DOKUZ EYLÜL UNIVERSITY

GRADUATE SCHOOL OF NATURAL AND APPLIED SCIENCES

T6 HEAT TREATMENT
OPTIMIZATION OF A356 ALLOY

by
Alper GÜNEREN

July, 2019
İZMİR
 T6 HEAT TREATMENT
OPTIMIZATION OF A356 ALLOY

A Thesis Submitted to the

Graduate School of Natural and Applied Sciences of Dokuz Eylül University
In Partial Fulfillment of the Requirements for the Degree of Master of Science in
Metallurgical and Materials Engineering

by
Alper GÜNEREN

July, 2019
İZMİR
 ACKNOWLEDGMENT

First and foremost, I would like to thank my advisor Dr. Esra DOKUMACI for
her support, patience and scientific guidance throughout the course of this thesis.

I would like to owe my special thanks to H. Emre ÇUBUKLUSU for his support
and providing useful suggestions about this thesis. I would like to express my
gratitude to Caner KALENDER and Bora YAY for their friendship and helps. I
would also like thank each person who work in CMS Jant ve Makina Sanayi A.Ş.
R&D and Foundry Departments.

Finally and deeply, I would like to thank my mother Filiz GÜNEREN, my father
Sabri GÜNEREN and my brother Berkay GÜNEREN for believing in me and
supporting me throughout my graduate career.

Alper GÜNEREN

iii
 T6 HEAT TREATMENT OPTIMIZATION OF A356 ALLOY

ABSTRACT

In this study, the effect of heat treatment stages on the yield-ultimate tensile
strength, the hardness and the elongation of the wheels produced by low-pressure
die-casting technology using Sr-modified A356 alloy, is examined. The study
consists of fundamentally four steps as follow; investigation of the effect of current
heat treatment stages and dye process, the effect of the solution treatment on the
eutectic silicon morphology and the mechanical properties, determination of the main
factors affecting the mechanical properties through the design of experiment and
optimizing the conditions, and the effect of the quenching phase on the cooling rate
and the mechanical properties. The experiments were carried out with temperature
controlled laboratory furnaces. Tensile and hardness testing was applied to the
specimen taken on the wheel and microstructure analyzes were performed by using
an optical microscope. As a result of the study, it was determined that 480°C is not
sufficient to provide a supersaturated solution for catalyzing the precipitation
hardening and the elongation values can be enhanced through the proper
spherodization of the eutectic silicons. Solution treatment has no effect on yield-
ultimate tensile strength and hardness by oneself. Whereas it was determined that
values vary considerably when the same aging or painting process applied after
different solution treatments. According to design of experiment and regression
analysis, the formulas were obtained based on solution temperature, solution time,
artificial aging temperature, and artificial aging time. Optimal heat treatment
parameters were determined for desired mechanical properties. Cooling rates and
Leidenfrost points were obtained at different quenching mediums.

Keywords: A356 alloy, wheel, T6 heat treatment, optimization, quenching

iv
 A356 ALAŞIMI T6 ISIL İŞLEMİ OPTİMİZASYONU

ÖZ

Bu çalışmada, Sr-modifiyeli A356 alüminyum alaşımı kullanılarak alçak basınçlı

döküm teknolojisi ile üretilen jantlarda, ısıl işlem aşamalarının akma-çekme
mukavemeti, sertlik ve uzama değerleri üzerindeki etkisi incelenmiştir. Çalışma
temel olarak; mevcut ısıl işlem aşamalarının ve boya prosesinin etkisinin
incelenmesi, çözeltiye alma işleminin ötektik silisyum morfolojisi ve mekanik
özellikler üzerindeki etkisinin incelenmesi, deney tasarımı yöntemi ile mekanik
özellikleri etkileyen ana faktörlerin belirlenmesi ve şartların optimize edilmesi, su
verme aşamasının mekanik özellikler ve soğuma hızı üzerindeki etkisinin
incelenmesi olarak dört ana bölümden oluşmaktadır. Deneyler sıcaklık kontrollü
laboratuvar tipi fırınlarda gerçekleştirilmiştir. Jant üzerinden alınan numunelere
çekme ve sertlik testi uygulanmış, optik mikroskop ile mikroyapı analizleri
yapılmıştır. Çalışma sonucunda aşırı doymuş katı özelti oluşturmak için 480°C’de
çözeltiye alma işleminin yetersiz olduğu, uygun çözeltiye alma işleminin ötektik
silisyumların küreselleşmesiyle uzama değerlerini önemli ölçüde arttırdığı, ancak
akma ve sertlik değerlerini tek başına etkilemediği anlaşılmıştır. Bunun yanı sıra,
farklı çözeltiye alma ve suni yaşlandırma kombinasyonlarında akma ve sertlik
değerlerinde önemli değişkenlikler gözlemlenmiştir. Deney tasarımı ve regresyon
analizine göre, çözeltiye alma sıcaklığı, çözeltiye alma süresi, suni yaşlandırma
sıcaklığı ve suni yaşlandırma süresine bağlı formulasyonlar oluşturulmuştur ve
istenilen mekanik özelliklere göre optimum şartlar belirlenmiştir. Farklı su verme
ortamlarında yapılan deneyler sonucunda soğuma hızları ve Leidenfrost noktaları
elde edilmiştir.

