growth velocity vs stress intensity of 7050 samples ............................ 92
6.12. Summary of V-K plot for 7075 alloy............................................................... 96
6.13. Summary of V-K plot for 7050 alloy............................................................... 96
6.14. Comparism of SCC behaviour in 7050 and 7075 alloy at TF/Q = 370 oC ........ 97
6.15. Double beam samples after SCC testing. ......................................................... 98
6.16. Optical images of as-received (a) 7075-T651 and (b) 7050-T74 alloy ........... 99
6.17. Effect of compositional modification on the microstructure of 7075 and
7050 alloy......................................................................................................... 99
6.18. TEM analyses of unaged 7075 alloy in (a) and (b) T6 (c) TF/Q= 405 oC (d)
TF/Q= 370 oC. .................................................................................................. 101
6.19. TEM analyses of unaged 7050 alloy in (a) and (b) T6 (c) TF/Q = 405 oC (d)
TF/Q = 370 oC .................................................................................................. 102
6.20. TEM analysis of grain boundary precipitate morphology of 7075 alloy. ...... 104
6.21. TEM analysis of grain boundary precipitate morphology of 7050 alloy ....... 105
6.22. EDS analysis across grain boundary of 7075 samples................................... 107
6.23. EDS analysis across grain boundary of 7050 samples................................... 108
6.24. EDS analysis showing the extent of scatter in results ................................... 109
x
7.1. Effect of heat treatment on electrical conductivity of 7050 and
7075 alloy....................................................................................................... 111
7.2. Effect of heat treatment on hardness of 7050 and 7075 alloys ...................... 113
7.3. Nucleation of precipitate phases during controlled cooling .......................... 113
7.4. Effect of heat treatment on EC and EXCO resistance ................................... 114
7.5. Relationship between EC and SCC resistance (using crack length measured
after 257 hours of SCC test) of 7075 and 7050 alloy .................................... 116
7.6. Summary of effect of heat treatment on electrical conductivity and crack
growth velocity at 3MPa√m stress intensity for 7075 alloy .......................... 117
7.7. Summary of effect of heat treatment on electrical conductivity and crack
growth velocity at 3MPa√m stress intensity for 7050 alloy .......................... 117
7.8. Summary of grain boundary copper solute concentration in (a) 7075 and
(b) 7050 alloy ................................................................................................. 121
xi
LIST OF COPYRIGHTED MATERIAL FOR WHICH PERMISSION WAS
OBTAINED
Figure 1.1: Source-“Advanced Materials and Processes” Reprinted with permission
from ASM International (27-02-2014).
Figure 1.2: Source-“Materials Forum” Reprinted with permission from Materials
Australia (13-02-2014).
Figure 1.3: Source-“Metallurgical Transactions A” Reprinted with permission from
Spinger (24-03-2014).
Figure 1.4: Source-“Journal of Materials Science” Reprinted with permission from
Spinger (24-03-2014).
Figure 2.1: Source-“Lightweight Materials-Understanding the basics” Reprinted with
permission from ASM International (06-03-2014).
Figure 2.2: Source-“Key to metals” Reprinted with permission from European Space
Agency (22-04-2014).
Figure 2.4: Source-“Canadian Metallurgical Quarterly” Reprinted with permission
from Maney publishing (24-03-2014).
Figure 2.5: Source-“Handbook of Aluminium” Reprinted with permission from
Taylor and Francis Group, LLC, a division of Informa PLC (18-04-2014).
Figure 2.6: Source-“Transactions of Non-ferrous Metals Society of China” Reprinted
with permission from Elsevier (06-03-2014).
xii
Figure 3.1: Source-“NDT Resource Centre” Reproduced with permission from the
NDT Resource Center/Center for Non-destructive Evaluation, Iowa State University
(05-03-2014).
Figure 3.3: Source-“Fatigue at elevated temperatures” Reprinted with permission
from ASTM International (12-03-2014).
Figure 3.4: Source-“Fatigue at elevated temperatures” Reprinted with permission
from ASTM International (12-03-2014).
Figure 3.5: Source-“Metallurgical Transactions A” Reprinted with permission from
Spinger (24-03-2014).
Figure 4.3: Source-“Journal of Materials Science” Reprinted with permission from
Spinger (24-03-2014).
Figure 4.8: Source-“Proceedings of Environment Induced Cracking of Metals” Reprinted
with permission from NACE (25-03-2014).
Figure 6.15: Source-“Materials Science and Engineering B” Reprinted with permission
from Elsevier (18-04-2014).
xiii
CHAPTER ONE
INTRODUCTION
7xxx series aluminium alloys are high strength, heat treatable alloys containing zinc
and magnesium as the main alloying elements. Similar to all heat treatable aluminium
alloys, 7xxx series alloys rely on precipitation hardening to improve properties [1].
This series of alloys can be divided into Al-Zn-Mg and Al-Zn-Mg-Cu alloys [2]. Al-
Zn-Mg alloys are relatively weldable and are referred to as medium strength alloys
[3]. Al-Zn-Mg-Cu alloys have the highest strength compared to other aluminium
alloys. 7xxx series alloys are often used for high strength applications, predominantly
in compressively loaded airframe structures, as shown in Figure 1.1 [4]. Examples are
upper wing panels, frames, stringers, longerons, extruded parts, etc. Other applications
include mobile equipment and other highly stressed components. Properties of
particular interest for structural applications of 7xxx series alloys are toughness,
fatigue crack growth rate, strength, exfoliation and stress corrosion resistance [3, 5].
1.1 Historical development of Al-Zn-Mg-Cu alloys for airframe structures
Airframe structures are high strength applications. For instance, upper wing structures
are loaded in compression during flight. Hence, materials selection for these parts
requires a high compression strength to weight ratio. Other important properties
considered for materials selection are cost, corrosion resistance and toughness [6].
Application of aluminium alloys in aircraft can be traced back to the engine crankcase
in Wright brothers’ plane in 1903 [7]. A study of the Wright Flyers internal
combustion engine crank case showed a composition of Al-8% copper, about 1.0%
iron and 0.4% silicon impurities.
1
Figure 1.1: Typical applications of aluminium alloys and tempers in aircraft
structures, such as the Boeing 777 illustrated [4]
The strength of the alloy, low weight requirements of the aircraft and good casting
qualities are likely reasons for selection of this material [8].
The discovery of age hardening of Al-Cu alloys by Alfred Wilm in 1906 led to
research on the mechanism of precipitation hardening [9]. Guinier and Preston’s work
provided evidence that explains the precipitation mechanism in aged Al-Cu alloy [9].
Further studies revealed that GP (Guinier-Preston) zones are formed during nucleation
of strengthening precipitate phases from the solid solution. These studies started the
evolution of alloy development for airframe structures [7, 9].
2
Earliest application of aluminium alloys in aircraft wing structures used alloys based
on the Al-Cu-Mg system (2xxx series alloys), an example being the Junkers F-13 and
DC-3 aircraft. These alloys had the highest yield strength at that time in the range of
275-310 MPa. The need for increased aircraft performance motivated effort to find
other precipitation hardenable alloys [9]. Among the few other alloys that showed
precipitation hardening, Al-Zn-Mg alloys were discovered in 1923. Investigation
showed that Al-Zn-Mg alloys showed the best response to precipitation hardening
compared to other aluminium alloy compositions. Figure 1.2 shows various materials
used for upper wing skin of aircrafts from 1919-1994 [9]. This shows that continuous
increase in demand for materials with higher strength to weight ratios has enabled the
development of precipitation hardenable Al-Cu (2xxx series) and Al-Zn-Mg-Cu (7xxx
series) alloys over the years [5]. The broken line in Figure 1.2 shows the transition in
aircraft application in early 1940’s from 2xxx to 7xxx alloys based on higher strength.
In the 1920’s and 30’s, studies were carried out to understand tensile strength and
corrosion resistant properties of Al-Zn-Mg alloys. Part of this was the development of
alloy X74S (5.2% Zn, 2.1% Mg, 1.5% Cu, 0.4% Mn) with a low Zn:Mg ratio in 1938.
7076-T6 alloy (7.5% Zn, 1.6% Mg, 0.7% Cu and 0.6% Mn) with a high Zn:Mg ratio
was developed in 1940 for application as a high strength forging alloy for propeller
blades. However, deformed sheet of this alloy was susceptible to stress corrosion
cracking. Studies showed that addition of 0.2-0.35% Cr increased the corrosion
resistance of X74S [10].
In 1943, 7075-T6 was developed based on the previous alloy compositions by
adjusting the composition of Zn, Mg and Cu for improved strength and the addition of
Cr. First application of 7075-T6 sheet was as skin and stringers in B-29 Fortress
3
Al-Cu Al-Zn-Mg-Cu
Figure 1.2: Materials used for upper wing skin from 1919-1994 [9]
bomber during World War II. Higher strength 7xxx alloy were developed for
passenger and military aircraft after the war [10].
In the 1950’s, forgings were used for several aircraft structures. The susceptibility of
7075-T6 to corrosion and high quench sensitivity led to development of another alloy
more suitable for forgings. Hy43 with low copper content (about 0.6% Cu) was
developed as a forging alloy and designed to have good heat treatment properties.
Hy43 was better in terms of ductility in short-transverse section, quench sensitivity
and strength. After successful accelerated stress corrosion time to failure testing was
carried out, Hy43 was commercialized as alloy 7179 and used for a wide range of old
and new designs. However, in the late 1950’s, it was discovered that alloy 7179
exhibited high susceptibility to stress corrosion that was not predicted by the
accelerated corrosion tests. This is due to the slow crack initiation in 7179, but higher
crack growth rate compared to 7075 alloy [10]. The severe corrosion problems of
7179 alloy led to its withdrawal from aerospace applications [11]. Nevertheless,
4
airworthiness issues related to the high stress corrosion cracking susceptibility of
7179/7079 alloy continue today [12]. Tables 1.1 and 1.2 show chemical composition
and properties of some of the alloys mentioned.
In the 1960’s, the problem of stress corrosion cracking and requirement for thicker
sections of 7075-T6 for forgings in aircraft designs led to development of 7075-T73
temper. 7075-T73 forgings were developed for improved corrosion resistance using a
two-step aging heat treatment procedure. After aging to T6 temper at about 120 oC for
24 hours, T7 temper was obtained by overaging above 150 oC for 7-9 hours to
increase resistance to stress corrosion cracking [1].
Although, this comes with about 10-15% loss of strength compared to 7075 and 7179-
T6, 7075-T73 was accepted by aircraft designers [10]. One of the first application of
7075-T73 was in DC10. T76 temper was later applied in Lockheed L1011 [7, 11].
The increasing demand for lighter weight, higher strength structures especially for
commercial aircraft led to the development of 7178-T651 alloy with higher Zn, Mg
and Cu content compared to 7075. However, the increasing demand for higher
fracture toughness and damage tolerance limited the use of this alloy [10]. Over the
years, applications of T73 alloys have no record of stress corrosion cracking [10].
In the T6 and T73 tempers, there is an inverse relationship between strength and SCC
resistance as shown in Figure 1.3 [13]. This shows that as aging time and temperature
increases, the strength decreases while resistance to SCC increases. In Figure 1.3,
stage I shows the initial aging step. Stage II can be related to T6 temper and it shows
that higher strength can be obtained but the resistance to SCC is low. Stage III shows
that prolonged aging can increase SCC resistance but there is loss of strength.
5
Table 1.1: Composition (wt.%) of some aluminium alloys used in aircrafts [14, 15]
Alloy Zn Cu Mg Mn Cr Zr Fe Si
2014 - 4.4 0.5 0.80 0.10 - 0.70 0.80

2024 - 4.4 1.5 0.60 0.10 - 0.50 0.50
7075 5.6 1.6 2.5 - 0.30 - 0.50 0.40
7178 6.8 2.0 2.7 - 0.30 - 0.50 0.40
7050 6.3 2.4 2.3 0.10 0.04 0.12 0.15 0.12
7079 4.3 0.6 3.3 0.20 0.20 - 0.50 0.30
7150 5.9-6.9 1.9-2.5 2.0-2.7 0.10 0.04 0.08-0.15 0.15 0.12
7055 7.6-8.4 2.0-2.6 1.8-2.3 0.05 0.04 0.08-0.25 0.15 0.10
7A52 4.4 0.13 0.13 0.24 0.13 0.12 0.25 0.20
6
Table 1.2: Typical mechanical properties of aluminium alloys [13, 15, 16, 17, 18, 19,
20, 21, 22]
Yield Fracture
Year of strength toughness SCC
Alloy introduction Temper (MPa) (MPa√m) resistance
2024 1931 T351 269-276 Excellent Good