Anahtar Kelimeler. A356 alaşımı, jant, T6 ısıl işlemi, optimizasyon, su verme

v
CONTENTS

Page

M.Sc THESIS EXAMINATION RESULT FORM ..................................................... ii

ACKNOWLEDGMENT ............................................................................................. iii
ABSTRACT ................................................................................................................ iv
ÖZ ................................................................................................................................ v
LIST OF FIGURES .................................................................................................... ix
LIST OF TABLES .................................................................................................... xiii

CHAPTER ONE - INTRODUCTION ..................................................................... 1

CHAPTER TWO - ALUMINIUM ALLOYS .......................................................... 3

2.1 Clasification of Aluminium Alloys .................................................................... 3

2.1.1 Designation of Aluminium Alloys .............................................................. 4

2.1.2 Al-Si-Mg Foundry Alloys ........................................................................... 7

2.1.2.1 Modification of Eutectic Silicon ........................................................ 10

2.1.2.2 Grain Refinement ............................................................................... 13

2.2 Production of Light Alloy Wheel ..................................................................... 15

2.2.1 Moulding ................................................................................................... 15

2.2.2 Melting and Degassing.............................................................................. 15

2.2.3 Low Pressure Die Casting ......................................................................... 16

2.2.4 Heat Treatment .......................................................................................... 17

2.2.5 Machining ................................................................................................. 17

2.2.6 Painting ..................................................................................................... 18

2.2.7 Quality Control ......................................................................................... 18

vi
CHAPTER THREE - HEAT TREATMENT ........................................................ 20

3.1 Heat Treatment of Aluminium Alloys .............................................................. 20

3.2 T6 Heat Treatment ............................................................................................ 20

3.2.1 Solution Treatment .................................................................................... 23

3.2.2 Quenching ................................................................................................. 26

3.2.2.1 Cooling Mediums and Quenchants .................................................... 30

3.2.2.2 Distortion and Residual Stress Problems ........................................... 34

3.2.3 Artificial Aging ......................................................................................... 36

3.3 Recent Researches on T6 Heat Treatment........................................................ 40

3.4 Surfactants ........................................................................................................ 45

CHAPTER FOUR - EXPERIMENTAL STUDIES .............................................. 46

4.1 Study of Current Situation ................................................................................ 46

4.2 Design of Experiment (DOE) and Heat Treatment Experiments ..................... 46

4.3 Mechanical Testing .......................................................................................... 51

4.3.1 Tensile Testing .......................................................................................... 51

4.3.2 Hardness Test ............................................................................................ 52

4.4 Microstructure Analysis ................................................................................... 52

CHAPTER FIVE - EXPERIMENTAL RESULTS AND DISCUSSION ........... 53

5.1 Tensile Testing Results .................................................................................... 53

5.1.1 Tensile Testing Results of Current Situation ............................................ 53

5.1.2 Tensile Testing Results of Solution Treatment Experiments .................... 55

vii
 5.1.3 Tensile Testing Results Of Optimization Experiments ............................. 62

5.1.3.1 Statistical Analysis of Yield Strength Results ................................... 63

5.1.3.2 Statistical Analysis of Elongation Results ......................................... 65

5.1.4 Tensile Testing Results of Quenching Experiments ................................. 67

5.2 Hardness Test Results ...................................................................................... 70

5.2.1 Hardness Test Results of Current Situation .............................................. 70

5.2.2 Hardness Test Results of Solution Treatment Experiments ...................... 71

5.2.3 Hardness Test Results of Optimization Experiments................................ 73

5.2.4 Hardness Test Results of Quenching Experiments ................................... 76

5.3 Microstructure Analysis Results ...................................................................... 77

CHAPTER SIX - CONCLUSION .......................................................................... 85

REFERENCES ......................................................................................................... 89

viii
LIST OF FIGURES

Page

Figure 2.1 Al–Si binary phase diagram ...................................................................... 7

Figure 2.2 (a) Microstructure of hypoeutectic alloy (b) eutectic alloy (c)
hypereutectic alloy .................................................................................... 8

Figure 2.3 Phase diagram of Al–Mg2Si pseudobinary section .................................. 9

Figure 2.4 Degree of eutectic silicon modification (a) Level 1, unmodified structure
200X (b) 800X(c) Level 2, lamellar structure 200X (d) 800X (e) Level 3,
partial modification 200X (f) 800X. ....................................................... 11

Figure 2.5 (g) Level 4, absence of lamellar structure 200X (h) 800X (i) Level 5,
fibrous silicon eutectic 200X (j) 800X (k) Level 6, very fine structure.
200X (l) 800X. ........................................................................................ 12

Figure 2.6 (a) Non-modified eutectic silicon (b) Spherical eutectic silicon after heat
treatment .................................................................................................. 13

Figure 2.7 Grain refinement effect (a) No grain refiner, coarse grains. (b) fine grains
................................................................................................................. 14

Figure 2.8 Schematically low pressure die casting working prencipe...................... 16

Figure 2.9 Machining process steps.......................................................................... 18

Figure 3.1 T6 heat treatment stages .......................................................................... 20

Figure 3.2 Chematic phase diagram for solution treatment and artificially aging
zones ........................................................................................................ 22

Figure 3.3 Microstructures of AlSi7Mg (Alloy 356.0). Light microscope

micrographs; etched with 1% HF (a) As-cast modified, 150X (b) As-cast
modified, 750X (c) After heat treatment (T6), 150X (d) After heat
treatment (T6), 750X ............................................................................... 22

Figure 3.4 Pseudo-binary phase system of AlSiMg0.3 and Pseudo-binary phase

system of AlSi7Mg.................................................................................. 24

ix
Figure 3.5 Effect of the percentage of the eutectic Si particles and the size of SDAS
on solution treatment time ....................................................................... 24

Figure 3.6 Solution treatment effects on hardness after aging process .................... 25

Figure 3.7 Quenching stages..................................................................................... 26

Figure 3.8 Heat transition phases and relation between surface, steam and fluid. ... 27

Figure 3.9 Wetting process during the quenching .................................................... 28

Figure 3.10 Cooling rate of (1) 65°C (2) 53°C (3) 41°C and (4) 19°C water medium
................................................................................................................. 29

Figure 3.11 Illustration of the surface cooling mechanism of (a) water-quenched and
(b) polymer quenchant ............................................................................ 31

Figure 3.12 Quenching severity coeffi cients H of typical quenchants ..................... 32

Figure 3.13 Cooling rate comparasion between PAG and oil .................................... 33

Figure 3.14 Cooling rate comparasion between different polymer quenchants and oil.
................................................................................................................. 34

Figure 3.15 Illustration of the mechanism of T6 heat treatment and precipitation

hardening ................................................................................................. 36

Figure 3.16 Hardness and Yield Strength curve for A356.0 aluinium alloy with
DTAT and STAT with 150°C and 180 °C ............................................. 37

Figure 3.17 GP Zones formation and overaging ........................................................ 38

Figure 3.18 Hardness curves at different aging temperature and overaging.............. 38

Figure 3.19 Modified and unmodified A356 alloy hardness comparison at different
aging parameters ..................................................................................... 39

Figure 3.20 Transition stage with (a) Polymer quenchant (b) Polymer quenchant with
surfactant additive ................................................................................... 44

Figure 4.1 Termocupl placed into the wheel .............................................................. 50

Figure 4.2 Area number of obtained testing specimen .............................................. 51

Figure 4.3 Tensile test specimen dimensions ............................................................. 52

x
Figure 5.1 YS (Rp) and UTS (Rm) results after different heat treatment procedures.
................................................................................................................. 53

Figure 5.2 ε% (A28) results results after different heat treatment procedures .......... 54

Figure 5.3 YS (Rp) values after solution treatment experiments ............................... 57

Figure 5.4 UTS (Rm) values after solution treatment experiments ........................... 59

Figure 5.5 ε% (A28) values after solution treatment experiments ............................. 61

Figure 5.6 Main effects screener for yield strength ................................................... 63

Figure 5.7 Interaction plots for yield strength ............................................................ 64

Figure 5.8 Prediction report and five alternative parameters for yield strength
(Target 155MPa) ..................................................................................... 64

Figure 5.9 Main effect screener for elongation .......................................................... 65

Figure 5.10 Interaction plots for elongation ............................................................... 66

Figure 5.11 Prediction report and five alternative parameters for elongation (Target
4.5 ε%) .................................................................................................... 66

Figure 5.12 Cooling behavior at different qunech mediums...................................... 68

Figure 5.13 Cooling rate at different quench mediums.............................................. 69

Figure 5.14 HB results at different heat treatment stages .......................................... 70

Figure 5.15 HB values of solution treatment experiments ......................................... 72

Figure 5.16 Main effect screener for hardness ........................................................... 74

Figure 5.17 Interaction plots for hardness.................................................................. 75

Figure 5.18 Prediction report and five alternative parameters for hardness (Target
75HB) ...................................................................................................... 75

Figure 5.19 HB values of quenching experiments ..................................................... 76

Figure 5.20 Microstructures of as-cast (a)200X, (b)500X and T6 heat treated

(c)200X, (d)500X samples ...................................................................... 77

Figure 5.21 Microstructures of solution treated parts at 510°C at 200X and 500X for
(a)(b)80 min, (c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min . 78

xi
Figure 5.22 Microstructures of solution treated parts at 520°C at 200X and 500X for
(a)(b)80 min, (c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min .79

Figure 5.23 Microstructures of solution treated parts at 530°C at 200X and 500X for
(a)(b)80 min, (c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min . 80

Figure 5.24 Microstructures of solution treated parts at 540°C at 200X and 500X for
(a)(b)80 min, (c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min . 81

Figure 5.25 Microstructures of solution treated parts at 550°C at 200X and 500X for
(a)(b)80 min, (c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min . 82

Figure 5.26 Fe-intermetallics in the microstructure of solution treated part at 530°C83

Figure 5.27 Microstructure of the Sr-modified A356 alloy samples after (a) 510°C for
80 min and (b) 510°C for 280 min solution treatment. ........................... 84