T851 386-400 Excellent High
T6 345 Good
2017 1920’s T4 276
7075 1943 T6 503 Moderate
T73 434 Excellent
7076 1940
7175 T6 503
T73 476
7178 1951 T6 537
T76 503
7179 T6
7050 T74 510
T76 455
7150 T7751 565 29.7
7055 T7751 614 28.6
T651 544
T7451 496
7079 1954 T6 469
7
Figure 1.3: Variation of SCC resistance and strength due to aging [13]
The loss of strength in 7075-T73 temper led to compositional modification to obtain
7050 alloy with about 2.22% copper and use of Zr in place of Cr for improved
strength and less quench sensitivity. Chromium containing dispersoids in 7075 alloy
control grain structure and prevent recrystallization during processing but causes
quench sensitivity, i.e. properties are dependent on the quenching rate. Hence, the
strength of 7075 alloy decreases as the quenching rate decreases. The Zr addition in
7050 alloy reduces the quench sensitivity. Thus, 7050 alloy is more useful for thick
structural sections [23].
In the 1970’s, Cina developed the Retrogression and Reaging (RRA) heat treatment to
address the trade-off between strength and stress corrosion resistance in the T6 and
T73 tempers. The RRA heat treatment is applied to 7075-T6 and involves
‘retrogression’ (partial re-solutionizing) of the T6 temper at a higher temperature for a
8
very short period of time (for example 200 oC for 2 minutes, 240 oC for 7 seconds).
During retrogression, dissolution of strengthening precipitate phase and dislocations
occur, causing loss of strength as shown in Figure 1.4 [24]. This is followed by
reaging using T6 aging conditions (121 oC for 24 hours) to achieve a better
combination of strength and SCC resistance [14, 25]. Figure 1.4 shows the effect of
retrogression time on hardness after retrogression and subsequent reaging heat
treatment. It was observed that the strength reaches the lowest minimum after a short
retrogression time. Increase in retrogression time causes increase in hardness but
further increase in retrogression time causes the hardness to decrease. Subsequent
reaging treatment increases the hardness. However, higher strength after reaging is
obtained at the lowest minimum on the retrogression curve corresponding to few
seconds of retrogression.
Figure 1.4: Changes in hardness during RRA heat treatment [24]. Arrows indicate
change in hardness after reaging
9
A T77 temper designation is used when RRA is applied to 7055 alloy. 7055-T77 is
used for several structural components on the Boeing 777, as shown in Figure 1.1.
However, the short retrogression time required to obtain high strength in RRA
treatment makes it difficult or impossible to apply RRA to thick section components
[24].
1.2 Motivation and Objectives of this Thesis Research
The difficulty of applying RRA to thick sections of components during manufacturing
creates the need to develop a heat treatment procedure that avoids the relatively high
temperature retrogression process.
This research aims to study the effect of high temperature pre-precipitation (HTPP)
heat treatment on strength and SCC resistance of 7xxx series alloys. HTPP is a
recently developed heat treatment procedure which involves slow cooling from
solution heat treatment temperatures to a lower, intermediate temperature before
quenching, followed by applying T6 aging. The aim of this procedure is to modify the
grain boundary microstructure to form coarse, discontinuously distributed precipitates
and achieve higher resistance to stress corrosion cracking [26]. Similar slow cooling
heat treatment procedures in other materials such as nickel superalloys or titanium
aluminide intermetallics showed that this procedure can modify the grain boundary
microstructure and improve targeted material properties [27]. Previous work on the
effect of HTPP on experimental Al-Zn-Mg-Cu alloys shows that HTPP treatment can
improve SCC resistance in experimental alloys [26, 28, 29]. However, the influence
of HTPP heat treatments applied to commercial 7xxx alloys is not well understood. It
is also important to understand the effect of the intermediate temperature used during
the HTPP process on the properties of Al-Zn-Mg-Cu alloys. Accordingly, the goal of
10
this thesis research is to study the effect of HTPP heat treatments on the electrical
conductivity, quench sensitivity, hardness, corrosion resistance and microstructure of
commercial 7075 and 7050 alloys.
11
CHAPTER TWO
Al-Zn-Mg-Cu ALLOYS
2.1 Alloying elements
Pure aluminium is well known for its low density and high corrosion resistance.
However, pure aluminum cannot be used for structural applications due to low
strength. Alloy development involves the addition of different alloying elements to
improve material properties. Alloying aluminium to high strength enables design
applications where high strength to weight ratio is important [2]. Although the
primary effect of alloying is increase in strength, other material properties are affected
by alloying. Aluminium alloys usually contain 90-96% aluminium and about two
major alloying elements to obtain a combination of properties. Major alloying
elements usually have significant solubility in aluminium. Zinc, magnesium,
manganese, copper and silicon are used as major alloying elements. Although, minor
elements may have low solubility in aluminium, addition of minor elements improves
fabrication and performance [30, 31].
Aluminium is a reactive metal but it relies on an ability to form a protective oxide
layer for good corrosion resistance. Generally, corrosion resistance decreases as the
alloying element content increases. Alloying elements may form solid solutions or
phases that sometimes affect the continuity of the protective oxide layer or
electrochemical potential of phases versus matrix [32]. Specific alloying elements in
7xxx series aluminium alloy are as follows:
12
 Zinc and Magnesium
The addition of zinc increases the solution potential of the alloy. However, binary
aluminium-zinc alloys are seldom used due to high susceptibility to SCC and hot
cracking in the wrought and cast alloys respectively. Magnesium and zinc are often
added together to increase strength by increasing the heat treatment response of the
alloy due to formation of MgZn2 precipitate phase. However, there is need for control
of composition, microstructure and processing (heat treatment) to obtain resistance to
SCC [2, 33].
 Copper
The addition of up to 1% copper in the presence of zinc and magnesium increases the
strength by solid solution strengthening. Increase in copper content to about 1.5%
increases resistance to SCC. However, high amount of copper increases quench
sensitivity and reduces weldability [2].
 Chromium/Manganese /Zirconium
Chromium, manganese and zirconium are used as additions in 7xxx alloys to control
grain structure and prevent recrystallization. Chromium can form finely dispersed
phases in these alloys due to its slow rate of diffusion [2]. However, the use of
chromium is challenged by increase in quench sensitivity. Zr is being used in newly
developed alloys to reduce quench sensitivity. This will be a subject of discussion
later in this chapter.
 Iron and silicon
Iron and silicon are the commonest impurities found in aluminium alloys. Iron has a
high solubility in aluminium in the molten state, but the solubility reduces in solid
state. This enables iron to form intermetallic compounds with aluminium and other
elements [2]. Silicon reduces the melting point, increases the strength and fluidity of
13
aluminium [1]. Both iron and silicon significantly affect properties of aluminium
alloy. Hence, strict limits on the quantity of impurity elements are important to
achieve required material properties. 7050 alloy contains lesser amount of iron and
silicon compared to 7075. This compositional modification reduces the amount of
constituent particles formed in 7050 alloy thereby improving the fracture toughness.
Constituent particles are intermetallic compounds containing Fe and Si formed during
solidification. More information on the types and effect of constituent particles will be
discussed later in this chapter. The effect of this compositional modification on the
microstructure of 7050 and 7075 alloys will be studied later in this thesis.
2.2 7xxx versus 2xxx series aluminium alloys for aircraft structures
Both 2xxx and 7xxx series are heat treatable alloys widely applied as airframe
structures. 2xxx series (Al-Cu) alloys have been widely applied since the discovery of
age hardening by Alfred Wilm which led to development of Duralumin (Al-3.5%Cu-
0.5%Mg-0.5%Mn) [7, 9]. Modifications in chemical composition led to development
of 2014 alloy with higher silicon content for higher strength and 2024 alloy with
higher magnesium and lower silicon content for better response to aging at room
temperature. Typical tensile strength of 2014 alloy is 485 MPa. 7xxx alloys have
higher strength in the range of 470-600 MPa [31]. This explains the replacement of
2xxx with 7xxx alloys for upper wing structures shown in Figure 1.2.
A critical property required for upper wings is high compressive strength. This is
necessary since the upper wing is under compression loading during flight [6]. 7xxx
alloys have higher compressive strength compared to 2xxx alloys. However, Figure
1.1 shows that 2xxx series alloys are still applied as structural materials in aircrafts
14
especially for high fracture toughness applications. An example is the lower wing
which is under tension loading during flight.
An important property that differentiates 2xxx and 7xxx alloys is fracture toughness.
Recently, reduction in the level of iron, silicon and copper has achieved an increase in
fracture toughness of 2xxx alloys. Also, high damage tolerance and high resistance to
fatigue crack propagation enables 2xxx alloys to be applied as aircraft fuselage skin
and lower wing skins on commercial aircrafts. Figure 2.1 shows the fracture
toughness-strength requirement of both alloys [34]. At lower strength compared to
7xxx series alloys, higher fracture toughness can be obtained in 2xxx series alloys
[34].
Figure 2.1: Fracture toughness versus yield strength relationship for 2xxx and 7xxx
series alloys [34]
15
2.3 Precipitation hardening in 7xxx alloys
Precipitation hardening is the process of developing fine, second phase particles
called precipitates in an alloy such that higher strength is achieved. Figure 2.2 shows
the phase diagram of precipitation hardenable alloys [35]. For precipitation hardening
to occur, it is important that the solid solubility limit of the solute in the alloy system
is decreasing as temperature decreases as shown by the broken line in Figure 2.2.
2xxx, 6xxx and 7xxx series alloys (with Cu, Mg-Si and Zn-Mg as main alloying
element respectively) are precipitation hardenable and are also known as heat
treatable alloys [33]. To achieve precipitation hardening in 7xxx alloys, the following
heat treatment steps (shown in Figure 2.2) must be carried out.
 Solution heat treatment
 Quenching
 Aging
Solution heat treatment (SHT) is the process of dissolving second phase particles in
an alloy to form a single phase. SHT involves heating to a temperature in the single
phase region as shown in Figure 2.2. Figure 2.3 summarizes the heat treatment
procedure for precipitation hardening in 7xxx alloys. The alloy is kept at the SHT
temperature (To) for some time to develop a single phase at equilibrium. Thermal
processes occurring during SHT also allows formation of vacancies in the single
phase. The choice of SHT temperature is determined by the alloy composition. High
SHT temperature is used to achieve high strength after aging. However, in alloys
containing eutectic phases, SHT temperature higher than eutectic temperature can
cause incipient melting of eutectic phases.
16
Solution
Figure 2.2: Phase diagram of a typical precipitation hardenable alloy showing heat
treatment processes for precipitation hardening. Broken line indicates decrease in
solubility of solute as temperature decreases [35]
Figure 2.3: Heat treatment process for precipitation hardening in 7xxx alloys
17
This will have a negative effect on the final mechanical properties of the alloy.
Depending on the alloy composition, potential improvement in the properties of
aluminium alloy can be obtained by appropriate design of SHT process. For instance,
non-isothermal SHT between the solvus temperature and the eutectic temperature
starting from low SHT temperature allows homogenization of the eutectic phase to
occur and subsequent increase in the temperature will maximize the solute
concentration [27].
Quenching is the process of rapidly cooling the alloy from the SHT (To to T1 as shown
in Figure 2.3) to form a supersaturated solid solution (SSS) of solute and highly
concentrated vacancies. SSS is important for the subsequent nucleation and growth of
precipitates during aging. Optimum strength is often associated with fast quenching
rate [33]. However, fast quenching rate may induce stress and cause distortion in
intricate parts. Slow quenching allows migration of solute and vacancies to grain
boundary regions which may cause a reduction in mechanical properties after aging.
Hence, the choice of quenching medium and temperature are important to determine
the quenching rate. Water is a common medium for quenching aluminium alloys. It is
important to avoid quench delays to achieve optimum strength properties [1].
Aging is the controlled decomposition of the SSS to form second phase particles
called precipitates. The supersaturated solid solution formed during quenching is
unstable and this provides a driving force for precipitation to occur through diffusion
[27, 33]. Aging can occur naturally at room temperature or artificially at temperature
below the equilibrium solvus (T2 in Figure 2.3). During aging, precipitates are formed
with an interface with the matrix which may be coherent (perfect match at the
interface between precipitate and the matrix), semi-coherent or incoherent. Fine
precipitates formed at the initial stage of precipitation hardening are coherent or semi-
18
coherent with the matrix. However, prolonged aging causes loss of coherency of the
precipitates with the matrix. This is called overaging and it is usually associated with
loss of strength.
2.4 Introduction to physical metallurgy of 7xxx alloys
7xxx series alloys have good solid solution range that allows formation of
supersaturated solid solution during quenching from SHT temperature [1]. 7xxx series
alloys are highly unstable after quenching from SHT such that natural aging occurs
even at room temperature. Artificial aging (aging above room temperature) is
commonly used in practical applications. During aging, precipitate phases are formed
due to precipitation reaction. In 7xxx alloys, the mechanism of homogeneous
precipitation can be summarized as follows:
Supersaturated Solid Solution (SSS) → Guinier-Preston (GP) zones → non-
equilibrium (metastable) phase (η′) → equilibrium precipitate (η) [26].
An increase in the concentration of vacancies in the supersaturated solid solution
enhances homogenous precipitation by formation of vacancy clusters and diffusion of
solute to vacancy clusters to form GP zones. As aging continues, diffusion of solutes
facilitates the growth of GP zones to intermediate precipitates. These are spherical,
metastable (η′) phases. Increase in internal strain induced by the intermediate
precipitates causes partial loss of coherency with the matrix. As aging continues,
equilibrium precipitates, η or T phase that are incoherent with the matrix are formed
[1].
The general precipitation mechanism of 7xxx alloys showing decomposition of GP
zones to intermediate (η′) phase and later equilibrium precipitate phase (η) is given
19
above. Precipitation sequence that follows such decomposition from GP zones to η is
common in alloys with high Zn:Mg ratio like 7075 and 7050 alloys. The composition
of intermediate precipitate (η′) is not so clear. Some studies claim that the
composition of intermediate precipitate is same as equilibrium precipitate, other
researchers have shown that the composition of intermediate precipitate is closer to
GP zone with Zn:Mg ratio 1:1 [1, 36, 37]. Equilibrium precipitate is hexagonal,
MgZn2 with Zn:Mg ratio 2:1. In alloys with low Zn:Mg ratio, the precipitation
mechanism involves formation of GP zones and decomposition to intermediate T′ and
later equilibrium T phase likely composed of cubic, Mg32(Al, Zn)49 [1, 37]. In 7075
and 7050 alloys, optimum strength is obtained from GP zones and intermediate
precipitates. However, continuous aging causes precipitates to grow to equilibrium
precipitates and this causes loss of strength.
Precipitation hardening also modifies the grain boundary precipitate structures. Since
7075 and 7050 alloys are susceptible to intergranular corrosion like SCC, heat
treatments are designed to develop precipitate structure that will prevent a continuous
path for corrosion at the grain boundary. As discussed earlier, a coarse, discontinuous
distribution of precipitates has been related to higher corrosion resistance of T7 and
T77 (RRA) tempers. The effect of HTPP on the grain boundary precipitate
morphology and corrosion resistance will be analyzed later in this study.
Figure 2.4 shows the simplified Al-MgZn2 equilibrium diagram for 7xxx series alloys
[27]. The composition of Zn and Mg content in 7075 alloy is represented by the
broken line. The presence of copper and impurities in commercial 7075 alloys
changes the composition of the equilibrium phase and this will alter the temperatures
given in Figure 2.4. For instance, the given solvus temperature is 420 oC for 7075, but
this might be in the range of 420-455 oC in commercial alloys [33].
20
Figure 2.4: The Al-MgZn2 equilibrium diagram for Al-Zn-Mg alloys. Zn and Mg
content in 7075 alloy corresponds to broken line [27]
2.5 Mechanism of precipitation hardening in 7xxx alloys
In 7xxx alloys, strength is increased due to the interaction between dislocation and
second phase particles formed during precipitation. Dislocation-precipitate interaction
is determined by size, spacing and degree of coherency between the precipitate and
the matrix. Depending on the alloy, strength is determined by the ability to resist
dislocation motion through the following [38, 39]:
Strain fields formed by coherent GP zones: The presence of misfit between the
precipitate and the matrix generates strain fields. This increases the internal stress and
higher stress will be required for dislocation motion thereby increasing strength.
21
Shearing of deformable precipitates: Interaction between small precipitates and
dislocations is often by shearing. This occurs due to deformability of small
precipitates that allows dislocations to cut through the precipitates. The stress required
to initiate dislocation motion is called critically resolved shear stress (CRSS). At the
initial stage of precipitate growth, the CRSS is low. This enables dislocations to shear
through precipitates. This form of interaction is also known as chemical hardening.
During chemical hardening, changes occur along the slip plane due to formation of an
additional interface. Strength is increased in that more work will be required by the
applied stress to achieve these changes.
Bypass of coarse, non-deformable precipitates: Dislocations bypass coarse particles
due to increase in the particle spacing and loss of coherency at the precipitate-matrix
interface. As the precipitates grow, resistance to shearing from dislocations increases.
Strengthening is obtained due to work hardening by the debris dislocation left after
looping of particles by dislocation. Figure 2.5 shows that particle size affects the
CRSS in deformable and non-deformable particles as precipitate particles grow [1].
As shown in the Figure, the critical particle size corresponds to high critically
resolved shear stress. At the critical particle size, high strength can be obtained due to
difficulty in achieving the high CRSS.
2.6 Important microstructural features
Some microstructural features affect properties of 7xxx series alloys. Dispersoids,
intermetallic compounds, constituent particles, grain boundary and matrix precipitates
among others are important features that affect fracture toughness, strength and
corrosion resistance of 7xxx alloys.
22
Figure 2.5: Effect of particle size and CRSS on dislocation-precipitate interaction [1]
 Matrix and grain boundary precipitate
The composition, structure and distribution of precipitates in the matrix and grain
boundary region affect the properties of 7xxx alloys. Among other microstructural
factors, matrix precipitates affect strength while the grain boundary precipitates affect
resistance to intergranular corrosion [29, 40]. During aging, coherent precipitates are
finely distributed in the matrix to achieve high strength by restricting movement of
dislocations. Continuous aging to the overaged condition increases precipitate size in
the matrix and grain boundary region, causing loss of strength and coherency. Figure
2.6 shows the fine and coarse precipitate morphology in T6 and T7 matrix
respectively. While high concentration of fine precipitates observed in T6 increases
the strength, coarsening of the precipitates in T7 temper causes loss of strength [29].
23
Figure 2.6: Distribution of precipitates within the matrix in (a) T6 and (b) T7 temper
respectively [29]
Figure 2.7 shows grain boundary precipitate morphology in T6 and T7 temper
respectively. A continuous distribution of small precipitates is observed in T6 while
T7 temper shows discontinuous distribution of coarse precipitates. The coarsening of
precipitates in the grain boundary during overaging improves the resistance to
intergranular corrosion by eliminating a continuous path for corrosion to occur [40].
Studies of other heat treatment procedure that have improved the resistance to SCC
like retrogression and reaging shows that coarse precipitates are discontinuously
distributed along the grain boundary (similar to T7 temper shown in Figure 2.7) [29].
 Constituent particles
Constituent particles are intermetallic compounds formed during solidification
through eutectic reactions. Constituent particles may contain Fe or Si with other
alloying elements and sometimes aluminium. Constituent particles containing Fe are
insoluble while those without Fe may be soluble or slightly soluble based on the
solute content in the solid solution [1]. Constituent particles larger than 1 µm in
24
diameter are undesirable in aluminium alloys. Due to incoherency with the matrix,
constituent particles are not effective strengthening particles. Constituent particles can
favour crack growth, reduce fatigue resistance and fracture toughness. In 7075 alloy,
Al7Cu2Fe, SiO2, Al12(Fe, Mn)3Si, Al23CuFe4, Al6(Fe, Mn), Mg2Si, are the common
constituent particles. The compositional modification through the use of lower
amounts of iron and silicon in 7050 alloy achieves decrease in the size and number of
constituent particles in 7050 alloy. Al7Cu2Fe, Mg2Si and Al2CuMg are common in
7050 alloy [1].
 Dispersoids
Dispersoids are small particles that are formed by aluminium and transition metal
alloying elements such as Zr, Cr and Mn during hot rolling. Due to small size and fine
distribution, dispersoids are useful in preventing recrystallization by pinning the
movement of grains. The ability of dispersoids to effectively prevent recrystallization
requires small size, small spacing and coherent or semi-coherent interface with the
matrix. However, dispersoids can nucleate microvoids and this is undesirable. In 7075
alloy, Al12Mg2Cr is a common dispersoid as shown in Figure 2.8 [1]. Al3Zr is
common in 7050 and other high strength aluminium alloys [1]. The type of
dispersoids formed in an alloy can affect the quench sensitivity.
2.6.1 Quench sensitivity
Quench sensitivity is a phenomenon in heat treatable alloys whereby the properties of
the alloy are dependent on the quench rate. An important factor that contributes to
quench sensitivity is formation of dispersoids. Figure 2.9 shows the effect of
quenching rate on strength of some aluminium alloys [1]. As the quenching rate is
decreased, there is decrease in strength of both alloys.
25
Figure 2.7: Continuous and discontinuous distribution of precipitates along grain
boundary in T6 and T7 temper respectively [29]
Figure 2.8: Dispersoid particles of Al12Mg2Cr (indicated by the arrows) in alloy 7075
[1]
26
However, 7075 alloy exhibits more loss of strength compared to 7050 alloy. 7075 and
7050 alloys show that the type of dispersoid affects quench sensitivity. As shown in
Figure 2.9, 7050 is less quench sensitive compared to 7075 alloy [1]. In 7075 alloy,
Cr is used to control grain size and prevent recrystallization. However, Cr forms
incoherent dispersoids that alloys heterogeneous nucleation of precipitates to occur
during quenching thereby causing reduction in strength called quench sensitivity. The
loss of strength is due to reduction in the concentration of solute atoms available for
the formation of strengthening phases through homogeneous precipitation. In 7050
alloys, the use of Zr allows formation of dispersoids at semi-coherent interface with
the matrix and this prevents heterogeneous precipitation at the interface.
600
Tensile strength (MPa)
550
500
7050
7075
450
400
1 10 100 1000
Average cooling rate (oC/s)
Figure 2.9: Effect of quenching cooling rate on strength of aluminium alloys [adapted
from 1]
27
2.6.2 Electrical conductivity
Electrical conductivity (EC) is used to easily assess the stress corrosion cracking
susceptibility of 7xxx series alloys. EC measurement provides an easy, fast method of
distinguishing between tempers likely to be prone to SCC and those likely to be
resistant. It is believed that there is a direct relationship between SCC resistance and
electrical conductivity. This means that as aging increases, EC increases and the SCC
resistance increases [41]. High electrical conductivity is obtained in high SCC
resistant T7 while low EC is obtained in T6 temper. The minimum acceptable level of
EC for T73 treated 7075 alloy is 38% IACS (International Annealed Copper
Standard) while T6 is 31-33% IACS [42]. Heat treatments are often designed to
obtain higher EC to increase resistance to SCC [43].
Electrical conductivity is a bulk property. The observed changes in EC of different
tempers can be due to the amount of impurity element and solutes in the solid
solution. A high amount of impurity elements in solution causes an increase in the
resistance to flow of electrical current thereby reducing the EC value. During
quenching, the high concentration of solutes in the supersaturated solid solution
increases resistivity and decreases EC. EC can also be related to hardness and
strength. Strength decreases due to loss of strengthening phases to the solid solution
after quenching from SHT. During aging, formation of precipitates increases strength
but decreases the amount of solutes in the matrix. Intermediate precipitates and GP
zones are associated with coherent strain and this induces scattering effect (deviation
from straight trajectory by one or more paths) on electrons thereby decreasing EC.
Continuous aging causes transformation of coherent precipitates to incoherent
28
precipitates (as in T7 temper) causing loss of strength. This transformation reduces
strain on the matrix to achieve increase in EC [41, 44, 45, 46].
Tsai et al. suggested that the correlation between EC and SCC resistance holds in the
near peak aging (T4) and overaged condition (T7) in a particular alloy [44]. For
instance, the EC of 7475-T6 is higher than 7075-T6 (as expected in view of the higher
impurity elements in 7075). However, results of SCC test showed that the average
time to failure of 7075-T6 is longer than 7475-T6. Also, EC of as-quenched 7475 is
less than 7475-T6 as expected, but the average time to failure to SCC is longer in as-
quenched state than the T6 [44]. This shows that even though the relationship between
EC and SCC resistance has been established for T6 and T7 temper, there is need to
understand the SCC response of EC values between these two extremes. The effect of
HTPP heat treatment on EC of 7075 and 7050 alloys as it relates to SCC resistance
will be discussed later in this thesis research.
29
CHAPTER THREE
LOCALISED CORROSION IN Al-Zn-Mg-Cu ALLOYS
Localized corrosion is a form of accelerated attack by a corrosive environment at
discrete locations on a component while the other parts of the component corrode at a
much slower rate. Localized corrosion may be due to breakdown of protective oxide
film or the effect of localized condition of the environment [47]. Among different
forms of localized corrosion, Al-Zn-Mg-Cu alloys are highly susceptible to
intergranular corrosion, exfoliation corrosion and stress corrosion cracking. Localised
corrosion affects mechanical properties and structural integrity of Al-Zn-Mg-Cu
alloys.
3.1 Intergranular Corrosion
Intergranular corrosion is a form of localized corrosion in which attack is localized to
grain boundaries and regions closely adjacent to grain boundaries while the grains
remain unattacked [48]. The selective attack on the grain boundary region is due to
segregation/depletion of impurity elements or precipitation of phases at the grain
boundary. Segregation or precipitation often causes localized decrease in corrosion
resistance in the alloy [48]. Intergranular corrosion penetrates into the material until
the self-limiting depth is reached. The limiting depth of penetration is determined by
the ease of transportation of corroding species and oxygen through the corrosion path
along the grain boundary. At the limiting depth, intergranular corrosion spreads over
the surface laterally. Intergranular corrosion is highly deleterious because it is difficult
to detect without the help of a microscope. Also, the sharp crack tips serve as stress
raisers making the component more prone to fatigue failure [32, 49].
30
3.2 Exfoliation Corrosion
Exfoliation corrosion is a form of intergranular corrosion also referred to as layered or
stratified corrosion. Exfoliation corrosion involves localized attack and build-up of
insoluble corrosion products along the grain boundary. Figure 3.1 shows an example
of exfoliation corrosion [50]. The expansion of insoluble corrosion products exerts
pressure on the grains causing swelling, leafing or lifting effect as shown by the
arrows in Figure 3.1. Exfoliation corrosion often starts from the sheared edge of the
material and progresses laterally into the material [32, 49, 51].
Exfoliation corrosion is highly deleterious because the corrosion rate is linear. This is
due to continuous splitting action of the grains exposing a fresh, film free surface.
Also, the strength of the material is lost due to the splitting off of uncorroded material
[32, 49].
Figure 3.1: Exfoliation corrosion causing delamination shown by the red arrows [50]
31
Exposure to salt, acidic deposits and high temperature accelerates the delamination of a
susceptible material. Al-Zn-Mg-Cu alloys are highly susceptible to exfoliation
corrosion especially in the peak age (T6) condition. The mechanism involves
electrochemical reaction between grain boundary precipitate (anode) and the matrix
(cathode) accompanied by expansion of insoluble corrosion products [32, 49].
3.3 Stress Corrosion Cracking
Stress corrosion cracking (SCC) is a form of intergranular corrosion that involves the
conjoint interaction of tensile stress, corrosive environment (water, atmospheric
moisture or aqueous solutions) and a susceptible material [32]. SCC often causes
brittle failure of a susceptible material. SCC is also a form of environmentally assisted
cracking because external influence of the environment is required. The stress
required for SCC to occur may be externally applied (due to use of the component in
service) or residual (initiated during manufacturing) at stress levels lower than the
yield stress [32]. As indicated by the arrows, Figure 3.2 shows the presence of stress
corrosion cracks in a component. SCC is highly deleterious because it is difficult to
detect by casual inspection, it causes slight metal loss but higher loss of mechanical
strength. Also, the cracks produced can initiate fast fracture of component as shown in
Figure 3.2 [52]. SCC in aluminium alloys is characterized by the presence of static
tensile stress. Most intergranular cracks are propagated perpendicular to tensile stress
[32, 49]. Fracture mechanics is usually used to evaluate SCC susceptibility. This
involves the use of pre-cracked specimens to relate the plane strain stress intensity at
the crack tip to crack growth velocity [53].
32
Figure 3.2: Stress corrosion cracking (shown by arrows) in a 7075-T6 wing lock [52]
3.3.1 Mechanism of Stress Corrosion Cracking
The actual mechanism of SCC is not fully understood. However, two commonly
accepted theories are stress assisted dissolution and stress sorption cracking
mechanism [33].
Stress assisted dissolution considers that heat treatment develops certain microstructural
features (e.g. grain boundary precipitates, precipitate free zone) with different
electrochemical potentials. In a corrosive environment, certain features may be anodic
with respect to others. This generates a galvanic cell, causing dissolution of the anodic
part leading to crack initiation by formation of pits [33]. Pits serve as stress raisers
such that application of tensile stress causes plastic deformation in the crack tip region
due to high stress concentration. The cold work effect of plastic deformation in this
region increases the local energy level making the material more susceptible to
33
corrosion. Film rupture mechanism proposes that protective film is initiated after
anodic dissolution. However, further application of tensile stress causes rupture of the
passive film, allowing more metal dissolution in the environment and continuous
corrosion of the material [54].
In Al-Zn-Mg-Cu alloys, precipitation of MgZn2 occurs preferentially at the grain
boundary. This creates the precipitate free zone that is depleted of precipitates
adjacent to the grain boundary. The difference in electrochemical potentials sets up a
galvanic corrosion cell between the PFZ and the solute rich matrix causing anodic
dissolution [32, 49]. However, experimental results showing that condensation will
not occur at the tip of a propagating crack at relatively low humidity, suggest that
anodic dissolution might not be responsible for such cracking [55].
The stress sorption cracking mechanism proposes that SCC occurs due to adsorption
of damaging species into the material causing weakening of atomic bonds. The
presence of the damaging species in the interstitial spacing of the grain boundary
reduces the surface energy and weakens the atomic bonds. Hydrogen is a peculiar
damaging specie causing hydrogen damage or hydrogen induced cracking (HIC) [33].
HIC is common in 7xxx aluminium alloys and it is due to incomplete reduction of
hydrogen ion. This causes high concentration of hydrogen atoms. The diffusion of the
atomic hydrogen into the grain boundary of the material causes breakdown of atomic
bonds. Also, the atomic hydrogen could migrate to preferred locations like voids and
combine to produce hydrogen gas. This reaction generates high pressure that causes
rupture of the material [33, 54].
34
3.4 Effect of slip character on stress corrosion cracking in Al-Zn-Mg-Cu
alloys
Aging heat treatment carried out after quenching develops microstructural features
that influence the SCC behavior of a material. An important effect of aging is the
change in slip character of dislocations in the material. Slip character measures the
extent of dispersion of dislocations during plastic deformation and it is an important
factor used to explain susceptibility of 7xxx alloys to SCC [14].
Within the underaged to peak age condition, the precipitates are small and deformable.
This causes long dislocation lines and planar slip character. Figure 3.3 shows planar
slip character of dislocations in a nickel based superalloys [56]. In planar slip, a high
concentration of dislocations form a planar array due to presence of shearable, semi-
coherent or coherent phases like GP zones and intermediate precipitate (η′) structures
as in T6 temper of Al-Zn-Mg-Cu alloys. Dislocations interact with the coherent
precipitates causing shearing of the precipitates and reducing resistance to dislocation
motion. Planar slip bands formed due to this interaction impinges on the grain
boundary causing shear stress concentration. Therefore, in planar slip, cracks with
sharp tips are formed, increasing the susceptibility to SCC [40, 53, 57].
Figure 3.4 shows the wavy slip character of dislocations in a nickel based superalloys
[56]. Overaging heat treatment causes precipitate particles to grow and lose coherency
with the matrix. Due to prolonged aging, there is decrease in the concentration of
dislocations. Dislocation-particle interaction occurs through bypassing the non-
deformable precipitates. This generates wavy slip character that is uniformly
distributed. Lesser concentration of dislocations with wavy slip character causes
blunting of the crack tip thereby increasing SCC resistance [40].
35
.
Figure 3.3: TEM micrograph showing planar dislocation slip in a nickel based
superalloy [56]
Figure 3.4: TEM micrograph showing dislocations in wavy slip in a nickel based
superalloy [56]
36
3.5 Influence of grain boundary precipitate structure on SCC
The structure of the grain boundary precipitate is largely affected by aging treatment.
As aging progresses, there is transition from continuous distribution of precipitates
(formed during the peak age) to discontinuous distribution in the overaged condition.
In Al-Zn-Mg-Cu alloys, overaging decreases the crack growth rate as the grain
boundary precipitates becomes coarse and discontinuous [58]. Grain boundary
precipitate morphology has been widely used to explain the theory that SCC occurs
through anodic dissolution of precipitates in Al-Cu and Al-Zn-Mg-Cu alloys [40].
The actual role of grain boundary precipitates in anodic dissolution mechanism of
SCC is not clear. Decrease in crack growth rate as the size of grain boundary
precipitates increases has been used to explain the decrease in susceptibility of Al-Zn-
Mg-Cu alloy to SCC. One explanation for this is that grain boundary act as internal
sacrificial anode during SCC [40]. This means that in Al-Zn-Mg-Cu alloys, SCC
susceptibility is due to sacrificial dissolution of grain boundary precipitates. In highly
susceptible conditions like T6 temper, small volume of continuous grain boundary
precipitates dissolves sacrificially, thereby increasing cracking along the grain
boundary region. Heat treatment to T7 and RRA temper causes the precipitates to
grow to larger volume such that anodic dissolution does not increase SCC [59].
Higher SCC resistance has also been related to the ability of large grain boundary
precipitates to act as hydrogen discharge sites thereby reducing SCC through HIC [60,
61]. However, other studies have reported that SCC resistance is improved by
increase in the amount of copper in grain boundary precipitates [62].
37
3.6 Influence of magnesium and copper content
Segregation of magnesium has been used to explain hydrogen embrittlement in Al-
Zn-Mg-Cu alloys. Song et al. showed that the amount of magnesium segregated at the
grain boundary decreases as the aging time increases in 7050 alloy aged at 145 oC
[63]. The decrease in magnesium solute segregated at the grain boundary can be
related to increase in the precipitation of MgZn2 precipitate as aging time increases.
Segregation of magnesium solute at the grain boundary accelerates hydrogen
embrittlement by increasing diffusion and absorption of hydrogen. The reaction of
magnesium and hydrogen causes reduction in fracture toughness thereby increasing
grain boundary embrittlement [63]. It has been shown that magnesium is important in
promoting environmentally active mechanical behavior in 7xxx series alloys [64].
This is supported by results showing that:
 magnesium oxide is preferentially developed at intersections of grain boundary
on external surface.
 magnesium segregation is observed at the grain boundary in as-quenched state
[65].
Grain boundary segregation studied by Hepples et al. show that Mg segregated at the
grain boundary in 7150-T651is higher compared to matrix but, grain boundary
segregation of Mg increased as aging increased in T7 and T77 conditions [62]. Higher
SCC resistance in T7 and RRA compared to T651 temper shows that Mg segregation
in the grain might not be the main factor responsible for SCC in Al-Zn-Mg-Cu alloys.
Compositional modifications in the development of Al-Zn-Mg-Cu alloys involve
increasing copper content to improve corrosion resistance as observed in 7079 to 7075
and 7050 alloy [15]. Research work on the effect of copper on SCC shows that
38
increasing the copper content of alloys decreases crack growth velocity in Al-Zn-Mg-
Cu alloys [66]. The presence of copper modifies the difference between the
electrochemical potential at the matrix and the grain boundary region thereby
reducing SCC through an anodic dissolution mechanism [67]. Also, a high amount of
copper slows down the kinetics of hydrogen evolution [68]. Copper also segregates at
the grain boundary causing toughening of the grain boundary region [64]. It has been
reported that copper content in grain boundary precipitate of 7075 alloy in the
overaged condition is higher compared to peak aged condition. This shows that
changes in the chemistry of grain boundary to increase copper content can improve
SCC resistance [62].
3.7 Crack initiation versus propagation and damage tolerance design