Figure 6.1 Optimization plot for (a) target elongation, (b) maximum elongation ..... 86

xii
LIST OF TABLES
Page

Table 2.1 Wrought aluminum alloy designation system ............................................. 4

Table 2.2 Cast aluminium alloy designation system ................................................... 5

Table 2.3 Basic temper designations ........................................................................... 6

Table 2.4 Temper system for aluminium alloys .......................................................... 6

Table 2.5 Composition of A356.0 aluminium alloy .................................................... 8

Table 2.6 GFR values of elements ............................................................................. 14

Table 3.1 ASTM standard for A356 aluminum alloy T6 heat treatment ................... 21

Table 3.2 Comparison of several commonly used quenchants in cooling rate and
distortion ................................................................................................... 35

Table 4.1 Design of solution treatment experiments ................................................. 48

Table 4.2 Design of optimization experiments .......................................................... 49

Table 4.3 Design of quenching experiments ............................................................. 50

Table 5.1 YS (Rp) values after solution treatment experiments ................................ 56

Table 5.2 UTS (Rm) values after solution treatment experiments ............................ 58

Table 5.3 ε% (A28) values after solution treatment experiments.............................. 60

Table 5.4 YS (Rp), UTS (Rm) and ε% (A28) values of optimization experiments .. 62

Table 5.5 YS (Rp), UTS (Rm), ε% (A28) values of quenching experiments ........... 67

Table 5.6 Hardness(HB) values of solution treatment experiments .......................... 71

Table 5.7 Hardness(HB) values of optimization experiments ................................... 73

Table 5.8 Hardness(HB) values of quenching experiments ...................................... 76

xiii
 CHAPTER ONE
INTRODUCTION

Aluminum is an important element which exists on earth in different

mineralogical forms such as Al2O3, corundum, bauxites, or bonded with silica and
alumina-silicates (Lumley, 2011; Totten & MacKenzie, 2003). The metallurgical
process is quite difficult due to its affinity to oxygen and the tendency of forming the
oxide layer. Metallic aluminium is produced with using Bayer and Hall-Heroult
processes consecutively.

For the last decades, its usage ratio in the industrial area only behind ferrous
alloys.The extensive use of Aluminium lies in its strength, density ratio, toughness,
low melting degree, good formability, weldability, high heat and electrical
conductivity and its corrosion resistance (Ahmad, 2012; Kvačkaj & Bidulský, 2011).
In these days, to decrease energy comsumption, otomotive industry need to alleviate
car’s weight. At the same time low weight critical safety components must provide
the technical requirements. Light aluminium alloy wheels are one of the major
cosmetic parts of the vehicles and these parts have to meet high impact and fatigue
requirements (Manente & Timelli, 2011).

Aluminium-Magnesium-Silicon alloys are the most demanded and widely used

casting alloys in wheel industry (Manente & Timelli, 2011; Ma, 2006) because of
their excellent fludity, high mechanical properties and lightness (Abdulwahab,
Madugu, Yaro, Hassan & Popoola, 2011). However, without any heat treatment,
these alloys are used in the as-cast condition because they exhibit deficient
elongation (toughness) due to the coarse acicular plates eutectic silicons. This phases
increases internal stress under an applied load (Paz, 2003; Ji-hua, Xiao-long, Jian-
ting & De-ying, 2011). Modifying the microstructure and enhancing the properties of
alloy, is only possible by applying such specific heat treatment after the casting
process.

1
 T6 heat treatment is widely applied in the wheel industry and stages of the process
are; solution treatment, quenching, and artificial aging (Brooks, 1991). Altough T6 is
an important process to enhance mechanical properties; high temperature (540°C)
that using in solution treatment in order to attain homogeneous microstructure, and
(180°C) in aging for enhancing mechanical properties with precipitation, increases
natural gas and electricity consumption. Optimization of the amount of heat and time
of the process is important for energy saving because solution treatment and artificial
aging stages cause approximately 25% of natural gas consumption of the company.
In quenching stage, wheels immersed in a cooling medium from high temperature to
room temperature. Cooling should be fast enough to obtain supersaturated solid
solution. Contrarily, cooling should be slow enough to refrain distortions and
extensive residual stresses. Determination of the critical cooling rate is essential
because of this conflict. Although many investigations examined the quenching
phenomenon, only few references in the literature systematically describe the effect
of cooling mediums for A356 aluminium alloy.

Tos um up, excess energy consumption and the distortion problems are the main
disadvantages of wheel heat treatment process. Purpose of this study is optimizing
the T6 heat treatment parameters. The findings of this thesis will use to determine the
heat treatment conditions of the company in future.

In this study, the effect of heat treatment stages on the yield-ultimate tensile
strength, the hardness and the elongation of the wheels produced by low-pressure
die-casting technology using Sr-modified A356 alloy, is examined. The study
consists of fundamentally four steps as follow; investigation of the effect of current
heat treatment stages and dye process, the effect of the solution treatment on the
eutectic silicon morphology and the mechanical properties, determination of the main
factors affecting the mechanical properties through the design of experiment and
optimizing the conditions, and the effect of the quenching phase on the cooling rate
and the mechanical properties.