requirement
The relationship between stress corrosion crack growth velocity (da/dt) and stress
intensity at the crack tip (K) is shown in the stages involved in SCC. Figure 3.5 shows
the V-K (crack growth velocity versus stress intensity) plot established for materials
that are susceptible to SCC [13]. This plot is used to evaluate SCC behavior of
susceptible materials. As shown in the Figure, the upper limit given as stress intensity
factor (KIC) is a design factor of the material [40]. KIC corresponds to the plane strain
crack tip stress intensity that causes unstable fast fracture [40, 69].
Three distinct regions are shown in Figure 3.5 [69]. Region I on the V-K plot shows
the first stage of SCC at low stress levels. In this region, crack growth rate is
dependent on stress intensity. KISCC is referred to as threshold stress level. At stresses
below the KISCC, unstable crack growth does not occur. In region I, as the stress
intensity increases from KISCC, the crack growth rate increases.
39
KIC
Figure 3.5: Stages of SCC showing KIC and KISCC [13]
Region II shows the second stage of SCC and the crack growth rate is independent of
stress intensity. As stress intensity increases, the velocity of crack growth remains
constant. This shows the influence of other factors like environment and composition
of materials on crack growth rate [69]. In region III, the crack growth rate is
dependent on stress intensity. As the stress intensity approaches KIC, the crack growth
rate also increases causing fracture of the component. Thus, the stages in crack
growth can be divided into crack initiation (stage I), propagation (stage II) and
fracture (stage III) based on Figure 3.5. KISCC (in region I) and plateau velocity (in
region II) are often used to characterize susceptibility or resistance of alloys to SCC.
Higher KISCC and lower plateau velocity are common in SCC resistant tempers like T7
and RRA compared to T6 temper [24].
Although SCC is as a result of several factors, infinite life design can be used to
reduce catastrophic failure due to SCC. This requires that the sum of in-service,
40
residual and fabrication stresses must be below the threshold stress level. However, at
such low stress intensity, the component will be thick and heavy. Conversely,
application of damage tolerance in design enables the structure to accommodate
cracks or flaws within stage I and II such that inspection and repair process would
detect the flaw before it can cause catastrophic failure [70, 71]. Although structures
with thin sections can be designed with this approach, there is higher risk of missing
cracks during inspection causing unexpected fracture of the component.
41
CHAPTER FOUR
EFFECT OF HEAT TREATMENT ON SCC RESISTANCE OF Al-Zn-Mg-Cu

ALLOYS
The main heat treatments that have achieved better resistance to SCC in Al-Zn-Mg-
Cu alloys are overaging (T7) and RRA (T77) heat treatments.
4.1 Overaging
Overaging involves prolonged aging of the alloy beyond maximum hardness from T6
to T7 temper. T6 temper is obtained by SHT at about 465 oC for 1-2 hours followed
by quenching and aging at 121 oC for 24 hours. T7 is obtained by overaging alloy in
T6 temper at about 177 oC for 7-8 hours [1]. Overaging heat treatment achieves
increase in SCC resistance.
A number of factors have been used to explain the improvement in SCC resistance
through overaging heat treatment. It has been reported that overaging causes increase
in size and discontinuity in the distribution of precipitates along the grain boundary as
shown in Figure 2.7 [29]. Discontinuous distribution of large precipitates reduces
anodic dissolution and prevents a continuous path for corrosion along the grain
boundaries [29]. Also, prolonged aging causes transformation of semi-coherent η′
phase to incoherent η phase thereby changing slip character of dislocations at the
grain boundaries from planar to wavy slip. In wavy slip character, homogenous
distribution of dislocations causes blunting of crack tip and increases SCC resistance
[40]. Large grain boundary precipitates formed during overaging can trap atomic
hydrogen to form bubbles. These bubbles cause blunting of the crack tip thereby
reducing susceptibility to SCC through hydrogen embrittlement [24, 33]. However,
the ≈10-15% loss of strength in T7 is very significant in view of high strength:weight
42
requirement for structural parts in aerospace applications. This was the main
motivation for the development of RRA heat treatment.
4.2 Retrogression and reaging
The retrogression and reaging heat treatment was developed by Cina based on the
principle that SCC is due to the high dislocation density formed during quenching
from SHT [14]. RRA involves carrying out peak aging heat treatment to achieve T6
temper followed by retrogression treatment at a temperature higher than age
hardening temperature but below the SHT temperature. As shown in Figure 4.1, 7075
alloys are usually retrogressed at 200-260 oC for about 5 minutes. The retrogression
step is carried out for a short time to prevent overaging. This is followed by reaging
step (at T6 aging condition) to allow precipitation of the strengthening phase to
reoccur [14].
Figure 4.1: Schematic showing retrogression and reaging heat treatment procedure
43
It is believed that the short retrogression step dissolves dislocation network responsible
for SCC [14]. Various works have shown that RRA can achieve high SCC resistance
and high strength and as obtained in T6 and T7 respectively [24, 43, 72]. Figure 4.2
shows the effect of RRA treatment on SCC resistance of 7075 alloy [24]. RRA
samples treated to retrogression heat treatment at 220 oC for 1 and 5 minutes
respectively followed by reaging showed better SCC resistance compared to standard
T6 temper. Also, high SCC resistance was observed in the sample subjected to only
retrogression heat treatment without reaging. This is shown by the higher KISCC and
lower stage II plateau crack growth rate in T7 and RRA samples compared to T6
temper. Further work done by Cina reaffirmed that RRA improves SCC resistance
through dissolution of dislocation density during the retrogression step [14, 73]. It is
believed that the high temperature involved in retrogression step is just enough to
cause dissolution of quenched-in dislocations without causing overaging.
Figure 4.2: Effect of heat treatment on SCC resistance in 7075 alloy heat treated to
T6, T73 and RRA retrogressed at 220oC for 1and 5 minutes respectively [24]
44
Dislocations can transport hydrogen atoms through the grain boundaries. Also, high
dislocation density provides additional stress field at the grain boundary that can
cause crack initiation. Hence, Cina’s work showed that decrease in dislocation density
after RRA treatment can be related to increase in SCC resistance [73].
Increase in SCC resistance through RRA has also been related to large, discontinuously
distributed precipitates at the grain boundary. Figure 4.3 shows discontinuous
distribution of precipitates along the grain boundary of 7075 alloy after RRA
treatment [24, 29, 40]. Since SCC occurs at the grain boundary, discontinuous
distribution of precipitates improves SCC resistance by preventing a continuous path
for corrosion to occur. As explained in the previous chapter, the size of grain
boundary precipitate is also important in preventing SCC. RRA produces coarse
precipitates at the grain boundary region thereby preventing SCC by anodic
dissolution of grain boundary precipitates [29].
However, application of RRA to thick sections of materials is difficult due to the short
retrogression time involved. Although Figure 4.2 shows that longer retrogression time
can achieve higher SCC resistance, Figure 1.4 shows that longer retrogression time
causes overaging and loss of strength. In order to achieve a high SCC resistance and
high strength, it is important to use a very short time for the retrogression step.
However, short retrogression time makes it difficult for the heat treatment to achieve
uniformity in the distribution of properties in thick sections. This limits the
application of RRA heat treatment to thin section of materials. 7075 and 7050 alloys
used as structural materials in aircrafts are usually in thick sections.
45
Figure 4.3: Discontinuous grain boundary precipitates in 7075 RRA [29]
Hence, there is need to develop a heat treatment that will achieve a good combination
of strength and SCC resistance without using high temperature involved in retrogression
process.
4.3 High Temperature Pre-precipitation heat treatment
High temperature pre-precipitation (HTPP) heat treatment has been suggested as a
potential heat treatment procedure that could increase resistance of 7xxx series alloys
to SCC [26, 28]. Figure 4.4 shows the steps involved in HTPP process. HTPP involves
solution heat treatment at a temperature in the single phase region followed by
controlled cooling to a temperature in the two phase region and quenching. This is
followed by aging as shown in Figure 4.4. It is believed that due to the controlled
cooling through the solvus, preferential heterogeneous precipitation will occur at the
grain boundary region.
46
Figure 4.4: High temperature pre-precipitation heat treatment procedure showing
(intermediate) TF/Q temperature
These precipitates serve as nucleation sites for more precipitation to occur during
subsequent artificial aging at the normal T6 conditions [29]. Previous research by
Huang et al. studied the effect of HTPP heat treatment on experimental 7A52 alloy
(composition is included in Table 1.1) [26]. Stepped SHT was carried out at 465 oC
for 30 minutes, heated to 470 oC for 30 minutes and 475 oC for 1 hour. This was
followed by controlled cooling at 30 oC/h to 400 oC. This temperature was held for 30
minutes followed by quenching and aging at 100 oC for 10 hours and 150 oC for 24
hours. The results showed that HTPP can achieve a combination of increase in
strength and resistance to SCC without significant loss of strength (just about 1.8%
loss of strength compared to sample without pre-precipitation) in experimental 7A52
alloy. TEM observation of 7A52 alloy after HTPP showed the presence of finely
distributed coherent, metastable precipitates within the grains and a discontinuous
distribution of incoherent, equilibrium precipitates at the grain boundary region [11].
47
In another study, Huang et al. carried out HTPP treatment on 7055 alloy using stepped
SHT at 450 oC for 1 h, 470 oC for 1 h and 480 oC for 3 h [28]. This was followed by
controlled cooling of different samples at 30 oC/h to 465 oC and 455 oC respectively.
The samples were held at this temperature for thirty minutes before quenching. Aging
was carried out at 130 oC for 24 h. The results showed that HTPP can achieve
discontinuous distribution of precipitates at the grain boundary, decrease dislocation
density and improve SCC resistance without significant loss of strength.
Further study of 7075 alloy by Li et al. showed that HTPP achieved better SCC
resistance, but loss of strength in the alloy [29]. Figure 4.5 shows TEM micrograph of
7075 matrix after HTPP. Figure 4.5 (a) shows that the loss of strength after HTPP can
be explained by decrease in the density of fine, coherent, non-equilibrium precipitates
in the matrix due to loss of solute element to grain boundary region during heterogeneous
precipitation. Hence there is lesser amount of solute available to form the
strengthening precipitates in the matrix [29]. The loss of strength can also be due to
formation of coarse precipitates in the matrix as shown in Figure 4.5 (b). Figure 4.6
shows the precipitate morphology at the grain boundary region. Discontinuous
distribution of equilibrium precipitates observed at the grain boundary region was
related to heterogeneous precipitation due to controlled cooling below the solvus [29].
In view of this, it is important to analyze the effect of HTPP heat treatment on
commercial 7xxx alloys in terms of strength and resistance to SCC. This thesis
research will focus on applying HTPP heat treatment to commercial 7050 and 7075
aluminium alloys. Particularly, the effect of the intermediate temperature to which the
sample is cooled before quenching will be studied and related to strength (measured
in terms of hardness) and electrical conductivity while corrosion resistance will be
determined by exfoliation corrosion and double beam SCC tests.
48
(a) (b)
Figure 4.5: Micrographs of (a) fine and (b) coarse precipitates in the grains of HTPP
temper [29]
Figure 4.6: Discontinuous precipitates at the grain boundary region of HTPP temper
[29]
49
4.4 Effect of heat treatment on grain boundary segregation
Heat treatment affects solute segregation along the grain boundaries. Hepples et al
analyzed the effect of T651, T73 and RRA heat treatment conditions on grain
boundary segregation in 7150 alloy [62]. Figure 4.7 shows that the copper solute
concentration in T651 is high as shown in Figure 4.7 (a). Figure 4.7 (b) and (c) shows
that there is decrease in copper solute concentration at the grain boundary in T73 and
RRA conditions. This corresponds to a higher copper content of grain boundary
precipitates in T73 and RRA compared to T651 temper. Similar trend was observed
for Zn. Low Mg level was observed in T651 but, this increased in T73 and RRA
conditions [62]. Huang et al. showed that HTPP can increase the copper solute
content of grain boundary precipitates [26].
50
Cu
Mg
Zn
(a)
Mg
Cu
Zn
(b)
Mg
Cu
Zn
(c)
Figure 4.7: Concentration profile of Zn, Mg and Cu solute segregated across the grain
boundary of (a) T651 (b) T73 (c) RRA tempers of 7150 alloy [62]
51
CHAPTER FIVE
EXPERIMENTAL PROCEDURE
The effect of HTPP on properties of 7075 and 7050 commercial aluminium alloys
was determined by carrying out HTPP treatment on the as-received tempers of both
alloys (T651 and T74 respectively). Samples of both materials were subjected to
HTPP treatment and standard heat treatments of peak aging (T6) and overaging (T7)
temper. The effect of the heat treatment on hardness and electrical conductivity were
tested before and after aging. Exfoliation corrosion tests were carried out on selected
heat treated samples. Double beam stress corrosion tests were used to determine SCC
resistance of selected heat treated samples. Transmission electron microscopy was
used to study microstructural features responsible for these properties.
5.1 Experimental materials
The materials used in this research are rolled plate of 7075-T651and 7050-T74 of
thickness 1 in and 1.5 in respectively. The actual composition (given by suppliers) and
nominal compositions of the alloys are listed in Table 5.1. The longitudinal (L)
direction is parallel to the rolling direction of the plate, transverse (T) direction is
perpendicular to the rolling direction while short (S) direction is parallel to the
thickness of the plate.
5.2 Heat treatment procedure
The heat treatments applied are standard T6, T7 tempers and ten HTPP treatments.
The heat treatment procedure is listed in Table 5.2. Heat treatments were conducted in
a box furnace shown in Figure 5.1. To achieve the desired sample temperature, a
52
thermocouple located immediately adjacent to the sample was used as an input to the
furnace temperature control. The furnace was heated to 465 oC for about two hours.
Table 5.1: Nominal and actual composition of 7075 and 7050 alloys used*
Composition (wt %)
Alloy Al Zn Mg Cu Fe Si Mn Ti Cr Zr Others
7075 Bal. 5.1- 2.1- 1.2- 0.5 0.4 0.3 0.2 0.2- 0.01 0.5
Nom. 6.1 2.9 2.0 0.3
7075 Bal. 5.6 2.5 1.5 0.2 0.09 0.03 0.03 0.20 0.01 0.03
Act.
7050 Bal. 5.7- 1.9- 2.0- 0.2 0.12 0.1 0.06 0.04 0.08- 0.5
Nom. 6.7 2.6 2.6 0.12
7050 Bal. 6.0 2.2 2.22 0.1 0.04 0.003 0.02 0.004 0.11 0.03
Act.
53
Table 5.2: Analysis of heat treatment procedure
MATERIAL TEMPER HEAT TREATMENT PROCEDURE§
T651 As-received (7075 alloy)

T74 As-received (7050 alloy)
T6 SHT 465 oC/1.5 h + WQ + 121 oC/24 h
T7 SHT 465 oC/1.5 h + WQ + 121 oC/24h + 177 oC /7 h
TF/Q = 455 oC SHT 465 oC/1 h + cool to 455 oC + WQ + 121 oC/24 h
§
SHT-solution heat treatment, WQ-water quench
The samples were then placed in the furnace for SHT. SHT was carried out at 465 oC
and a period of about ten minutes was allowed before starting the solution heat
treatment (SHT) time to allow the sample to reach the solutionizing temperature. For
standard tempers like T6 and T7, SHT was carried out for one and half hours. This
was followed by quenching in cold water at 0 to 2 oC. The time lapse before quenching
did not exceed 15 seconds as specified in the standard [33]. This was followed by
aging at 121 oC for 24 hours using a silicone oil bath shown in Figure 5.2 to obtain T6
temper. T7 temper was obtained by further aging of T6 samples at 177 oC for 7 hours.
54
Figure 5.1: Box furnace used for HTPP treatment
Figure 5.2: Fisher Scientific silicon oil bath used for aging treatment
55
The procedure for HTPP treatment is schematically represented in Figure 5.3. HTPP
samples were first subjected to SHT at 465 oC for one hour followed by slow cooling
at 30 oC/h to an intermediate temperature from 455 to 370 oC at 10 oC intervals. The
intermediate temperature to which the sample was cooled before quenching is referred
to as TF/Q (intermediate temperature between SHT in the furnace and quenching). As
shown in Figure 2.4, the choice of TF/Q temperature is based on the solvus temperature
of the alloy. For 7075 alloy, solvus temperature is approximately at 420 oC. It is
believed that appreciable precipitation would occur just below the solvus temperature.
Hence, cooling to temperatures above and below solvus will show the effect of pre-
precipitation on the properties of the alloys. Previous work show that cooling rate of
30 oC/h has been useful in studying the effect of HTPP on Al-Zn-Mg-Cu alloys [26,
27, 28, 33].
Solution heat
o treatment
465 C Controlled cooling
o
(30 C/h)
o
T F/Q = 455-370 C
Water quenching
o Aging
121 C
1h 24 h
Figure 5.3: Heat treatment procedure for HTPP
56
5.3 Electrical conductivity testing
Following heat treatment, the samples were prepared by polishing to 1200 fine grit on
SiC paper. Electrical conductivity testing was carried out using digital electrical
conductivity tester (EE0021 eddy current device) shown in Figure 5.4. For each
measurement, the meter was first calibrated using standard copper and aluminium
samples of known EC. Percent error in EC measurements is 1.5% of readings. The
probe of the tester was placed on the polished surface to obtain values of electrical
conductivities in the transverse-short (TS) direction. An average of three different
measurements was recorded.
Figure 5.4: EE0021 digital electrical conductivity tester
57
5.4 Hardness testing
Hardness testing was conducted on the same samples used for EC testing using the
Versitron Rockwell tester shown in Figure 5.5. The measurements were taken on
Rockwell scale B recommended for aluminium alloys. Using a standard sample, the
percent error in the measurements is 1.2% of readings. An average of ten different
measurements were taken and recorded in different orientations of long-short (LS),
transverse-long (TL) and transverse-short (TS) respectively.
Figure 5.5: Versitron Rockwell hardness tester
58
5.5 Corrosion tests
5.5.1 Exfoliation corrosion testing
Test specimens of 50×100×5 mm (in LS, TL and TS direction respectively) were cut
from the as-received plates. Exfoliation tests were carried out on samples subjected to
selected heat treatments, including T6, T7 and HTPP treated samples of TF/Q = 455,
425, 405 and 370 oC. Figure 5.6 shows front and back view of a sample prepared for
exfoliation corrosion test. Following heat treatment, samples were prepared by
grinding using SiC paper followed by polishing the surface (TL direction) to 6 micron
and 1 micron using diamond solution. The samples were rinsed with water and dried
in air. The other surfaces apart from the one being observed were coated with paraffin
wax. Exfoliation corrosion test was conducted according to ASTM G34 standard [74].
The test solution had a composition of 4.0 M of NaCl, 0.5 M of KNO3 and 0.1 M of
HNO3. The solution was prepared by dissolving 234 g of NaCl, 50 g of KNO3 and 6.3
mL of conc.(70 wt%) HNO3 in 1litre of distilled water. The solution was maintained
at room temperature [74]. The samples were immersed in the test solution in a
container. The test surface (transverse-long direction) was upward in horizontal
direction to prevent loss of exfoliated material. The specimens were exposed for 48
hours followed by visual inspection. The exfoliation corrosion susceptibility was rated
based on Table 5.3. This rating system is a modified version of the ASTM standard to
better reflect the range of results obtained from this experiment.
59
Table 5.3: Modified exfoliation corrosion rating
CORROSION RATING
RESULT
Severe Exco 8
Moderate Exco 7
Mild Exco 6
Light Exco 5
Severe General 4
Moderate Pitting 3
Light Pitting 2
Areas Unattacked 1
(a) (b)
Figure 5.6: Polished plate prepared for exfoliation corrosion test showing (a) polished
surface (b) unexposed parts coated with paraffin
60
5.5.2 Stress corrosion test (Double beam test)
Stress corrosion testing was carried out using the pre-cracked double beam (DB)
method based on ASTM G168 [75]. Blanks of about 25.4×25.4×127 mm (drawing is
included in appendix A) were cut from plates of 7075 and 7050 alloy respectively.
Modification of ASTM standard is in the use of straight notch at 50o angle for easy
machining. Heat treatment was conducted on these samples based on the procedure
given for selected tempers including standard temper T6, T7 and HTPP treated
samples with TF/Q = 455, 425, 405 and 370 oC for both 7075 and 7050 alloys. T74 (as-
received) condition was also tested for the 7050 alloy. Three samples were tested for
each of the conditions of 7050 alloy. For 7075 alloy, two samples were tested for each
HTPP condition and one sample was used for T6 and T7 temper respectively. Final
machining was carried out after heat treatment to get a smooth surface and to create a
notch in the sample. The samples were machined to notch angle 50o to create a sharp
tip such that the direction of crack growth was in SL (short-long) direction. After
machining, the SL surface was ground using 1200 SiC paper to remove scratches.
This was followed by cleaning using ultrasonic bath to remove grease and dirt.
The DB samples were tested in constant displacement condition by using steel bolts
as shown in Figure 5.7. The steel bolts were mechanically loaded to create a pre-
crack. The length of initial crack (ao) was measured from the load line to the root of
the crack. Load line crack opening displacement (Vo) was measured from the
displacement in the crack opening at the load line. A corrosion solution of 3.62%
NaCl was added to the samples in three drops, twice a day. The temperature during
the test period is provided in appendix B. Measurements of crack length were taken as
average of crack length on both sides of the samples at intervals by using a travelling
61
microscope (Model TVM-02 made by Scientific equipment and services) shown in
Figure 5.8. The greatest possible error is 0.05. To get an accurate crack length
reading, build-up of corrosion products were removed using a soft brush [75]. The
time of taking measurements were recorded in hours. The starting stress intensity K I
as a function of crack length was determined using the relationship between stress
intensity obtained from equation 1 and crack length as shown in Figure 5.9. This
relationship shows the effect of the crack growth on stress intensity. The initiation of
crack causes stress concentration at the crack tip. As the crack length increases, stress
intensity decreases [76]:
KI = (1)
Where:
KI = Starting stress intensity as a function of crack length (MPa√m)
v = Crack opening displacement at load line (m)
a = Average crack length (m)
h = Specimen half height (m)
E= Young’s modulus (MPa)
Kf = Final stress intensity
af = Final crack length
62
Loading bolt
Pre-crack
Figure 5.7: A loaded double beam sample
Figure 5.8: Travelling microscope
63
25
Stress intensity (MPa√m)

20
15
10
0
0 20 40 60 80 100
Crack length (mm)
Figure 5.9: Stress intensity vs crack length as shown in equation 1
5.6 Microstructural Analysis
Optical microscopy was used to analyse the as-received materials and the exfoliation
corrosion path. Samples for these analyses were prepared by:
 Cutting small blanks of about 5 mm thick from the material using Electrical
Discharge Machining.
 Mounting in Phenolic resin using hydraulic mounting press.
 Grinding on SiC paper to 1200 grit size.
 Polishing with 6 and later 1 µm diamond suspension.
 Cleaning with soapy water soaked in cotton wool and rinsing in water.
 Cleaning using Ultrasonic bath for about 15 minutes followed by rinsing with
water, rinsing with alcohol and drying with air.
 Samples were etched in Keller’s reagent (190 ml H20, 5 ml HNO3, 3 ml HCl, 2
ml HF) by swabbing for 20 seconds.
64
Metallographic preparation for Transmission Electron Microscope observation
involved cutting of thin foil from heat treated coupons and grinding on both sides to
obtain a smooth surface on samples of about 100 µm thick. Figure 5.10 shows stages
of sample preparation for TEM analysis. Samples of 3 mm diameter were punched
from these samples and dimpled (to reduce the thickness at the center) to depth of
about 50-60 µm (as shown in Figure 5.10 (a)). This was followed by electropolishing
using an electrolyte of 25% HNO3 and 75% methanol at 20 V, 1 A current. The
temperature of the electrolyte was cooled to -40 oC using liquid nitrogen. Figure 5.10
(b) shows the hole in an electropolished sample. Two grain boundaries were selected
to analyze the segregation of solute elements across grain boundary regions. Using
DigitalMicrograph software, a line scan was drawn across the grain boundary and
Energy-Dispersive X-Ray Spectroscopy (EDS) analysis of various points across the
grain boundary was obtained using a beam diameter of 1nm for EDS analysis in
Scanning Transmission Electron Microscope (STEM) mode. The same procedure was
repeated on another grain boundary and compositions obtained were recorded for
each point.
65
(a) 1000 μm (b)
Figure 5.10: Stages of preparation of 3 mm TEM sample showing (a) dimpled surface
(b) polished surface (arrow shows the hole)
66
CHAPTER SIX
EXPERIMENTAL RESULTS
6.1 Electrical conductivity results
Tables 6.1 and 6.2 show the electrical conductivity (EC) values measured before and
after aging of 7075 and 7050 alloy respectively. EC of as-received material and
standard T6 and T7 tempers are also listed in Table 6.2. Figure 6.1 compares the EC
of 7075 and 7050 alloy (listed in Tables 6.1 and 6.2) in the unaged and aged condition
for all the HTPP and standard T6 and T7 tempers.
As expected, a big change in EC is observed from T6 to T7 temper. It appears that
aging has little effect on EC of HTPP treated samples. This indicates that EC of HTPP
treated samples is determined prior to aging. However, there is gradual increase in the
EC as TF/Q temperature decreases. In fact, 7050 alloy heat treated to HTPP at TF/Q =
370 oC has the same EC as the T7 temper. The results for both alloys shows a sharp
increase in EC for HTPP treated alloys at TF/Q = 445 and 415 oC in both the aged and
unaged conditions. The cause of these changes requires more investigation.
67
Table 6.1: Electrical conductivity results of 7075 alloy before and after aging
ELECTRICAL
HEAT CONDUCTIVITY RESULT
TREATMENT (%IACS)
(7075 ALLOY) Before aging After aging
T651 (as-received) 32.2 33.1

T6 32.2 32.5
T7 32.2 39.3
o
TF/Q = 455 C 32.7 32.6
TF/Q = 445 oC 32.5 32.7
TF/Q = 435 oC 32.9 33.1
TF/Q = 425 oC 34.1 34.0
TF/Q = 415 oC 34.1 34.3
TF/Q = 405 oC 35.8 36.3
. o
TF/Q = 395 C 35.8 36.8
TF/Q = 385 oC 36.5 37.0
TF/Q = 375 oC 37.3 37.5
TF/Q = 370 oC 37.9 38.3
68
Table 6.2: Electrical conductivity results of 7050 alloy before and after aging
ELECTRICAL
HEAT CONDUCTIVITY RESULT
TREATMENT (%IACS)
(7050 ALLOY) Before aging After aging
T74 (as-received) 32.4 42.1

T6 32.4 32.6
T7 32.4 40.2
TF/Q = 455oC 32.5 32.7
TF/Q = 445 oC 32.4 33.0
o
TF/Q = 435 C 34.8 34.4
TF/Q = 425 oC 35.6 35.1
TF/Q = 415 oC 35.6 35.3
TF/Q = 405 oC 37.0 37.2
TF/Q = 395 oC 37.0 37.8
TF/Q = 385 oC 37.5 38.3
TF/Q = 375 oC 38.4 39.3
TF/Q = 370 oC 38.7 40.1
69
Electrical Conductivity (%IACS)
44
42 T74
40 T7
7050 unaged
T7
38
7075 unaged
36
7050 aged
34
7075 aged
32
30
T651 T6 455 445 435 425 415 405 395 385 375 370
TF/Q (oC)
Figure 6.1: Effect of heat treatment on electrical conductivity of 7075 and 7050
alloys. Green broken lines indicate as-received T74 and standard T7 temper of 7050
alloy. Purple line indicates standard T7 temper of 7075 alloy
6.2 Hardness results
Tables 6.3-6.6 list the hardness measurements of 7075 and 7050 alloys before and
after aging. In tables 6.4 and 6.6, hardness of the as-received material and standard
tempers T6 and T7 are also listed. Figure 6.2 and 6.3 shows the effect of HTPP heat
treatment on hardness of 7075 and 7050 alloy respectively.
It is evident from these results that there is loss of strength in the alloys before aging
was applied. Compared to T6 temper, about 7% loss of hardness in T7 temper can be
observed in both alloys after aging. This result is comparable to 10-15% loss of yield
strength in T7 temper reported in the literature [10]. The results show that subsequent
70
aging of HTPP treated samples increases the hardness in both alloys. However,
hardness decreases as the TF/Q temperature decreases.
Table 6.3: Hardness result (HRB) of 7075 alloy before aging
Heat Treatment LT LS TS
T6 36.0 36.0 36.0

o
TF/Q = 455 C 45.1 47.0 47.5
TF/Q = 445 oC 44.8 45.3 49.1
TF/Q = 435 oC 34.7 39.2 37.0
TF/Q = 425 oC 33.6 36.2 36.5
TF/Q = 415 oC 32.8 35.6 35.0
TF/Q = 405 oC 21.4 25.5 24.2
o
TF/Q = 395 C 21.2 23.8 23.2
TF/Q = 385 oC 18.0 21.3 23.8
TF/Q = 375 oC 14.0 14.0 14.3
TF/Q = 370 oC 14.0 14.6 16.7
71
Table 6.4: Hardness result (HRB) of 7075 alloy after aging
T651 (as-received) 89.2 89.5 89.3

T7 83.6 82.4 81.1
T6 90.0 89.0 90.0
TF/Q = 455 oC 90.7 91.0 90.7
TF/Q = 445 oC 91.3 91.2 90.2
o
TF/Q = 435 C 90.6 90.7 91.0
TF/Q = 425 oC 87.2 89.1 88.8
TF/Q = 415 oC 88.0 88.0 88.3
TF/Q = 405 oC 81.0 85.1 83.8
TF/Q = 395 oC 73.8 74.0 75.0
TF/Q = 385 oC 69.2 72.5 73.6
TF/Q = 375 oC 64.8 67.6 66.4
TF/Q = 370 oC 63.0 62.7 65.0
Table 6.5: Hardness result (HRB) of 7050 alloy before aging
T6 32.0 34.5 32.0

TF/Q = 455 oC 40.5 45.0 47.1
o
TF/Q = 445 C 39.3 40.7 42.7
TF/Q = 435 oC 22.9 26.2 25.0
TF/Q = 425 oC 20.6 23.5 21.8
TF/Q = 415 oC 23.0 23.9 22.0
TF/Q = 405 oC 17.2 16.5 16.0
TF/Q = 395 oC 14.0 14.0 14.0
o
TF/Q = 385 C 14.0 14.0 14.0
TF/Q = 375 oC 14.0 14.0 14.0
TF/Q = 370 oC 14.0 14.0 14.0
72
Table 6.6: Hardness result (HRB) of 7050 alloy after aging
Heat treatment LT LS TS
T74 (as-received) 84.5 83.8 85.4