2
 CHAPTER TWO
ALUMINIUM ALLOYS

In non-alloyed state, pure aluminium is a comparatively soft material with a yield

strength of 34.5 MPa, a tensile strength of 90 MPa and density of approximately 2.7
gr/cm3 (Sheasby & Pinner, 2001).

To generate different type of aluminium alloys, Silicon (Si), Magnesium (Mg),

Copper (Cu), Zinc (Zn), Manganese (Mn), and Nickel (Ni) are used. All of these
elements are added into the pure aluminium to enhance the mechanical properties.
Adding Cu and Mg makes the alloy heat treatable by means of precipitation
hardening mechanism.

2.1 Clasification of Aluminium Alloys

Aluminium alloys are classified by means of their production process, the heat
treatment ability and the chemical composition (Mazzolani, 1995). There are two
type of aluminium alloys as casting and wrought alloys. Invesment casting, semi-
solid casting, sand casting, gravity die casting, low pressure die casting (LPDC), high
pressure die casting (HPDC), squeeze casting, thixocasting are the main casting
methods. Wrought alloys are cast in ingots or billets then worked (cold or hot)
mechanically and transformed into various forms as extrusions, plate, sheet, forgings,
foil, tube and wire (Sheasby & Pinner, 2001).

3
2.1.1 Designation of Aluminium Alloys

In order to describe wrought alloys 4 digit numerical system is used as given in

Table 2.1. The first digit shows the group of alloy. The second digit indicates
modifications (from 1 to 9) of the original alloy or impurity limits. The last two
digits indicate the aluminium alloy or the aluminium purity.

Table 2.1 Wrought aluminum alloy designation system (Cayless, 1991)

Casting alloys are shown with 4 digit numerical designation as given in Table 2.2.
A modification of the original alloy or impurity limits is indicated by a serial letter
before the numerical designation (exp. A356.2, B356.0). The first digit shows the
group of alloy. The second two digits determine the alloy or indicate the aluminium
purity. The last digit that separated by a point identify the production type such as.
castings (0) or ingot (1, 2).

4
Table 2.2 Cast aluminium alloy designation system (Cayless, 1991)

Individual capital letters identifies the basic temper designations. Sub-branches of

the main process are named with extra digits. Different type of temper conditions can
be applied during heat treatment to obtain differ properties of the alloys. Basic
temper designation and systems are given below Table 2.3 and 2.4.

5
Table 2.3 Basic temper designations (Cayless, 1991)

Table 2.4 Temper system for aluminium alloys (Cayless, 1991)

6
2.1.2 Al-Si-Mg Foundry Alloys

Al-Si alloys are composed of grains (1mm-10mm), dendrites (typically 10µ -150µ
DAS), eutectic Silicons (2mm acicular shapes or 1 µm round particles),
intermetallics and inclusions. Hard Si particles improve the wear resistance of
aluminium alloys (Ernst, 2004).

In terms of the amount of atomic percentage of Si, the Al-Si casting alloys are
seperated into 3 groups as shown in Fig. 2.1 and 2.2. Alloys that include 5%-10% Si
are named Hypoeutectic alloys. Commonly, eutectic alloys contain 10%-14% Si, and
hypereutectic alloys contain 14% and 20% Si (Paz, 2003).

Figure 2.1 Al–Si binary phase diagram (Wang, Schmidt, Senz & Gösele, 2006)

7
Figure 2.2 (a) Microstructure of hypoeutectic alloy. (b) eutectic alloy. (c) hypereutectic alloy
(Warmuzek, 2004)

“Magnesium is the main solid solution strengthener to Al–Si alloy (to form Al–
Si–Mg alloys) and its addition leads to increase in response to precipitation
hardening which in turn results in higher yield strength in these alloys (Abdulwahab
et al., 2011).” Mechanism of precipation is shown in section 3.2.3 in detail.

Hypoeutectic cast A356 alloys (Al–7Si–0.3Mg) is common industry products.

Chemical composition of A356.0 is given in Table 2.5.

Table 2.5 Composition of A356.0 aluminium alloy

8
Figure 2.3 Phase diagram of Al–Mg2Si pseudobinary section (Malekan, Emamy, Rassizadehghani &
Malekan, 2012)

A356 alloys are consisted of soft primary α-Al dendrites, long acicular eutectic
silicons and hard Mg2Si which decreases the toughness and limits the usage ratio in
industry (Zhu, Jian, Yang & Zhou, 2012). Al–Mg2Si pseudo-binary diagram is
shown above as Fig. 2.3. The mechanical properties such as elongation, hardness and
yield strength depends on the microstructures of the alloys and morpholgy of silicion
particles (size, shape and distiribution) (Shabestari & Shahri, 2004). Despite the high
melting temperature (1085°C), low coefficient of thermal expansion (7.5×10-6 K-1),
low density (1.99 g/cm3), high hardness (4.5 GPa), and high elastic modulus, plate
type Mg2Si phase is not desirable phase for toughness. Besides that its presence in
the form of large blocky or Fe-based α-Chinese script shape and Fe-based β particles
significantly decreases the alloy’s mechanical properties (Mandal & Makhlouf,
2016). Heat treatment changes the form of the Mg2Si phase, fine Mg2Si particles
precipitate into the Al matrix homogeneously, therefore, mechanical properties are
enhanced.

9
 2.1.2.1 Modification of Eutectic Silicon

“Morphology of eutectic silicons are changed by the rapid solidification, the

chemical modification and the thermal modification in the solid state (Shabestari &
Shahri, 2004, p. 2023).”

First of all, the casting technique and solidification rate affect the microstructure
of casting parts. Low-pressure die casting provides rapid and directional
solidification and dendritic structure. To obtain better mechanical properties, size of
DAS (Dentrite Arm Spacing) and SDAS (Secondary Dentrite Arm Spacing) must be
reduced and eutectic silicons must be distributed homogeneously.

In order to transform the acicular shape eutectic silicon to the fibrous type,
Stronsium (Sr), Sodium (Na), Potasium(K), Calcium (Ca) and Cerium (Ce) is used as
chemical modificator. Sr and Na are commonly used for hypoeutectic alloys in
industrial application due to their modification ability. Generally, 100-300 ppm Sr is
used for modification of hypoeutectic aluminium alloys. Modified alloys show
higher yield and elongation properties comparing to unmodified alloys (Kaufman &
Roy, 2004). Finer eutectic distribution and fibrous type silicons can be obtain with
high cooling rate or chemically modifying (Ogris, 2002).

The more eutectic silicon modification, in the casting process, provides the shorter
solution treatment time and modification level than be increased easily. Modification
levels are given in Fig. 2.4 and 2.5 with range of 50 and 12.5 nm. Transformation of
the eutectic silicon, from acicular shape to spheroidal and finer shape, can be seen in
detail.

10
Figure 2.4 Degree of eutectic silicon modification. (a) Level 1, unmodified structure 200X. (b) 800X.
(c) Level 2, lamellar structure 200X. (d) 800X. (e) Level 3, partial modification 200X. (f) 800X.
(Kaufman & Roy, 2004)

11
Figure 2.5 (g) Level 4, absence of lamellar structure 200X. (h) 800X. (i) Level 5, fibrous silicon
eutectic 200X. (j) 800X. (k) Level 6, very fine structure 200X. (l) 800X. (Kaufman & Roy, 2004)

12
 Finally, the thermal modification is occurred in the heat treatment process in
solution treatment stage, already modified eutectic silicons are converted to fine fully
spherical silicon particles in soft Al matrix as shown in Fig. 2.6 (Azadi &
Shirazabad, 2012).

Figure 2.6 (a) Non-modified eutectic silicon (b) Spherical eutectic silicon after heat treatment

2.1.2.2 Grain Refinement

The grain refinement is the prior and best way in order to enhance mechanical
properties without decreasing ductility (Muszka, Majta & Bienias, 2006). A plenty of
article has been published about the grain refirenment and there have been several
studies in the literature reporting that grain size is directly related to toughness,
strength, fatigue properties alongside the ligthness of aluminium casting part (Birol,
2012a, 2012b). Reducing the grain size to the minimum, increase the wheel strength,
thus the thickness of the wheel can be decreased and extra ligthness can be obtained.

13
 During solidification grain growth must be decelerated because of the strength-
grain size relationship (Hall-petch). In order to describe ability of restriction of grain
growth, ‘GFR’ term is used. As given in Table 2.6. Titanium is the most coherent
element with aluminium structure to use as grain refiner.

Table 2.6 GFR values of elements

Ti Si Cr Ni Mg Fe Cu

GFR 246 5.9 3.5 3.3 3.0 2.9 2.8

Master alloying elements are added into liquid metal before the casting in order to
attain fine grains (Fig. 2.7). Foundry companies generally use Ti-B master alloy with
different ratio according to the spektrometer results. TiB2 and Al3Ti phases that
comprise particles must distribute into melt homogeneously.

Figure 2.7 Grain refinement effect (a) No grain refiner, coarse grains. (b) fine grains (Rooy, 1992)

Together with material properties, heat treatment conditions are also effected by
grain size. Hence, refirenment process must be carried out adequately. Otherwise,
solution treatment time might extend and spending excess time causes stepdown of
production rate and quantity. Not only treatment time but also process temperature
might be increased.

14
2.2 Production of Light Alloy Wheel

2.2.1 Moulding

Metal moulds, in other words, permanent moulds are used for producing wheel at
low pressure die casting technique. Moulds are designed by using such software as;
Catia, Unigraphics, Solidworks, Sutcast etc. and the computer aided manufacturing
system is used to produce. Mould consists of three part; upper, lower and sider core.
Cores cover with refractory based sodium silicate material in order to provide better
casting and non-wetting property. Cores have a certain lifetime, therefore,
maintenance is made periodically. Sandblasting, welding, machining and coating are
applied for preparing the mould to cast when cores damaged. Before setup to low
pressure die casting machine, the mould should be heated up to 400-500°C to avoid
casting defect.

2.2.2 Melting and Degassing

Striko furnace consists of melting and holding units. Primary aluminium ingots,
wastage wheels and aluminium scraps are loaded to the melting unit of Striko. Liquid
metal which is melted by using natural gas, are passed to holding unit. Brulor is
burned for keeping the metal temperature stable in holding unit. Secondary
aluminium scraps melted via reverberatory furnace and poured to Striko holding unit.
Metal is taken to transfer ladle and alloying elements (Stronsium, Titanium Diboride
and Magnesium) are added according to chemical analysis.