T7 84.0 86.0 85.0
T6 90.0 90.0 90.0
TF/Q = 455 oC 91.0 91.0 91.8
TF/Q = 445 oC 90.6 91.5 91.3
TF/Q = 435 oC 90.1 90.4 90.0
TF/Q = 425 oC 89.0 89.4 89.0
TF/Q = 415 oC 89.1 89.6 89.1
o
TF/Q = 405 C 87.2 88.3 87.5
TF/Q = 395 oC 85.1 86.0 86.0
TF/Q = 385 oC 84.0 83.0 84.4
TF/Q = 375 oC 81.8 84.0 83.6
TF/Q = 370 oC 67.9 75.7 74.0
73
100
90
80
T7
70
Hardness (HRB)
60
50
40
30
7075 unaged
20 7075 aged
10
0
T651 T6 455 445 435 425 415 405 395 385 375 370
TF/Q (oC)
Figure 6.2: Effect of HTPP heat treatment on hardness of 7075 alloy. The green
broken line shows hardness obtained for T7 temper
100
90
80 T7/T74
70
Hardness (HRB)
60
50
7050 unaged
40
7050 aged
30
20
10
0
T6 455 445 435 425 415 405 395 385 375 370 T7
TF/Q (oC)
Figure 6.3: Effect of HTPP heat treatment on hardness of 7050 alloy. The red broken
line shows hardness obtained for T74 and T7 temper
74
6.3 Corrosion test results
6.3.1 Exfoliation corrosion result
The samples used for exfoliation corrosion tests are shown in Figures 6.4 and 6.5 for
7075 and 7050 alloy respectively. The results presented in these Figures show one
sample out of the two samples tested for each condition. The extent of exfoliation
corrosion was rated based on the surface appearance of samples after exposure to
exfoliation corrosion solution for 48 hours as shown in Table 6.7.
It is evident that both alloys are susceptible to exfoliation corrosion in almost all the
conditions. From Figure 6.4 and 6.5 (a) and (b), T6 and TF/Q = 455 oC samples showed
severe exfoliation and loss of material across the entire surface. Both alloys showed
light exfoliation in TF/Q = 425 oC conditions. From Figure 6.4 and 6.5 (d) and (e), it
appears that samples treated to TF/Q = 405 oC were more susceptible to exfoliation
corrosion than TF/Q = 425 oC conditions. The cause of this variation in EXCO
resistance despite lower TF/Q should be further investigated. From Figure 6.4 and 6.5
(e), TF/Q = 370 oC samples showed general pitting across the surface of the samples.
Figure 6.4 and 6.5 (f) shows that T7 temper is highly resistant to exfoliation corrosion.
These results show that, samples treated to HTPP at TF/Q = 425 and 370 oC showed
better resistant to exfoliation corrosion compared to T6 and other HTPP conditions.
Although, none of the HTPP treated samples achieved as good corrosion resistance as
T7 temper, samples treated to TF/Q = 370 oC showed comparable exfoliation corrosion
resistance to the T7 temper. The TF/Q = 370 oC samples showed pitting corrosion while
few pits were observed in T7 temper. The presence of pits has been related to increase
in EXCO resistance in RRA treated 7150 alloy [62].
75
Figure 6.6 shows the optical micrograph of an exfoliated sample. It is evident from
the image that exfoliation corrosion is an intergranular corrosion that occurs
preferentially at the grain boundaries. The disintegration of grains observed in the
image also shows the leafing effect of corrosion products in exfoliation corrosion. The
pitting corrosion observed in T7 samples and HTPP samples treated to TF/Q = 370 oC
of both alloys show that there is a direct relationship between exfoliation corrosion
and SCC.
Table 6.7: Exfoliation corrosion (EXCO) rating of heat treated samples
Temper 7050 alloy 7075 alloy 7050 7075

Electrical Electrical EXCO EXCO
Conductivity Conductivity rating rating
(%IACS) (%IACS)
T6 32.6 32.5 8 8
TF/Q = 455 oC 32.7 32.6 7 8
TF/Q = 425 oC 35.1 34.0 5 5
o
TF/Q = 405 C 37.2 36.3 6 7
TF/Q = 370 oC 40.1 38.3 4 4
T7 40.2 39.3 1 1
76
10cm
10 cm
Figure 6.4 (a): EXCO sample of 7075 alloy in T6 temper showing severe exfoliation
and disintegration of the sample surface
10 cm
Figure 6.4 (b): EXCO sample of HTPP treated 7075 alloy at TF/Q= 455 oC showing
severe exfoliation and disintegration of sample surface
77
10 cm
Figure 6.4 (c): EXCO sample of HTPP treated 7075 alloy at TF/Q= 425 oC showing
light exfoliation on sample surface
10 cm
Figure 6.4 (d): EXCO sample of HTPP treated 7075 alloy at TF/Q= 405 oC showing
moderate exfoliation on sample surface
78
10 cm
Figure 6.4 (e): EXCO sample of HTPP treated 7075 alloy at TF/Q= 370 oC showing
severe general pitting on sample surface
10 cm
Figure 6.4 (f): EXCO sample of 7075 alloy in T7 temper showing some pitting and
unattacked areas on the sample surface
Figure 6.4: EXCO behaviour of 7075 samples in (a) T6 (b) TF/Q = 455 oC (c) TF/Q =
425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC (f) T7 temper
79
10 cm
Figure 6.5 (a): EXCO sample of 7050 alloy inT6 temper showing severe exfoliation
of sample surface
10 cm
Figure 6.5 (b): EXCO sample of HTPP treated 7050 alloy at TF/Q = 455 oC showing
severe exfoliation corrosion on sample surface
80
10 cm
Figure 6.5 (c): EXCO sample of HTPP treated 7050 alloy at TF/Q = 425 oC showing
light exfoliation of sample surface
10 cm
Figure 6.5 (d): EXCO sample of HTPP treated 7050 alloy at TF/Q = 405 oC showing
mild exfoliation of sample surface
81
10 cm
Figure 6.5 (e): EXCO sample of HTPP treated 7050 alloy at TF/Q = 370 oC showing
some pits and areas unattacked on sample surface
10 cm
Figure 6.5 (f): EXCO sample of 7050 alloy in T7 temper showing some pits and areas
unattacked on sample surface
Figure 6.5: EXCO samples of 7050 alloy in (a) T6 (b) TF/Q = 455 oC (c) TF/Q = 425 oC
(d) TF/Q = 405 oC (e) TF/Q = 370 oC (f) T7 temper
82
Figure 6.6: Optical micrograph of a section of an exfoliated sample showing
intergranular corrosion
6.3.2 Stress Corrosion Cracking results
Tables 6.8 and 6.9 summarize SCC results obtained from double beam samples of
7075 and 7050 alloys respectively. The SCC behaviour of heat treated samples was
measured in terms of crack length versus time. The data for these results are in
appendix C. Since more than one samples were tested, Figure 6.7 compares change in
crack length in each sample of TF/Q = 455 and 370 oC 7075 alloy. This Figure shows
the consistency and similarity in trends for results obtained from samples with the
same heat treatment condition.
83
Table 6.8: Summary of results obtained from 7075 double beam samples
Initial Final
Crack Initial Final stress stress
opening crack crack intensity intensity
Heat Time displacement length length KI Kf
Treatment (h) Vo (m) ao (m) af (m) (MPa√m) (MPa√m)
T6 746 0.0004 0.018 0.117 24.18 1.01
T7 1346 0.0003 0.016 0.024 27.12 15.6
TF/Q = 455 oC 746 0.0004 0.018 0.117 23.41 1.01
TF/Q = 425 oC 746 0.0004 0.016 0.116 24.19 0.87
TF/Q = 405 oC 1346 0.0004 0.018 0.116 24.37 1.00
TF/Q = 370 oC 1446 0.0004 0.016 0.043 27.61 6.38
Table 6.9: Results obtained from 7050 double beam samples
Initial Final
Crack Initial Final stress stress
opening crack crack intensity intensity
Heat Time displacement length length KI Kf
Treatment (h) Vo (m) ao (m) af (m) (MPa√m) (MPa√m)
T6 746 0.0003 0.016 0.117 23.91 0.87

T7 1346 0.0003 0.016 0.024 26.93 14.54
T74 1346 0.0003 0.013 0.014 28.34 24.96
TF/Q = 455 oC 1146 0.0004 0.018 0.116 23.89 1.03
TF/Q = 425 oC 1346 0.0004 0.018 0.111 24.50 1.25
TF/Q = 405 oC 1346 0.0003 0.015 0.096 24.28 1.39
TF/Q = 370 oC 1346 0.0004 0.018 0.069 24.93 2.61
84
140
120
455 o1C-Sample 1
TF/Q=455-
7075
Crack length (mm)
100
TF/Q455-2 o
= 455 C-Sample 2
80 7075
60 TF/Q= 370 oC-Sample 1

7075 370-1
40
7075
TF/Q=370-2
370 oC-Sample 2
20
0
0 200 400 600 800 1000 1200 1400
Time (h)
Figure 6.7: Comparism of crack length with time in two SCC samples for each of
7075 alloy treated at HTPP condition TF/Q = 455 and 370 oC
Figures 6.8 and 6.9 show the effect of heat treatment on SCC resistance (of 7075 and
7050 alloys respectively) measured in terms of the crack length at time intervals. The
results show that T6 temper is very susceptible to SCC while T7 is very resistant. The
results show that HTPP improved the resistance to SCC in all the conditions tested.
This is shown by the gradual decrease in the crack length as TF/Q decreases. It is
evident from these results that HTPP heat treatment affects SCC resistance of both
7075 and 7050 alloy.
Figure 6.10 and 6.11 show the results obtained from crack growth rate (da/dt or V)
versus stress intensity (K) for each of the tested condition in 7075 and 7050 alloy
respectively. Data for all the samples and conditions tested are included in appendix
C. The plots show the stages of SCC during the test. Figures 6.12 and 6.13 show the
summary of V-K plot of all the tested conditions for 7075 and 7050 alloy
85
respectively. The results show that the corrosion rate decreased as the TF/Q decreased.
This is shown in the decrease in the plateau velocity and threshold stress intensity as
TF/Q decreases as shown in Figures 6.12 and 6.13. This shows that HTPP can improve
SCC resistance in 7075 and 7050 alloys. In Figure 6.12, it appears that at TF/Q = 370
o
C and T7 conditions, the stress corrosion cracking of 7075 alloy remained in stage II.
This shows that TF/Q = 370 oC and T7 conditions are highly resistant to SCC. Figure
6.13 shows that similar trend of decrease in the plateau velocity and threshold stress
intensity as TF/Q decreases was obtained in 7050 alloy. These results show that
compared to T6 temper HTPP can achieve increase in SCC resistance but, none of the
HTPP conditions achieved better SCC resistance compared to T7 and T74 tempers.
From Figure 6.13, it appears that T74 temper has better SCC resistance compared to
T7. The high SCC resistance in T74 temper can be attributed to the effect of cold
work after heat treatment.
Generally, it is believed that 7050 alloy has higher SCC resistance than 7075 alloy.
This is observed in all the conditions tested except for HTPP treated sample at TF/Q =
370 oC. Figure 6.14 compares V-K plot of 7075 and 7050 alloys at TF/Q = 370 oC
condition. It is noteworthy that at TF/Q = 370 oC, 7050 alloy showed a lesser SCC
resistance compared to 7075 alloy. Similar observation is noticed in results shown in
Figure 6.8, 6.9, 6.12 and 6.13. By comparing the corrosion results at TF/Q = 370 oC to
EC results in Figure 6.1, 7075 alloy has lesser EC compared to 7050 alloy. This
shows that other factors are involved in determining SCC behaviour of different
alloys. Further investigation is required to explain this anomaly in SCC behaviour of
7050 versus 7075 alloy.
The SCC behaviour observed in this research is shows similar trend to previous
studies in the literature. By comparing this result to result obtained by Rajan et al for
86
SCC behaviour of 7075-T651 temper and Huang et al for 7055 at TF/Q = 455 oC,
similar trend of increase in SCC resistance was observed in HTPP treated condition
compared to the T651 temper [24, 28]. However, it appears that results obtained from
this study show that the corrosion rate is faster compared to previous studies. The
faster corrosion rate in the present work can be attributed to higher humidity of the
environment and higher concentration of salt in the solution used in this study.
140
120
Crack length (mm)
100 T6
455
TF/Q= 455 oC
80
425
T = 425 oC
F/Q
60 405
TF/Q= 405 oC
370
T = 370oC
F/Q
40
T7
20
0
0 200 400 600 800 1000 1200 1400 1600
Time (h)
Figure 6.8: Average crack length with time of 7075 double beam samples
87
140
120 T6
455
Crack length (mm)
100 TF/Q= 455 oC

TF/Q= 425 oC
425
80
405
TF/Q= 405 oC
60
370
TF/Q= 370oC
40 T7
20 T74
0
0 200 400 600 800 1000 1200 1400 1600
Time (h)
Figure 6.9: Average crack length with time of 7050 double beam samples
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Stress Intensity (MPa√m)
Figure 6.10 (a): Crack growth velocity vs stress intensity of 7075 alloy in T6 temper
88
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.10 (b): Crack growth velocity vs stress intensity of HTPP treated 7075 alloy
at TF/Q = 455 oC
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.10 (c): Crack growth velocity vs stress intensity of HTPP treated 7075 alloy
at TF/Q = 425 oC
89
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.10 (d): Crack growth velocity vs stress intensity of HTPP treated 7075 alloy
at TF/Q = 405 oC
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.10 (e): Crack growth velocity vs stress intensity of HTPP treated 7075 alloy
at TF/Q = 370 oC
90
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.10 (f): Crack growth velocity vs stress intensity of 7075 alloy in T7 temper
Figure 6.10: Crack growth velocity vs stress intensity of 7075 samples showing (a) T6
(b) TF/Q = 455 oC (c) TF/Q = 425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC (f) T7
91
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (a): Crack growth velocity vs stress intensity of 7050 alloy in T6 temper
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (b): Crack growth velocity vs stress intensity of HTPP treated 7050 alloy
at TF/Q = 455 oC
92
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (c): Crack growth velocity vs stress intensity of HTPP treated 7050 alloy
at TF/Q = 425 oC
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (d): Crack growth velocity vs stress intensity of HTPP treated 7050 alloy
at TF/Q = 405 oC
93
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (e): Crack growth velocity vs stress intensity of HTPP treated 7050 alloy
at TF/Q = 370 oC
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (f): Crack growth velocity vs stress intensity of 7050 alloy in T7 temper
94
10
1
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.11 (g): Crack growth velocity vs stress intensity of 7050 alloy in T74
Figure 6.11: Crack growth velocity vs stress intensity of 7050 samples showing (a) T6
(b) TF/Q = 455 oC (c) TF/Q = 425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC (f) T7 (g) T74
95
10
T6 & TF/Q = 455 oC
TF/Q = 425, 405 oC
1
TF/Q = 370 oC
da/dt (mm/h)
0.1
0.01
T7
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.12: Summary of V-K plot for 7075 alloy
10 T6 & TF/Q = 455 oC
TF/Q = 425, 405 , 370 oC

1
T7
da/dt (mm/h)
0.1
T74
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.13: Summary of V-K plot for 7050 alloy
96
10
7050 TF/Q = 370 oC
1
7075 TF/Q = 370 oC
da/dt (mm/h)
0.1
0.01
0.001
0.0001
0 5 10 15 20 25 30
Figure 6.14: Comparism of SCC behaviour in 7050 and 7075 alloy at TF/Q = 370 oC
At the end of the experiment, the samples were broken by mechanical overload.
Figure 6.15 shows the fractured surface of double beam samples of 7050 alloy in T6
and TF/Q = 370 oC condition after SCC test. As shown by the blue arrows in Figure
6.15 (b), the fractured surfaces show the initial crack initiated through mechanical
loading. Addition of corrosive solution to the crack caused stress corrosion crack to
propagate and grow with time. As shown in the TF/Q = 370 oC sample, this is a form of
brittle failure accompanied by crack tunnelling (shown by red arrows). Crack
tunneling is the difference in crack length at midsection of sample compared to the
sample surface. Longer crack length can be observed at the mid-section due to a plane
strain condition at the mid-section versus a plane stress condition at the surface.
97
1 cm
(a)
(b) 1 cm
Figure 6.15: Double beam samples of 7050 alloy in (a) T6 (b) TF/Q = 370 oC
condition after SCC testing. The blue arrows indicate crack growth from right to left.
The red arrows indicate longer crack length in the mid-section compared to the
surface (crack tunneling)
6.4 Results of microstructural analysis
Optical microscopy was used to analyze the as-received material as shown in Figure
6.16. From Figure 6.16 the elongated grains in the alloys are shown. TEM analysis of
both alloys as shown in Figure 6.17 shows the effect of compositional modification on
98
the alloys. Both Figure 6.16 and 6.17 show the effect of compositional modification
on the microstructure of the alloys. High concentration of constituent particles can be
observed in 7075 alloy as shown in Figure 6.17 (a). Reducing the composition of iron
and silicon (as shown in Table 5.1) reduced the constituent particles in 7050 alloy
thereby improving the properties of the alloy and homogeneity of the microstructure.
(a) (b)
Figure 6.16: Optical images of as received (a) 7075-T651 and (b) 7050-T74 alloy in
SL direction
(a) (b)
Figure 6.17: Effect of compositional modification on the microstructure of (a) 7075
and (b) 7050 alloy. Red arrows indicate large constituent particles in 7075 alloy
99
6.5 Microstructural analysis of unaged samples using TEM
TEM was used to study grain boundary precipitate morphology of some selected
tempers of 7075 and 7050 alloys in the unaged condition as shown in Figure 6.18 and
6.19 respectively. Red arrows indicate dislocation network while yellow arrows
indicate grain boundary precipitation. Figure 6.18 (a) and (b) shows unaged 7075-T6
sample. In Figure 6.18 (b), the sample orientation shows high density of quenched-in
dislocations. A similar result was obtained for 7050 alloy as shown in Figure 6.19 (b).
High dislocation density is expected in HTPP treated sample of T F/Q = 455 oC due to
quenching from a high TF/Q temperature. Figure 6.18 (c) and (d) shows HTPP treated
sample of TF/Q = 405 and 370 oC respectively. It appears that the density of dislocations
decreases as the TF/Q temperature decreases. This may be due to quenching from a
lower temperature as TF/Q decreases. Also, decreasing TF/Q causes some heterogeneous
precipitation at the grain boundary as shown in Figure 6.18 (c) and (d). A similar
trend was observed in 7050 alloy as shown in Figure 6.19 (c) and (d). The contrast
lines in Figure 6.19 (d) can be attributed to slight changes in thickness and bending of
sample.
100
(a) (b)
(c) (d)
Figure 6.18: TEM analyses of unaged 7075 alloy in (a) and (b) T6 (c) TF/Q= 405 oC
(d) TF/Q= 370 oC. Red arrows indicate dislocation network. Yellow arrows indicate
precipitation along the grain boundary
101
(a) (b)
(c) (d)
Figure 6.19: TEM analyses of unaged 7050 alloy in (a) and (b) T6 (c) TF/Q = 405 oC
(d) TF/Q = 370 oC. Red arrows indicate dislocation network. Yellow arrows indicate
precipitation along the grain boundary
102
6.6 Microstructural analysis of aged samples using TEM
After aging, TEM was used to analyse the precipitate morphology in the grain
boundary region of the alloys. Figure 6.20 and 6.21 shows TEM analyses of the grain
boundary region of 7075 and 7050 respectively. The results presented in this thesis
were obtained after examining minimum of two grain boundaries. The grain
boundaries are shown as either tilted or in planar view to the direction of TEM beam.
As shown in Figure 6.20 (a), tilted view gives a partial plan view of the precipitates in
the grain boundary region to provide more information on the density of precipitates
along the grain boundary region. As shown in Figure 6.20 (f) planar view shows the
precipitates lying in one plane.
In Figure 6.20 and 6.21 (a) small precipitates are continuously distributed along the
grain boundary in T6 treated samples as expected. Figure 6.20 and 6.21 (b)-(e) show
that HTPP heat treatment affects the microstructure of both 7075 and 7050 alloy
respectively. As shown by the yellow arrows, there is gradual increase in the size of
the grain boundary precipitates as TF/Q temperature decreases in both 7075 and 7050
alloy respectively. Although Figure 6.20 (f) is in planar view, it is obvious that there
are discontinuous, large precipitates along the grain boundary. Similar result was
obtained for 7050 alloy as shown in Figure 6.21 (f).
103
(a) (b)
(c) (d)
(e) 200nm (f)

Figure 6.20: TEM analysis of grain boundary precipitate morphology of 7075 alloy in
(a) T6 (b) TF/Q = 455 oC (c) TF/Q = 425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC (f) T7.
Yellow arrows indicate precipitation along the grain boundary
104
(a) (b)
(c) (d)
(e) 200nm (f)