Hydrogen (H) is the solely element that soluble in aluminium metal and it has
detrimental effect on mechanical properties. Rotary degassing is carried out with an
inert gasses e.g. nitrogen or argon in order to remove the hydrogen gas.

15
Additionally, while the rotor is turning, flux is added simultaneously. Impurities,
oxides and undesirable particles are removed from liquid metal and gather the top of
the transfer ladle. These undesirable particles must be cleaned carefully otherwise
they may affect material properties of the final product.

2.2.3 Low Pressure Die Casting

Low pressure die casting (LPDC) is currently applied for producing light alloy
wheels due to the dimensional solidification, the high production rate and reduced
the finishing requirements. As illustrated in Fig. 2.8 metal is filled into a mould
cavity by passing through the riser tube by using air pressure and pressure is applied
during the solidification. Then the air pressure is reduced to zero and rest of the
molten metal turn back into the chamber. At the end of the casting process, upper and
bottom cores separate to each other and plungers push the part out. Simulation
programmes are used to determine solidification behaviour or casting defects before
production in the design period.

Figure 2.8 Schematically low pressure die casting working prencipe

16
2.2.4 Heat Treatment

Casting wheels are transferred with conveyors from casting shop to heat treatment
plant which has a solution and aging treatment furnaces. These furnaces are heated
up by using natural gas and electricity. Plant expends 24% and 8% of natural gas and
electricity of total consumption respectively. In order to attain a homogeneous
medium, hot air is circulated with fans.

Solution treatment is applied at 540°C for 240 minutes then wheels are cooled
down from 540°C to room temperature. As quench medium, water at 80°C is used.
After quenching stage, artificial aging is applied at 150°C for 180 minute. Quench
tank temperature is held stable with circulation and all parameters are controlled and
monitored by computer system.

2.2.5 Machining

Heat treated wheels are transported to machining shop. According to technical

drawing, CNC programmes are prepared depending on the chosen machining tools.
Machining of the wheels is done in three steps as illustrated in Fig. 2.9; in first
operation, hub mating surface, spoke back surface, inner flange, center hole and
inner tire contact areas are machined. Then the wheel is clamped to the chuck from
the inner flange, outer rim part and tier mating surfaces are machined. As a final
operation, lug holes are machined and chamfered as a single operation followed by
valve hole drilling. For helium leak testing, wheels are taken to bath and test is
applied. After these steps, proper wheels are sent to painting shop.

17
 Figure 2.9 Machining process steps

2.2.6 Painting

Wheels surface that comes from the machining process should be cleaned because
there might be dirt, dust or oil residues on it. Cleaning is done with using chemical
baths not only for decreasing amount of wastage but also preparing the wheel surface
to the painting process. Excess water is dried by using compressed air and painting is
carried out respectively with powder dye, powder varnish, liquid dye and liquid
varnish. Wheels are baked at painting furnace then cooled at room temperature. It is
important that, this process may cause over-aging and mechanical properties may
decrease. Temperature and time should be adjusted properly, over-aging should be
taken into account.

2.2.7 Quality Control

Products are controlled in mechanical and material laboratory as cast, heat treated
condition and painted condition. Before the first confirmation for new designs by
consumer and after a certain production time in order to ensure that sustainable
quality, quality control tests that shown below are carried out.

18
 Radial fatigue test
 Dual-axis fatigue test
 13° and 90° Impact test
 ZWARP test
 Chemical composition analysis (Spectrometer)
 Inner flange deformation test
 Micro and macrostructure analysis
 Tensile testing
 Brinell hardness test
 Charpy-impact test
 Salt-bath corrosion test

19
 CHAPTER THREE
HEAT TREATMENT

3.1 Heat Treatment of Aluminium Alloys

Heat treatment can be simply identfied as the operation of heating and cooling in
order to change the metallurgical structure, enhance the mechanical properties and
decrease the residual stresses of a metal product (Brooks, 2012). The strength of
metallic materials can often be adjusted by special heat treatments (Milkereita,
Wanderkab, Schickc & Olaf, 2012). Heat treatment of aluminium alloys is
considerably different from steel treatment. Mg and Cu is main alloying element
which makes aluminium alloy heat treatable and age hardenable.

3.2 T6 Heat Treatment

T6 heat treatment is the most common process to strength age-hardenable

aluminium alloys which comprises solution treatment, quenching, and artificial aging
(Fig. 3.1).

Figure 3.1 T6 heat treatment stages

20
 The properties that achieved with this heat treatment, depend on the combination
of the different parameters involved in the process. Fundamentally, aluminium
casting part is heated up in solid state to single phase area then quenched in any
medium to room temperature and artificially aged at relatively low temperature so as
to precipitate Mg2Si phase in aluminium matrix.