Figure 6.21: TEM analysis of grain boundary precipitate morphology of 7050 alloy in
(a) T6 (b) TF/Q = 455 oC (c) TF/Q = 425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC (f) T7.
Yellow arrows indicate precipitation along the grain boundary
105
6.7 Energy Dispersive X-ray Spectrometry (EDS) analysis
Figures 6.22 and 6.23 show the mean solute concentration of Zn, Mg and Cu solutes
segregated across two grain boundaries in 7075 and 7050 alloy respectively. Solute
segregation at the grain boundary has been suggested to have influence on SCC
resistance of Al-Zn-Mg-Cu alloys [60]. Decrease in solute segregation can be related
to increase in solute concentration of grain boundary precipitates. The presence of
copper in grain boundary precipitates has been reported in some SCC resistant alloys
[63]. Results obtained in Figures 6.22 and 6.23 provide an overview of the amount of
Zn, Mg and Cu segregated at the grain boundary. Note that some scatters are present
in the result due to slight variation in solute concentration at different grain
boundaries as shown in Figure 6.24. Variation of about 1nm was also observed in the
position of the beam across the grain boundary. Corresponding data for Figure 6.22
and 6.23 are in appendix D.
106
(a) (b)
(c) (d)
(e) (f)
Figure 6.22: EDS analysis across grain boundary of 7075 samples showing (a) T6 (b)
TF/Q = 455 oC (c) TF/Q= 425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC and (f) T7. As
shown in Figure 6.23 (f) the blue line represents Zn, red represents Mg and green
represents Cu
107
(a) (b)
(c) (d)
(e) (f)
Figure 6.23: EDS analysis across grain boundary of 7050 samples showing (a) T6 (b)
TF/Q = 455 oC (c) TF/Q = 425 oC (d) TF/Q = 405 oC (e) TF/Q = 370 oC and (f) T7. As
shown in Figure 6.24 (f) the blue line represents Zn, red represents Mg and green
represents Cu
108
12
10
Composition (wt%)
8
6 Zn
Mg
4
Cu
2
0
-15 -10 -5 0 5 10 15
Distance from grain boundary (nm)
Figure 6.24: EDS analysis showing the extent of scatter in results for 7075 alloy at
TF/Q = 425 oC
109
CHAPTER SEVEN
DISCUSSION OF RESULTS
7.1 Effect of heat treatment on electrical conductivity of 7075 and 7050 alloys
Figure 7.1 summarizes the effect of standard heat treatments and HTPP process on EC
of aged 7050 and 7075 alloys. The result shows the EC of T6 as the lowest and
T7/T74 temper as the highest. It is evident from this result that HTPP achieved
increased EC in both alloys as TF/Q decreases and this provides a range of EC values
between T6 and T7 temper. The increase in EC as TF/Q decreases may be explained by
decrease in the concentration of solute due to loss of solute during pre-precipitation.
Hence, there is decrease in resistance to flow of electrical current and an increase in
EC. Another explanation for the increase in EC might be due to decrease in strain at
the precipitate-matrix interface as the precipitates transform from coherent to semi-
coherent or incoherent as TF/Q decreases. Further investigation will be required to
confirm this explanation [77]. The higher EC observed in 7050 compared to 7075
alloy might be due to lower impurity levels in 7050 alloy. The arrows in Figure 7.1
indicates sharp increase in EC observed at about TF/Q = 445 oC and 415 oC.
110
45
44
Electrical conductivity (%IACS) 43
42 T74
41
40 T7
39 T7
38
37
36 7050 aged
35
34 7075 aged
33
32
31
30
T651 T6 455 445 435 425 415 405 395 385 375 370
TF/Q (oC)
Figure 7.1: Effect of heat treatment on electrical conductivity of 7050 and 7075 alloy.
Blue arrows indicate the sharp increase in electrical conductivity
7.2 Effect of heat treatment on hardness of 7050 and 7075 alloys
Figure 7.2 compares the effect of standard T6, T7 and HTPP heat treatment
conditions on the hardness of both 7050 and 7075 alloys. Both alloys experienced loss
of strength before aging. This is due to dissolution of strengthening phases and loss of
solute atoms during pre-precipitation. The results show that subsequent aging of
HTPP treated samples increases the hardness in both alloys. The increase in strength
of the alloys after aging is due to formation of strengthening precipitate phase.
However, strength decreases as the TF/Q temperature decreases. This is likely due to
decrease in the solute atoms available for homogenous precipitation during aging. As
TF/Q decreases more pre-precipitation occurs causing loss of solute atoms to
heterogeneous precipitation during slow cooling to intermediate (TF/Q) temperature.
111
However, gradual loss of hardness was observed as TF/Q decreased from 435 oC. This
might be due to the solvus temperature being in that temperature range, causing more
pre-precipitation to occur. Sharp changes in hardness comparable to the changes noted
by the arrows in Figure 7.1 can be observed in Figure 7.2. From Figure 7.2, the
hardness result of both alloys in the unaged condition show that significant changes in
the hardness started at 445 oC. Thus, the solvus temperature can be estimated to be at
445-435 oC. Figure 7.3 shows that different phases can be nucleated during cooling
below the solvus. Just below the solvus, the arrow shows that nucleation of η phase
occurs and as the TF/Q temperature decreases, other phases will be formed. Thus, the
sharp changes observed in EC and hardness might be related to nucleation of different
phases. Further research using Differential Scanning Calorimetry (DSC) is required to
confirm this conclusion.
It is evident that 7050 alloy can be treated to higher hardness than 7075 through
HTPP. This can be related to the effect of compositional modification in replacement
of Cr with Zr in 7050 to reduce quench sensitivity associated with 7075 alloy. In fact,
TF/Q up to 385 oC in 7050 alloy achieves better hardness compared to T7 temper.
112
100
90
80
T7
70
Hardness (HRB)
60 7050 unaged
50
7075 unaged
40
30 7050 aged
20 7075 aged
10
0
T651 T6 455 445 435 425 415 405 395 385 375 370
TF/Q (oC)
Figure 7.2: Effect of heat treatment on hardness of 7050 and 7075 alloys. Purple
broken line indicates standard T7 temper. Blue arrows indicate sharp decrease in
hardness
Figure 7.3: Nucleation of precipitate phases during controlled cooling possibly

causing the marked changes observed in EC and hardness results
113
7.3 Exfoliation Corrosion (EXCO) versus Electrical conductivity of 7075 and
7050 alloy
Electrical conductivity is often used to assess and predict corrosion resistance in 7xxx
alloys especially in T6 and T7 tempers. Figure 7.4 relates the exfoliation corrosion
resistance of both alloys to electrical conductivity at different heat treatment
conditions. The general trend observed in this result is that exfoliation corrosion
susceptibility decreases as EC increases. EC obtained at TF/Q = 370 oC in 7050 alloy is
almost the same as T7 temper but T7 showed higher resistance to exfoliation
corrosion.
42 9
8
40
7
38 6
EC (% IACS)
EXCO rating
5 7050 EC
36
4 7075 EC
7050 exco rating
34 3
7075 exco rating
2
32
1
30 0
T6 455 425 405 370 T7
o
TF/Q ( C)
Figure 7.4: Effect of heat treatment on EC and EXCO resistance
114
7.4 Effect of HTPP on Stress corrosion cracking of 7075 and 7050 alloy
Figure 7.5 relates EC to SCC resistance in both alloys (using crack length measurement
after 257 hours) for T7 and T6 tempers and the tested HTPP conditions. It is evident
that there is a relationship between SCC resistance and EC measured as T F/Q
decreases. Although the mechanism is not clear, these results show that SCC
resistance in HTPP treated alloys is directly related to EC measurement. This is
shown by decrease in crack length as EC increases. Figures 7.6 and 7.7 relate SCC
resistance (based on the crack growth rate at stress intensity of 3 MPa√m) of 7075 and
7050 alloy in different heat treatment conditions to EC and the approximate time to
reach stress intensity of 3 MPa√m (corresponding to ≈69 mm based on Figure 5.9). It
is evident from these results that the crack growth rate is inversely proportional to EC
and time to reach stress intensity of 3 MPa√m in stage II of SCC. This confirms that
SCC is directly related to EC. These results also show that each HTTP treatment has
significant effect on the microstructure thereby increasing SCC resistance of the
alloys. HTPP heat treatment reduces the crack growth rate, achieves increase in the
EC and time involved in crack propagation and this relates to the observed increase in
SCC resistance as the TF/Q temperature decreases.
115
140
120 425
Crack length (mm) 100 455 &
T6 405
80 370
60
40
T7
20
0 7050
30 31 32 33 34 35 36 37 38 39 40 41
7075
Electrical conductivity (%IACS)
Figure 7.5: Relationship between EC and SCC resistance (using crack length
measured after 257 hours) of 7075 and 7050 alloy
116
0.5 30
102 102
32
0.4 150
34
210
EC (% IACS)
da/dt (mm/h)
0.3
36
˃1446
38
0.2
˃1446 40
0.1 Crack growth
42 velocity
Crack growth
0 44 velocity
T6 455 425 405 370 T7
TF/Q (oC) Electrical
conductivity
Figure 7.6: Summary of effect of heat treatment of 7075 alloy on electrical

conductivity and crack growth velocity at 3 MPa√m. Numbers in red are the time (h)
for stress intensity to decrease to 3 MPa√m (corresponding to a crack length of ≈ 69
mm from Figure 5.9)
0.3 30
150 186 32
0.25
EC (% IACS)
279 34
0.2
da/dt (mm/h)
36
327
0.15
38
Crack growth
0.1 ˃1446 velocity
40
1178
0.05 42 Crack growth
˃1446 velocity
0 44
T6 455 425 405 370 T7 T74 Electrical
Conductivity
TF/Q (oC)
Figure 7.7: Summary of effect of heat treatment of 7050 alloy on electrical

conductivity and crack growth velocity at 3 MPa√m. Numbers in red are the time (h)
for stress intensity to decrease to 3 MPa√m (corresponding to a crack length of ≈ 69
mm from Figure 5.9)
117
7.5 Grain boundary precipitate versus SCC resistance
From Figure 6.20 (a) and 6.21 (a) small, discontinuous grain boundary precipitates in
T6 can be related to poor corrosion resistance while the large grain boundary
precipitates in T7 temper (Figure 6.20 (f) and 6.21 (f)) correlates with high SCC
resistance obtained in both alloys. Figures 6.20 (b-e) and 6.21 (b-e) show that grain
boundary precipitates gradually increased in size as TF/Q decreased during HTPP
while Figure 7.5 shows that as TF/Q decreased, crack length decreased in both alloys.
Summary of V-K plot of both alloys shown in Figures 6.12 and 6.13 show that HTPP
treatment causes decrease in the plateau velocity as TF/Q decrease. TF/Q = 370 oC
showed the best resistance to SCC of all the HTPP conditions tested. Results shown in
Figures 6.12, 6.13, 7.5, 7.6 and 7.7 correspond to increase in size and discontinuity of
grain boundary precipitates observed in Figure 6.21 and 6.22. These results correlate
with studies by Li et al. (2008) that shows that HTPP can achieve higher SCC
resistance [29]. In terms of the size of the grain boundary precipitates, studies have
shown that large grain boundary precipitates can serve as nucleation site for hydrogen
bubbles thereby reducing SCC by hydrogen embrittlement. Also, large grain boundary
precipitates reduce the effect of SCC by anodic dissolution [77].
The gradual increase in SCC resistance as TF/Q decreases can also be related to
increase in copper concentration of grain boundary precipitates. This is supported by
EDS analysis in Figures 6.22 and 6.23 showing that as TF/Q decreases, there is decrease in
copper solute segregated at the grain boundary. The increase in the potential of the
grain boundary precipitate reduces SCC through anodic dissolution. The increase in
homogeneity and uniformity of solute concentration at the grain boundaries as TF/Q
118
decreases can also improve SCC resistance by reducing the formation of local
galvanic cells that might cause SCC.
7.6 Effect of HTPP on microstructure
TEM analysis of the unaged samples in Figure 6.18 and 6.19 shows that dislocations
were present in the unaged samples after quenching. These can be identified as
quenched-in dislocations formed due to internal stress generated during quenching. It
appears that there is decrease in dislocation density as TF/Q decreases. This shows that
HTPP heat treatment can reduce the dislocation density in 7075 and 7050 alloys.
Some preferential heterogeneous precipitation occurred at the grain boundary region
in all the HTPP conditions observed due to prior slow cooling before quenching. TEM
analysis in Figure 6.20 relates the morphology of grain boundary precipitates in HTPP
treated conditions to standard T6 and T7 tempers of 7075 alloy. As shown in Figure
6.20 (a). The morphology of precipitates in the grain boundary region of T6 shows
high concentration of small precipitates that are continuously distributed along the
grain boundary. From Figure 6.20 (b)-(e) it is evident that the initial precipitation
during quenching enabled more precipitation to occur at the grain boundary region
after aging. This is evident from the increase in size of grain boundary precipitates as
TF/Q temperature decreases from TF/Q = 455 to 370 oC. The gradual increase in
precipitate size agrees with the literature [26, 28]. This can be explained by increase
in precipitation at the grain boundary due to prior pre-precipitation during slow
cooling from SHT to a lower (TF/Q) temperature. Figure 6.20 (f) shows the coarse
precipitates that are discontinuously distributed along the grain boundary precipitate
morphology in T7 temper. The increase in size of the precipitates is due to overaging
treatment. Coarse discontinuous grain boundary precipitates are observed at TF/Q = 370
119
o
C and T7 temper. Large discontinuous grain boundary precipitates has been related to
high SCC resistance of T7 temper [40]. Similar result was observed in 7050 alloy as
shown in Figure 6.21.
By comparison to unaged condition shown in Figure 6.18 and 6.19, it appears that
subsequent aging after quenching of HTPP treated samples reduces the dislocation
density. Thus, this results show that the TF/Q temperature used in HTPP treatment
plays an important role in increasing the size of grain boundary precipitates and
decreasing dislocation density.
Using Energy Dispersive X-ray Spectrometry (EDS) analysis, concentration of solute
elements segregated across grain boundary was analysed. Figure 6.22 and 6.23 show
the results obtained from 7075 and 7050 alloy respectively. It is evident that decrease
in TF/Q temperature causes increases homogeneity in the distribution of Zn, Mg and
Cu across the grain boundary. This can be related to increase and uniformity in the
diffusion of Zn, Mg and Cu into grain boundary precipitates. This trend is similar to
results reported by Hepples et al. shown in Figure 4.8 [62]. Figure 7.8 shows that
there is decrease in the amount of copper segregated in the HTPP treated samples as
TF/Q decreases. This means increase in Cu concentration in the grain boundary
precipitates. This result corresponds with the literature that HTPP can increase in Cu
content at the grain boundary precipitates [26, 28]. Hepples et al. showed that copper
segregated at grain boundary decreased in T7 and RRA compared to T6 [62].
In terms of Mg content, it appears that the amount of Mg segregated is higher in the
HTPP treated conditions compared to T6. This correlates with literature on grain
boundary segregation of Mg in 7150 alloy by Hepples et al. [62]. Although some
studies show that, the presence of Mg can be related to SCC by hydrogen
120
embrittlement, this result confirms that Mg segregation may not be the dominant
factor for SCC in these alloys [62, 64, 65].
12
10
Composition (wt%)
8 T6
TF/Q= 455 oC
455
6 TF/Q= 425 oC
425
4 405
TF/Q= 405 oC
370
TF/Q= 370 oC
2 T7
0
-15 -10 -5 0 5 10 15
(a)
12
10
Composition (wt%)
8
T6
6 TF/Q= 455 oC
455
TF/Q= 425 oC
425
4
TF/Q= 405 oC
405
2 TF/Q= 370 oC
370
T7
0
-15 -10 -5 0 5 10 15
(b)
Figure 7.8: Summary of grain boundary copper concentration in (a) 7075 and (b) 7050
alloy
121
CHAPTER EIGHT
CONCLUSIONS
This research has studied HTPP as a potential heat treatment approach to achieve a
combination of high strength and corrosion resistance in 7075 and 7050 commercial
alloys. This was achieved by using experimental procedure that involved electrical
conductivity measurement, hardness measurement, exfoliation corrosion testing,
stress corrosion cracking testing and analysis of grain boundary using TEM. The
following conclusions can be made based on the results obtained from the
experiments in this research:
• The intermediate temperature (TF/Q) used during HTPP has a significant effect
on the properties of both alloys after HTPP heat treatment.
• Both alloys exhibit a decrease in hardness as the T F/Q temperature decreased
especially at TF/Q= 435 oC. However, 7050 can be heat treated to higher
hardness than 7075 alloy. Zr addition in 7050 reduces the quench sensitivity
during HTPP heat treatment.
• HTPP heat treatment achieves increase in SCC resistance as the TF/Q
temperature decreased.
• Electrical conductivity varies directly with SCC resistance in both alloys. EC
can thus be used to determine SCC resistance in 7050 and 7075 HTPP treated
alloys.
• HTPP causes homogeneity of solute distribution at the grain boundary. Also,
there is increase in discontinuity, size, and Cu concentration of grain boundary
122
precipitates as TF/Q decreases. Hence, increase in SCC resistance of HTPP
treated samples can be attributed to a combination of these factors.
• None of the HTPP treated conditions achieved a good combination of strength
and SCC resistance as standard T6 and T7 temper respectively. However, the
range of TF/Q temperatures between 425 and 405 oC provides the best balance
in strength and SCC resistance.
8.1 Recommendations for future work
Based on the results obtained in this research and some of the challenges experienced,
the following recommendations are suggested for future work:
 The cause of stepwise changes observed in the hardness and EC results should
be further investigated.
 The effect of multistep aging process in HTPP on the properties of 7050 and
7075 alloys should be investigated.
 To obtain sufficient data for V-K plot of HTPP treated samples, SCC test with
slower rate is suggested using fatigue pre-cracked samples and test solution of
3.5% NaCl.
123
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133
APPENDIX
Appendix A: Double beam sample
134
APPENDIX B: TEMPERATURE MEASUREMENT DURING SCC TESTING
[78]
Date Temperature (oC) Date Temperature (oC)

30-08-2013 22 01-10-2013 13
31-08-2013 22 02-10-2013 13
01-09-2013 22 03-10-2013 13
02-09-2013 22 04-10-2013 13
03-09-2013 21 05-10-2013 13
04-09-2013 21 06-10-2013 13
05-09-2013 21 07-10-2013 13
06-09-2013 21 08-10-2013 12
07-09-2013 20 09-10-2013 12
08-09-2013 20 10-10-2013 11
09-09-2013 20 11-10-2013 11
10-09-2013 19 12-10-2013 10
11-09-2013 19 13-10-2013 10
12-09-2013 19 14-10-2013 9
13-09-2013 19 15-10-2013 9
14-09-2013 18 16-10-2013 9
15-09-2013 18 17-10-2013 8
16-09-2013 18 18-10-2013 8
17-09-2013 17 19-10-2013 8
18-09-2013 17 20-10-2013 7
19-09-2013 17 21-10-2013 7
20-09-2013 16 22-10-2013 7
21-09-2013 16 23-10-2013 6
22-09-2013 16 24-10-2013 6
23-09-2013 16 25-10-2013 6
24-09-2013 15
25-09-2013 15
26-09-2013 14
27-09-2013 14
28-09-2013 14
29-09-2013 13
30-09-2013 13
135
APPENDIX C: SCC DATA
Table 1: Data for crack length vs time for 7075 alloy
Time (h) 7075-T6 7075 7075 7075 7075 7075-T7

TF/Q = TF/Q = TF/Q = TF/Q =
455 oC 425 oC 405 oC 370 oC
0 17.75 18.13 15.88 18.00 16.48 16.00
30 54.50 52.25 42.75 35.00 16.93 16.50
78 71.50 68.00 54.00 42.00 17.08 16.75
126 112.75 95.75 64.75 50.50 17.13 16.80
174 115.00 115.05 75.78 57.00 18.25 16.83
198 115.45 115.10 85.00 60.00 19.25 16.83
222 115.50 115.15 95.38 64.25 21.00 16.85
257 116.00 115.23 98.40 69.55 22.50 16.85
302 116.35 116.15 105.68 84.75 24.50 17.40
353 116.40 116.25 115.23 90.75 26.00 17.75
526 116.45 116.33 115.75 98.15 28.75 18.00
746 116.50 116.50 116.13 114.00 32.00 21.50
842 114.38 32.75 22.15
986 114.75 34.50 22.50
1178 115.13 35.38 23.00
1346 115.50 37.25 23.50
Table 2: Data for crack length vs time for 7050 alloy
Time (h) 7050- 7050 7050 7050 7050 7050- 7050

T6 TF/Q = TF/Q = TF/Q = TF/Q = T7 T74
455 oC 425 oC 405 oC 370 oC
0 15.93 17.63 18.38 15.37 17.70 15.83 12.75
30 44.70 45.27 42.60 35.67 34.07 16.60 13.40
78 53.03 53.50 49.10 42.00 39.40 17.00 13.47
126 63.28 60.27 54.72 45.67 42.07 17.32 13.50
174 72.20 72.17 58.93 51.33 45.57 17.73 13.52
198 75.53 74.67 61.35 53.17 50.07 18.07 13.53
222 80.20 76.67 64.02 54.25 51.15 18.53 13.55
257 87.083 85.27 69.18 57.75 55.90 18.72 13.82
302 97.77 87.20 72.77 59.75 56.98 18.80 13.86
353 105.53 88.82 76.68 64.08 57.57 20.00 13.87
526 116.00 100.35 87.93 71.08 58.57 21.18 13.88
746 116.50 114.53 99.77 76.58 59.73 22.47 13.89
842 114.82 101.13 79.92 61.07 22.75 13.95
986 115.12 103.13 81.58 62.48 23.27 14.06
1178 115.38 107.33 86.33 63.40 23.67
1346 115.52 109.13 90.83 64.32 24.30
136
Table 3: 7075-T6 sample
Time ao ao Ave. da/dt Co Vo K Kave

(h) (mm) (mm) ao (mm) (mm/h) (mm) (mm) (MPa√ m) (MPa√ m)
0 17.50 18.00 17.75 9.00 0.35 24.18
30 53.50 55.50 54.50 1.230 4.04 14.11
78 71.00 72.00 71.50 0.350 2.49 3.27
126 113.00 112.50 112.75 0.850 1.08 1.79
174 115.00 115.00 115.00 0.047 1.04 1.06
198 115.50 115.40 115.45 0.019 1.03 1.04
222 115.50 115.50 115.50 0.002 1.03 1.03
257 116.00 116.00 116.00 0.014 1.02 1.03
302 116.20 116.50 116.35 0.008 1.02 1.02
353 116.30 116.50 116.40 0.001 1.02 1.02
526 116.40 116.50 116.45 0.0002 1.02 1.02
746 116.50 116.50 116.50 0.0002 1.01 1.01
Table 4: 7075-T7 sample

0 17.00 15.00 16.00 9.00 0.34 27.12
30 17.00 16.00 16.50 0.017 26.00 26.56
78 17.00 16.50 16.75 0.005 25.47 25.74
126 17.00 16.60 16.80 0.001 25.36 25.42
174 17.00 16.65 16.83 0.000 25.31 25.34
198 17.00 16.66 16.83 0.000 25.30 25.31
222 17.00 16.70 16.85 0.000 25.26 25.29
257 17.00 16.80 16.90 0.001 25.16 25.21
302 18.00 16.80 17.40 0.011 24.16 24.66
353 18.50 17.00 17.75 0.006 23.49 23.82
526 19.00 17.00 18.00 0.001 23.03 23.26
746 22.00 21.00 21.50 0.015 17.82 20.43
842 22.30 22.00 22.15 0.007 17.05 17.43
986 22.50 22.50 22.50 0.002 16.65 16.86
1178 23.00 23.00 23.00 0.003 16.11 16.38
1346 23.00 24.00 23.50 0.003 15.60 15.86
137
Table 5: 7075-HTPP at TF/Q = 455 oC sample 1

0 20.00 20.50 20.25 9.00 0.4 22.89
30 53.50 53.50 53.50 1.108 4.77 13.83
78 68.00 69.00 68.50 0.313 3.08 3.93
126 113.50 115.50 114.50 0.958 1.20 2.14
174 116.00 116.00 116.00 0.031 1.17 1.19
198 116.00 116.10 116.05 0.002 1.17 1.17
222 116.00 116.20 116.1 0.002 1.17 1.17
257 116.00 116.30 116.15 0.001 1.17 1.17
302 116.10 116.5 116.3 0.003 1.16 1.16
353 116.20 116.5 116.35 0.001 1.16 1.16
526 116.30 116.5 116.4 0.000 1.16 1.16
746 116.50 116.5 116.5 0.000 1.16 1.16

0 16.50 15.50 16.00 9.00 0.30 23.93
30 50.00 52.00 51.00 1.167 3.89 13.91
78 68.50 66.50 67.50 0.344 2.37 3.13
126 77.00 77.00 77.00 0.198 1.87 2.12
174 114.10 114.10 114.10 0.773 0.90 1.39
198 114.10 114.20 114.15 0.002 0.90 0.90
222 114.20 114.20 114.20 0.002 0.90 0.90
257 114.30 114.30 114.30 0.003 0.90 0.90
302 116.00 116.00 116.00 0.038 0.88 0.89
353 116.20 116.10 116.15 0.003 0.87 0.88
526 116.30 116.20 116.25 0.001 0.87 0.88
746 116.50 116.50 116.5 0.001 0.87 0.87
138

(h) (mm) (mm) ao (mm) (mm/h) (mm) (mm) (MPa√m) (MPa√m)
0 15.50 16.50 16.00 9.00 0.30 23.93
30 49.00 49.00 49.00 1.100 4.17 14.05
78 61.00 61.00 61.00 0.250 2.84 3.50
126 73.50 72.50 73.00 0.250 2.06 2.45
174 86.80 87.00 86.90 0.290 1.50 1.78
198 103.00 103.00 103.00 0.671 1.09 1.30
222 115.50 116.00 115.75 0.531 0.88 0.99
257 115.60 116.00 115.80 0.001 0.88 0.88
302 115.70 116.00 115.85 0.001 0.88 0.88
353 116.00 115.90 115.95 0.002 0.88 0.88
526 116.00 116.00 116.00 0.000 0.88 0.88
746 116.00 116.50 116.25 0.001 0.87 0.87

0 15.50 16.00 15.75 9.00 0.30 24.45
30 35.00 38.00 36.50 0.692 6.86 15.65
78 46.00 48.00 47.00 0.219 4.48 5.67
126 55.50 57.50 56.50 0.198 3.25 3.87
174 62.00 67.30 64.65 0.170 2.56 2.91
198 66.00 68.00 67.00 0.098 2.40 2.48
222 75.00 75.00 75.00 0.333 1.96 2.18
257 81.00 81.00 81.00 0.171 1.70 1.83
302 94.00 97.00 95.50 0.322 1.26 1.48
353 115.0 114.0 114.50 0.373 0.90 1.08
526 0
116.0 0
115.0 115.50 0.006 0.88 0.89
746 0
116.0 116.0 116.00 0.002 0.88 0.88
0 0
139

0 18.50 19.00 18.75 9.00 0.38 24.29
30 37.00 38.00 37.50 0.625 6.18 15.24
78 39.00 40.00 39.50 0.042 5.73 5.96
126 45.50 46.50 46.00 0.135 4.56 5.15
174 52.80 51.50 52.15 0.128 3.76 4.16
198 55.00 55.00 55.00 0.119 3.46 3.61
222 59.00 59.00 59.00 0.167 3.09 3.28
257 59.10 59.10 59.10 0.003 3.09 3.09
302 78.00 81.00 79.50 0.453 1.90 2.49
353 83.50 83.50 83.50 0.078 1.74 1.82
526 83.50 83.60 83.55 0.000 1.74 1.74
746 113.00 113.00 113.00 0.134 1.03 1.39
842 113.50 113.50 113.50 0.005 1.03 1.03
986 114.00 114.00 114.00 0.003 1.02 1.02
1178 114.50 114.50 114.50 0.003 1.01 1.01
1346 115.00 115.00 115.00 0.003 1.00 1.01
Time (h) ao ao Ave. da/dt Co Vo K Kave

(mm) (mm) ao (mm) (mm/h) (mm) (mm) (MPa√m (MPa√m
) )
0 17.50 17.00 17.25 9.00 0.34 24.45
30 33.00 32.00 32.50 0.508 9.39 16.92
78 46.00 43.00 44.50 0.250 5.57 7.48
126 55.00 55.00 55.00 0.219 3.86 4.72
174 63.2 60.50 61.85 0.143 3.14 3.50
198 64.00 66.00 65.00 0.131 2.87 3.01
222 70.00 69.00 69.50 0.188 2.55 2.71
257 80.00 80.00 80.00 0.300 1.98 2.26
302 90.00 90.00 90.00 0.222 1.59 1.78
353 98.00 98.00 98.00 0.157 1.36 1.48
526 113.0 112.5 112.7 0.085 1.05 1.20
746 0
115.0 0
115.0 5
115.0 0.010 1.01 1.03
842 0
115.0 0
115.5 0
115.2 0.003 1.01 1.01
986 0
115.5 0
115.5 5
115.5 0.002 1.00 1.00
1178 116.0 0
115.5 0
115.7 0.001 1.00 1.00
1346 0
116.0 0
116.0 5
116.0 0.001 0.99 1.00
0 0 0
140

0 17.00 16.60 16.80 10.00 0.36 26.86
30 17.00 16.70 16.85 0.002 26.75 26.80
78 17.00 16.90 16.95 0.002 26.53 26.64
126 17.00 17.00 17.00 0.001 26.42 26.47
174 19.00 19.00 19.00 0.042 22.58 24.50
198 20.00 20.00 20.00 0.042 20.97 21.78
222 23.00 23.00 23.00 0.125 17.06 19.02
257 25.00 25.00 25.00 0.057 15.03 16.05
302 27.00 27.00 27.00 0.044 13.35 14.19
353 28.00 28.00 28.00 0.020 12.61 12.98
526 33.00 32.00 32.50 0.025 9.95 11.65
746 33.00 34.00 33.50 0.005 9.47 9.71
842 34.00 35.00 34.50 0.010 9.03 9.25
986 37.00 37.00 37.00 0.017 8.04 8.53
1178 38.00 38.00 38.00 0.005 7.70 7.87
1346 40.00 43.00 41.50 0.021 6.64 7.17
1446 44.50 45.00 44.75 0.033 5.84 6.24

0 16.30 16.00 16.15 9.00 0.36 28.35
30 17.50 16.50 17.00 0.028 26.42 27.39
78 17.50 16.90 17.20 0.004 25.99 26.21
126 17.50 17.00 17.25 0.001 25.89 25.94
174 17.50 17.50 17.50 0.006 25.37 25.63
198 18.50 18.50 18.50 0.042 23.46 24.42
222 19.00 19.00 19.00 0.021 22.58 23.02
257 20.00 20.00 20.00 0.029 20.97 21.78
302 22.00 22.00 22.00 0.044 18.23 19.60
353 24.00 24.00 24.00 0.039 16.00 17.12
526 26.00 24.00 25.00 0.013 15.03 16.63
746 30.00 31.00 30.50 0.025 11.02 13.02
842 31.00 31.00 31.00 0.005 10.73 10.87
986 32.00 32.00 32.00 0.007 10.20 10.46
1178 32.50 33.00 32.75 0.004 9.82 10.01
1346 33.00 33.00 33.00 0.001 9.82 9.82
1446 40.00 41.00 40.50 0.075 6.92 8.37
141
Table 13: 7050-T6 sample 1

0 21.20 19.70 20.45 9.7 0.4 22.56
30 46.30 45.30 45.80 0.845 6.24 14.40
78 54.30 54.30 54.30 0.177 4.65 5.44
126 65.80 65.80 65.80 0.240 3.31 3.98
174 74.30 76.30 75.30 0.198 2.59 2.95
198 80.30 79.30 79.80 0.188 2.33 2.46
222 86.30 85.30 85.80 0.250 2.04 2.19
257 102.30 102.30 102.30 0.471 1.48 1.76
302 114.30 114.30 114.30 0.267 1.20 1.34
353 115.30 115.30 115.30 0.020 1.18 1.19
526 116.00 116.00 116.00 0.004 1.17 1.18
746 116.50 116.50 116.50 0.002 1.16 1.16

0 14.70 13.00 13.85 9.50 0.25 24.18
30 44.50 45.50 45.00 1.038 4.02 14.10
78 52.50 54.50 53.50 0.177 2.98 3.50
126 62.00 63.50 62.75 0.193 2.25 2.62
174 72.00 70.50 71.25 0.177 1.79 2.02
198 75.00 74.50 74.75 0.146 1.64 1.72
222 77.5 77.50 77.50 0.115 1.54 1.59
257 82.50 80.50 81.50 0.114 1.40 1.47
302 94.50 95.00 94.75 0.294 1.06 1.23
353 113.00 113.00 113.00 0.358 0.77 0.92
526 116 116.00 116.00 0.017 0.73 0.75
746 116.50 116.50 116.50 0.002 0.72 0.73
142

0 13.50 13.50 13.50 8.70 0.25 25.00
30 43.30 43.30 43.30 0.993 4.29 14.65
78 51.30 51.30 51.30 0.167 3.21 3.76
126 59.80 62.80 61.30 0.208 2.35 2.78
174 69.30 70.80 70.05 0.182 1.85 2.10
198 70.80 73.30 72.05 0.083 1.76 1.80
222 77.30 77.30 77.30 0.219 1.55 1.65
257 77.30 77.60 77.45 0.004 1.54 1.54
302 84.50 84.00 84.25 0.151 1.32 1.43
353 88.30 88.30 88.30 0.079 1.21 1.27
526 116.00 116.00 116.00 0.160 0.73 0.97
746 116.50 116.50 116.50 0.002 0.72 0.73

(h) (mm) (mm) ao (mm/h) (mm) (mm) (MPa√m) (MPa√m)
(mm)
0 13.00 12.00 12.50 10.00 0.25 27.59
30 14.00 13.00 13.50 0.033 25.00 26.29
78 14.00 13.50 13.75 0.005 24.41 24.71
126 14.00 14.00 14.00 0.005 23.84 24.134
174 14.00 14.20 14.10 0.002 23.62 23.73
198 14.00 14.30 14.15 0.002 23.51 23.57
222 14.00 14.40 14.20 0.002 23.40 23.46
257 14.00 14.50 14.25 0.001 23.30 23.35
302 14.20 14.50 14.35 0.002 23.08 23.19
526 18.00 16.00 17.00 0.011 18.35 20.71
746 17.30 17.30 17.30 0.001 17.91 18.13
842 17.50 17.50 17.50 0.002 17.62 17.76
986 18.00 18.00 18.00 0.003 16.94 17.28
1178 18.50 18.50 18.50 0.003 16.29 16.61
1346 19.30 19.30 19.30 0.005 15.33 15.81
143

0 15.30 11.70 13.50 9.70 0.27 27.00
30 15.30 12.30 13.80 0.010 26.24 26.62
78 15.30 12.70 14.00 0.004 25.75 26.00
126 15.30 13.30 14.30 0.006 25.04 25.40
174 15.30 14.70 15.00 0.015 23.50 24.27
198 15.30 15.30 15.30 0.013 22.89 23.19
222 15.30 15.70 15.50 0.008 22.49 22.69
257 15.30 16.30 15.80 0.009 21.91 22.20
302 15.30 16.50 15.90 0.002 21.72 21.82
526 22.30 18.30 20.30 0.020 15.39 18.56
746 25.30 22.30 23.80 0.016 12.15 13.77
842 25.50 22.50 24.00 0.002 12.00 12.08
986 26.30 23.00 24.65 0.005 11.52 11.76
1178 27.00 23.00 25.00 0.001 11.28 11.40
1346 23.30 27.30 25.30 0.002 11.07 11.17

0 24.00 19.00 21.50 9.70 0.5 26.20
30 25.00 20.00 22.50 0.033 24.49 25.35
78 25.50 21.00 23.25 0.016 23.31 23.90
126 26.00 21.30 23.65 0.008 22.72 23.02
174 26.20 22.00 24.10 0.009 22.08 22.40
198 26.50 23.00 24.75 0.027 21.20 21.64
222 26.80 25.00 25.90 0.048 19.77 20.49
257 27.00 25.20 26.10 0.006 19.54 19.66
302 27.10 25.20 26.15 0.001 19.48 19.51
526 27.20 25.30 26.25 0.000 19.37 19.43
746 27.30 25.30 26.30 0.000 19.31 19.34
842 27.50 26.00 26.75 0.005 18.81 19.06
986 28.00 26.30 27.15 0.003 18.38 18.60
1178 28.00 27.00 27.50 0.002 18.02 18.20
1346 28.30 28.30 28.30 0.005 17.22 17.62
144

0 16.00 12.00 14.00 9.00 0.25 23.84
30 51.00 51.00 51.00 1.233 3.24 13.54
78 62.00 59.00 60.50 0.198 2.40 2.82
126 72.00 71.50 71.75 0.234 1.77 2.09
174 81.00 80.00 80.50 0.182 1.44 1.60
198 85.00 84.00 84.50 0.167 1.31 1.38
222 89.00 88.00 88.50 0.167 1.21 1.26
257 112.00 112.00 112.00 0.671 0.78 0.99
302 113.10 113.00 113.05 0.023 0.77 0.77
353 113.30 113.00 113.15 0.002 0.77 0.77
526 115.50 116.00 115.75 0.015 0.73 0.75
746 116.00 116.20 116.10 0.002 0.73 0.73
842 116.00 116.40 116.20 0.001 0.73 0.73
986 116.30 116.40 116.35 0.001 0.73 0.73
1178 116.40 116.4 116.40 0.000 0.73 0.73
1346 116.50 116.40 116.45 0.000 0.73 0.73

0 23.00 23.00 23.00 9.00 0.50 23.70
30 46.00 47.00 46.50 0.783 7.60 15.65
78 54.00 53.00 53.50 0.146 5.96 6.78
126 57.00 54.50 55.75 0.047 5.55 5.76
174 73.00 70.00 71.50 0.328 3.56 4.55
198 73.00 73.00 73.00 0.063 3.43 3.50
222 74.00 74.00 74.00 0.042 3.35 3.39
257 75.00 74.00 74.50 0.014 3.31 3.33
302 76.00 74.00 75.00 0.011 3.27 3.29
353 79.00 79.00 79.00 0.078 2.97 3.12
526 96.00 96.00 96.00 0.098 2.08 2.53
746 114.00 113.00 113.50 0.080 1.52 1.80
842 114.00 113.50 113.75 0.003 1.52 1.52
986 114.50 114.00 114.25 0.003 1.50 1.51
1178 115.00 114.50 114.705 0.003 1.49 1.50
1346 115.00 115.00 115.00 0.001 1.48 1.49
145

0 15.50 16.30 15.90 9.70 0.30 24.14
30 38.30 38.30 38.30 0.747 6.33 15.23
78 45.30 47.70 46.50 0.171 4.56 5.45
126 51.8 54.80 53.30 0.142 3.60 4.08
174 64.00 65.00 64.50 0.233 2.57 3.09
198 65.00 68.00 66.50 0.083 2.43 2.50
222 68.00 67.00 67.50 0.042 2.37 2.40
257 69.30 69.30 69.30 0.051 2.26 2.32
302 73.80 73.3 73.55 0.094 2.03 2.15
353 74.30 74.30 74.30 0.015 1.99 2.01
526 89.30 89.30 89.30 0.087 1.43 1.71
746 114.00 114.00 114.00 0.112 0.91 1.17
842 114.50 114.50 114.50 0.005 0.89 0.90
986 115.00 114.50 114.75 0.002 0.89 0.89
1178 115.00 115.00 115.00 0.001 0.89 0.89
1346 115.00 115.20 115.10 0.001 0.89 0.89

0 16.00 15.50 15.75 9.00 0.30 24.45
30 43.00 43.00 43.00 0.908 5.21 14.83
78 50.00 51.00 50.50 0.156 3.96 4.58
126 57.50 57.70 57.60 0.148 3.14 3.55
174 63.00 61.00 62.00 0.092 2.76 2.95
198 65.00 64.00 64.50 0.104 2.57 2.67
222 66.00 66.50 66.25 0.073 2.45 2.51
257 74.00 74.00 74.00 0.221 2.01 2.23
302 75.00 75.00 75.00 0.022 1.96 1.98
353 79.00 79.00 79.00 0.078 1.78 1.87
526 83.00 83.00 83.00 0.023 1.63 1.71
746 112.00 112.00 112.00 0.132 0.94 1.28
842 112.00 112.50 112.25 0.003 0.93 0.93
986 113.00 113.00 113.00 0.005 0.92 0.93
1178 114.00 114.00 114.00 0.005 0.91 0.91
1346 114.50 114.50 114.50 0.003 0.90 0.90
1446 115.00 115.00 115.00 0.005 0.89 0.89
146

0 21.00 22.00 21.50 10.00 0.48 25.15
30 44.00 45.00 44.50 0.767 7.87 16.51
78 49.00 49.00 49.00 0.094 6.67 7.27
126 53.00 54.50 53.75 0.099 5.68 6.17
174 57.00 58.00 57.50 0.078 5.04 5.36
198 58.50 61.00 59.75 0.094 4.71 4.88
222 61.00 65.00 63.00 0.135 4.29 4.5
257 68.5 67.00 67.75 0.136 3.77 4.03
302 75.00 74.00 74.50 0.15 3.17 3.47
353 81.00 79.50 80.25 0.113 2.77 2.97
526 86.00 88.00 87.00 0.039 2.39 2.58
746 91.00 92.00 91.50 0.020 2.18 2.29
842 95.00 94.00 94.50 0.031 2.05 2.12
986 99.00 99.00 99.00 0.031 1.88 1.97
1178 110.00 110.00 110.00 0.057 1.55 1.72
1346 115.00 114.00 114.50 0.027 1.44 1.49
1446 115.00 115.00 115.00 0.005 1.43 1.43

0 18.20 17.60 17.90 9.00 0.35 23.90
30 39.80 40.80 40.30 0.747 6.78 15.34
78 47.80 47.80 47.80 0.156 5.07 5.93
126 52.30 53.30 52.80 0.104 4.27 4.67
174 57.30 57.30 57.30 0.094 3.70 3.99
198 59.80 59.80 59.80 0.104 3.43 3.57
222 62.80 62.80 62.80 0.125 3.15 3.29
257 65.80 65.80 65.80 0.086 2.89 3.02
302 68.80 68.80 68.80 0.067 2.67 2.78
353 70.80 70.80 70.80 0.039 2.54 2.61
526 93.80 93.80 93.80 0.133 1.52 2.03
746 95.80 95.8 95.80 0.009 1.46 1.49
842 96.50 96.80 96.65 0.009 1.44 1.45
986 97.00 97.80 97.40 0.005 1.42 1.43
1178 98.00 98.00 98.00 0.003 1.40 1.41
1346 98.00 98.80 98.40 0.002 1.46 1.43
1446 103.60 103.60 103.60 0.052 1.44 1.45
147

0 14.00 14.50 14.25 9.00 0.25 23.30
30 38.00 39.00 38.50 0.808 5.23 14.26
78 44.00 45.00 44.50 0.125 4.10 4.66
126 47.50 48.50 48.00 0.073 3.60 3.85
174 54.50 54.50 54.50 0.135 2.89 3.24
198 57.00 57.00 57.00 0.104 2.67 2.78
222 58.00 58.00 58.00 0.042 2.59 2.63
257 62.00 62.00 62.00 0.114 2.30 2.44
302 63.00 63.00 63.00 0.022 2.23 2.27
353 68.00 68.00 68.00 0.098 1.95 2.09
526 80.00 77.00 78.50 0.061 1.50 1.73
746 84.00 81.00 82.50 0.018 1.37 1.44
842 89.00 87.00 88.00 0.057 1.22 1.30
986 90.00 89.00 89.50 0.010 1.183 1.20
1178 95.00 95.00 95.00 0.029 1.06 1.12
1346 101.0 101.00 101.0 0.03571 0.95 1.00
1446 0
104.0 104.00 0
104.0 4
0.03 0.90 0.92
0 0

0 15.20 19.50 17.35 9.50 0.35 24.97
30 33.50 34.5 34.00 0.555 13.53 19.25
78 40.50 40.5 40.50 0.135 9.54 11.54
126 45.00 45.00 45.00 0.094 7.73 8.63
174 50.50 50.50 50.50 0.115 6.13 6.93
198 51.50 51.50 51.50 0.042 5.90 6.02
222 53.50 53.50 53.50 0.083 5.47 5.68
257 57.50 57.00 57.25 0.107 4.77 5.11
302 60.50 60.00 60.25 0.067 4.31 4.54
353 64.50 64.00 64.21 0.078 3.79 4.05
526 70.00 69.50 69.75 0.032 3.26 3.50
746 76.50 76.00 76.25 0.030 2.69 2.95
842 76.50 77.00 76.75 0.005 2.66 2.67
986 79.00 78.50 78.75 0.014 2.52 2.59
1178 85.00 85.00 85.00 0.033 2.17 2.34
1346 89.00 89.50 89.25 0.025 1.96 2.06
1446 93.40 93.40 93.40 0.042 1.79 1.88
148

0 13.00 16.00 14.50 9.00 0.27 24.59
30 34.00 35.00 34.50 0.667 6.77 15.68
78 41.00 41.00 41.00 0.135 5.08 5.93
126 44.00 44.00 44.00 0.063 4.51 4.80
174 49.00 49.00 49.00 0.104 3.75 4.13
198 51.00 51.00 51.00 0.083 3.50 3.63
222 51.00 51.50 51.25 0.010 3.47 3.49
257 54.00 54.00 54.00 0.079 3.17 3.32
302 56.00 56.00 56.00 0.044 2.97 3.07
353 60.00 60.00 60.00 0.078 2.63 2.81
526 65.00 65.00 65.00 0.029 2.28 2.46
746 71.00 71.00 71.00 0.027 1.95 2.12
842 75.00 75.00 75.00 0.042 1.76 1.86
986 77.00 76.00 76.50 0.010 1.70 1.73
1178 79.00 79.00 79.00 0.013 1.61 1.65
1346 82.00 82.50 82.25 0.019 1.49 1.55
1446 90.00 90.00 90.00 0.078 1.26 1.37

0 19.00 19.00 19.00 9.50 0.40 25.09
30 35.50 35.50 35.50 0.550 6.98 16.03
78 40.50 39.50 40.00 0.094 5.87 6.42
126 45.00 45.00 45.00 0.104 4.92 5.39
174 48.00 48.00 48.00 0.063 4.46 4.69
198 51.50 52.50 52.00 0.167 3.94 4.20
222 51.50 53.00 52.25 0.010 3.91 3.93
257 55.50 55.50 55.50 0.093 3.56 3.74
302 57.00 57.50 57.25 0.039 3.39 3.48
353 58.00 58.50 58.25 0.020 3.30 3.34
526 59.00 59.00 59.00 0.004 3.23 3.26
746 60.00 60.00 60.00 0.005 3.15 3.19
842 62.00 61.00 61.50 0.016 3.02 3.08
986 62.50 62.00 62.25 0.006 2.96 2.99
1178 63.00 63.00 63.00 0.004 2.91 2.94
1346 63.50 63.50 63.50 0.003 2.87 2.89
1446 68.80 68.80 68.80 0.053 2.52 2.70
149

0 15.00 20.00 17.50 8.50 0.35 24.67
30 34.50 35.50 35.00 0.583 8.57 16.62
78 38.50 40.50 39.50 0.094 7.01 7.79
126 40.50 41.50 41.00 0.0313 6.59 6.80
174 44.50 43.50 44.00 0.063 5.85 6.22
198 49.50 49.50 49.50 0.229 4.78 5.31
222 51.00 51.00 51.00 0.063 4.54 4.66
257 57.50 57.50 57.50 0.186 3.68 4.11
302 58.50 58.50 58.50 0.022 3.57 3.62
353 59.00 58.50 58.75 0.005 3.54 3.55
526 59.00 59.00 59.00 0.001 3.51 3.53
746 60.00 60.00 60.00 0.005 3.41 3.46
842 61.00 61.00 61.00 0.010 3.31 3.36
986 62.00 62.00 62.00 0.007 3.22 3.27
1178 63.00 63.00 63.00 0.005 3.13 3.17
1346 63.50 63.00 63.25 0.001 3.11 3.12
1446 68.70 68.70 68.70 0.055 2.68 2.89

0 16.00 17.20 16.60 9.80 0.33 25.03
30 31.20 32.20 31.70 0.503 9.49 17.26
78 38.20 39.20 38.70 0.146 6.84 8.17
126 40.20 40.20 40.20 0.031 6.42 6.63
174 45.20 44.20 44.70 0.094 5.37 5.89
198 48.20 49.20 48.70 0.167 4.63 5.00
222 50.20 50.20 50.20 0.063 4.40 4.52
257 54.20 55.20 54.70 0.129 3.79 4.09
302 54.20 56.20 55.20 0.011 3.73 3.76
353 55.20 56.20 55.70 0.010 3.67 3.70
526 57.20 58.20 57.70 0.012 3.45 3.56
746 59.20 59.20 59.20 0.007 3.29 3.37
842 60.20 61.20 60.70 0.016 3.15 3.22
986 63.20 63.20 63.20 0.017 2.93 3.04
1178 64.20 64.20 64.20 0.005 2.85 2.89
1346 66.20 66.20 66.20 0.012 2.70 2.78
1446 70.20 70.20 70.20 0.040 2.43 2.56
150
Table 31: 7050 T74-1

0 11.80 12.30 12.05 9.70 0.25 28.89
30 12.20 12.80 12.50 0.015 27.59 28.24
78 12.20 13.10 12.65 0.003 27.17 27.38
126 12.20 13.20 12.70 0.001 27.04 27.11
174 12.30 13.20 12.75 0.001 26.90 26.97
198 12.30 13.30 12.80 0.002 26.77 26.84
222 12.30 13.35 12.83 0.001 26.70 26.74
257 13.00 13.30 13.15 0.009 25.86 26.28
302 13.25 13.30 13.28 0.003 25.55 25.71
353 13.30 13.30 13.30 0.000 25.49 25.52
526 13.30 13.40 13.35 0.000 25.36 25.43
746 13.30 13.45 13.375 0.000 25.30 25.33
842 13.40 13.50 13.45 0.001 25.12 25.21
986 13.50 13.50 13.50 0.000 25.00 25.06
Table 32: 7050 T74-2

0 14.50 14.70 14.60 9.30 0.30 27.07
30 14.70 15.50 15.10 0.017 25.88 26.48
78 14.70 15.60 15.15 0.001 25.77 25.83
126 14.70 15.70 15.20 0.001 25.65 25.72
174 14.70 15.70 15.20 0 25.65 25.65
198 14.70 15.70 15.20 0 25.65 25.65
222 14.70 15.70 15.20 0 25.65 25.65
257 15.70 15.70 15.70 0.014 24.56 25.12
302 15.70 15.70 15.70 0 24.56 24.56
353 15.70 15.70 15.70 0 24.56 24.56
526 15.70 15.70 15.70 0 24.56 24.56
746 15.70 15.70 15.70 0 24.56 24.56
842 16.00 16.00 15.70 0 23.93 24.24
986 16.00 16.00 16.00 0.002 23.93 23.93
151

0 11.60 11.60 11.60 9.40 0.24 29.07
30 12.60 12.60 12.60 0.033 26.22 27.65
78 12.60 12.60 12.60 0 26.22 26.22
126 12.60 12.60 12.60 0 26.22 26.22
174 12.60 12.60 12.60 0 26.22 26.22
198 12.60 12.60 12.60 0 26.22 26.22
222 12.60 12.60 12.60 0 26.22 26.22
257 12.60 12.60 12.60 0 26.22 26.22
302 12.60 12.60 12.60 0 26.22 26.22
353 12.60 12.60 12.60 0 26.22 26.22
526 12.60 12.60 12.60 0 26.22 26.22
746 12.60 12.6 12.60 0 26.22 26.22
842 12.80 12.60 12.70 0.001 25.96 26.09
986 12.80 12.60 12.70 0 25.96 25.96
152
APPENDIX D: EDS ANALYSIS DATA
Table 1: 7075-T6
Distance from grain Zn Mg Cu

boundary (nm) (wt%) (wt%) (wt%)
Point 1
10 0 0 9.22
5 0 2.48 7.37
0 0 2.58 6.69
-5 9.99 4.17 0
-10 0 3.19 6.25
Point 2
10 0 0 7.05
5 0 3.46 6.48
0 0 0 6.65
-5 0 0 9.18
-10 5.45 0 8.43
Table 2: 7075-T7

Point 1
10 1.31 0 5.3
5 0 0 5.54
0 2.45 0 7.38
-5 0 0 6.59
-10 1.44 0 5.49
Point 2
10 3.25 0 5.27
5 4.25 0 5.45
0 3.54 2.18 5.84
-5 4.54 1.99 6.48
-10 4.5 1.92 5.9
153
Table 3: 7075-HTPP at TF/Q = 455 oC

Point 1
10 0 0 7.64
5 0 0 5.42
0 0 0 7.24
-5 0 0 7.49
-10 3.45 0 6
Point 2
10 0 3.62 6.41
5 0 0 6.69
0 0 0 6.11
-5 0 0 6.52
-10 0 0 7.63

Point 1
10 6.97 0 5.72
5 4.73 0 4.81
0 5.46 3.3 6.31
-5 14.8 0 8.21
-10 14.75 3.93 6.36
Point 2
10 5.46 2.97 7.38
5 3.92 2.67 7.78
0 4.13 2.53 6.15
-5 5.89 2.65 5.77
-10 5.35 0 5.81
154

Point 1
10 3.83 3.17 5.75
5 6.23 3.05 5.76
0 12.72 2.86 5.27
-5 9.79 3.24 6.52
-10 6.17 0 3.85
Point 2
10 5.4 4.3 4.64
5 10.69 0 5.29
0 9.39 0 5.29
-5 7.11 0 5.87
-10 6.75 4.25 5.67

Point 1
10 3.71 2.29 3.47
5 3.8 2.66 3.79
0 3.08 3.31 3.24
-5 2.65 2.5 3.44
-10 2.15 2.82 3.35
Point 2
10 2.91 2.34 4.03
5 2.72 2.87 3.34
0 3.24 3.3 3.74
-5 8.22 3.4 3.93
-10 4.6 3.42 4.08
155
Table 7: 7050-T6

Point 1
10 6.94 0 5.73
5 4.57 0 5.82
0 3.34 0 5.83
-5 0 0 7.26
-10 0 0 7.3
Point 2
10 8.56 0 5.14
5 6.74 0 7.25
0 0 0 0
-5 6.6 0 6.09
-10 0 0 7.89
Table 8: 7050-T7

Point 1
10 1.94 2.22 3.3
5 1.32 2.82 3.94
0 0 2.03 2.61
-5 1.18 2.38 3.64
-10 0 2.49 3.69
Point 2
10 1.98 2.5 3.45
5 1.5 2 3.2
0 0.97 1.76 3.12
-5 1.19 1.58 3.33
-10 1.91 2.56 3.86
156

Point 1
10 6.62 0 5.82
5 0 3.68 6.87
0 0 0 7.33
-5 3.19 2.31 6.74
-10 0 0 7.47
Point 2
10 4.47 0 7.6
5 5.13 0 6.53
0 0 0 6.53
-5 5.97 0 7.02
-10 6.73 2.91 6.76

Point 1
10 2.14 4.71 4.19
5 1.29 3.8 5.34
0 10.04 0 5.74
-5 3.7 4.19 5.87
-10 5.85 3.47 5.7
Point 2
10 3.01 3.12 5.53
5 2.67 4.16 4.71
0 6.04 3.61 6.13
-5 3.62 0 6.82
-10 4.9 3.7 4.53
157

Point 1
10 9.53 0 4.03
5 7.33 0 3.77
0 9.58 0 3.41
-5 4.89 0 3.83
-10 4.54 2.67 3.73
Point 2
10 5.72 0 3.59
5 5.18 2.99 3.79
0 4.27 2.65 4.49
-5 5.43 0 3.71
-10 4.95 0 4.36

Point 1
10 1.98 0 4.91
5 2.21 3.01 4.58
0 2.66 0 4.96
-5 1.7 0 5.03
-10 2.15 0 4.95
Point 2
10 1.41 2.02 3.99
5 1.82 0 3.43
0 2.43 0 3.61
-5 1.69 2.57 3.37
-10 2.1 0 3.47
158

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RESPONSE OF 7075 AND 7050 ALUMINIUM ALLOYS TO HIGH

TEMPERATURE PRE-PRECIPITATION HEAT TREATMENT

OLAYINKA BLESSING TEHINSE

A Thesis submitted to the Faculty of Graduate Studies of

The University of Manitoba

in partial fulfilment of the requirements of the degree of

Department of Mechanical Engineering

Copyright © 2014 by Olayinka Blessing Tehinse

It is difficult to obtain a combination of optimal strength and stress corrosion cracking

boundary precipitate morphology is to introduce a controlled cooling procedure

referred to as High Temperature Pre-precipitation (HTPP) treatment following the

properties of commercial Al-Zn-Mg-Cu alloys using different intermediate

electrical conductivity, corrosion resistance, TEM analysis of grain boundary

precipitation aged to a higher hardness compared to 7075; this result is associated

electrical conductivity and corrosion resistance superior to standard T6 and T7X

The financial supports of Natural Science and Engineering Research Council of

Canada, Faculty of Graduate studies and Faculty of Engineering, University of

Manitoba on this research are highly appreciated. I am grateful to Mike Boswick,

are highly appreciated. I am thankful to my friends/colleagues: Dr. Oshoba, Dr. Ola,

help and guidance. I am thankful to my roommates Bolanle Akinwumi and Victoria

God for His unconditional love, mercy and grace.

LIST OF TABLES .....................................................................................................vii

LIST OF FIGURES ..................................................................................................viii

LIST OF COPYRIGHTED MATERIAL FOR WHICH PERMISSION WAS

CHAPTER ONE: INTRODUCTION ........................................................................ 1

1.1 Historical development of Al-Zn-Mg-Cu alloys for airframe structures ........ 1

1.2 Motivation and Objectives of this Thesis Research ...................................... 10

CHAPTER TWO: Al-Zn-Mg-Cu ALLOYS............................................................ 12

2.1 Alloying elements ......................................................................................... 12

2.3 Precipitation hardening in 7xxx alloys .......................................................... 16

2.4 Introduction to physical metallurgy of 7xxx alloys ...................................... 19

2.5 Mechanism of precipitation hardening in 7xxx alloys .................................. 21

2.6 Important microstructural features ................................................................ 22

2.6.1 Quench sensitivity.................................................................................. 25

2.6.2 Electrical conductivity ........................................................................... 28

CHAPTER THREE: LOCALISED CORROSION IN Al-Zn-Mg-Cu

3.1 Intergranular Corrosion ................................................................................. 30

3.3 Stress Corrosion Cracking............................................................................. 32

3.3.1 Mechanism of Stress Corrosion Cracking ............................................. 33

3.4 Effect of slip character on SCC in Al-Zn-Mg-Cu alloys .............................. 35

3.5 Influence of grain boundary precipitate structure on SCC ............................ 37

3.6 Influence of magnesium and copper content................................................. 38

3.7 Crack initiation versus propagation and damage tolerance design

CHAPTER FOUR: EFFECT OF HEAT TREATMENT ON SCC RESISTANCE

OF Al-Zn-Mg-Cu ALLOYS ...................................................................................... 42

4.1 Overaging ...................................................................................................... 42

4.2 Retrogression and reaging ............................................................................. 43

4.3 High Temperature Pre-precipitation heat treatment ...................................... 46

4.4 Effect of heat treatment on grain boundary segregation…………………… 50

CHAPTER FIVE: EXPERIMENTAL PROCEDURE .......................................... 52

5.1 Experimental materials .................................................................................. 52

5.2 Heat treatment procedure .............................................................................. 52

5.3 Electrical conductivity testing ....................................................................... 57

5.4 Hardness testing ............................................................................................ 58

5.5 Corrosion tests ............................................................................................... 59

5.5.1 Exfoliation corrosion testing .................................................................. 59

5.5.2 Stress corrosion test (Double beam test) ................................................ 61

CHAPTER SIX: EXPERIMENTAL RESULTS .................................................... 67

6.1 Electrical conductivity results ....................................................................... 67