Process temperature and time depend on chemical composition, master alloying,

casting part shape, and thickness. Additionally, grain size and secondary dendritic
arm space (SDAS) are parameters which assist to designate treatment temperature
and time. As illustrated in Fig. 3.2 phase diagrams, continuously cooling
precipitation diagrams(CCP) are used in order to determine parameters. Standard
treatment conditions have determined and published by ASTM as given below Table
3.1.

ASTM has determined the temperature and time of T6 heat tratment for
parmenant mould casting and published in B917/B917M – 12.

Table 3.1 ASTM standard for A356 aluminum alloy T6 heat treatment (ASTM International, 2012)

Traditionality, these parameters are used by aluminium casting part producers

despite the fact that each casting part has different thickness and shape. Both short-
insufficient and long-redundant treatment effects production quality and quantity. As
indicated above in Table 3.1 ASTM standard does not give information about
cooling medium moreover quenching temperature. On account of these reasons,
optimal heat treatment circumstances should be evaluated and empirical studies
should be done to reach maximum or target properties with minimum energy
consumption for A356 aluminium alloy.

21
Figure 3.2 Chematic phase diagram for solution treatment and artificially aging zones (Liscic, Tensi,
Canale & Totten, 2010)

T6 heat treatment provide two advantegeous effects in A356 alloy. Elongation and
the fracture toughness values are increased by the spheroidization and globarization
of the rod shape lamellar eutectic silicons (Fig. 3.3). Likewise, yield and ultimate
tensile strength is enhanced through the formation of a large quantity of fine β’’ and
β’ precipitates in α-Al matrix. The first advantage is provided through the application
of only solution treatment and the second advantage is provided through the
application of T6 treatment completely (Azadi & Shirazabad, 2012).

Figure 3.3 Microstructures of AlSi7Mg (Alloy 356.0) Light microscope micrographs; etched with 1%
HF (a) As-cast modified, 150X (b) As-cast modified, 750X (c) After heat treatment (T6), 150X (d)
After heat treatment (T6), 750X (Warmuzek, 2004)

22
 Alongside the beneficial effects, there are two main problems in the process. One
of these problems is high amount of natural gas which is consuming in order to
obtain adequately modificated microstructure and the mechanical properties through
the solution treatment and aging stages. Excess heat may use because of insufficient
calculation or deficient experimental studies. The Second problem which is given in
section 3.2.2.2 elaborately, occurs in quenching stage after solution treatment.
Casting parts immersed quenching media and cooled down to room temperature.
Adjusting the quench rate is important to avoid dimensional changes (distortions),
micro cracks and residual stresses.

Prevention of these two main problems are quite momentous in order to save
energy, decrease amount of wastage, increase the wheel quality, enhance the
mechanical properties and the lifetime.

3.2.1 Solution Treatment

Solution treatment makes the large plate shape Mg2Si particles in the aluminum
alloy dissolved and diffuse throughout the matrix as solid solution. Supersaturated
solid solution (SSS) is obtained after this stage. Besides that, during the treatment;
homogenization of the casting microstructure occurs and the spheroidization and
coarsening of the morphology of the eutectic silicon provides (Kuntongnum,
Wisutmethangoon, Plookphol & Wannasin, 2008; Paz, 2003).

The solution treatment temperature is determined according to Pseudo-binary

phase diagrams as illustrated in Fig. 3.4 and raised nearly to a eutectic point. Possible
treatment temperature interval is marked with red dashed lines.

Besides that, chemical modification level, solidification rate and obtained

microstructure (DAS, SDAS, grain size) after the casting process affects the solution
treatment temperature and time. Effect of the percentage of the eutectic Si particles
and the size of SDAS on solution treatment time for A356 is shown in Fig. 3.5.

23
Figure 3.4 Pseudo-binary phase system of AlSiMg0.3 and Pseudo-binary phase system of AlSi7Mg

Figure 3.5 Effect of the percentage of the eutectic Si particles and the size of SDAS on solution
treatment time (Lee, 2013)

24
 The infuluence of solution treatment time on hardness after artificial aging is
shown in some researches. Paz (2003) claim that the parts solution treated for 2 hours
at 540°C, exhibit larger hardness than those treated for 4 and 6 hours as shown in
Fig. 3.6. The improved of hardness value could only be explained by forming small
vacancy clusters. Long, Chen, Liu, Li, & Li (2013) explained in their study that Mg
atoms may diffuse to the boundary of porosities during solution treatment and
amount of available solutes atoms to form Mg2Si precipitates in aging phase
decreases. Furthermore, as mentioned before diffused atoms leaves vacancies and
creates distortion at the beginning of the solution treatment. At longer treatment,
distortions (defects in matrix) are reduced and then this defects become less and less
active as nuclei to precipitate for aging treatment (Zedan, Samuel, Samuel & Doty,
2010).

On the other hand, Fracasso (2010) mentioned that high temperature of solution
treatment improves the hardness properties after ageing treatment.

Figure 3.6 Solution treatment effects on hardness after aging process (Paz, 2003)

25
3.2.2 Quenching

Quenching is a controlled cooling application after solution treatment in variable

mediums. Above the critical cooling rate, magnesium stays in the matrix as the
supersaturated solid solution(SSS) and ready to precipitate out during the aging
process (Kuntongnum et al., 2008). Quenching has basically three stages; Vapor
blanket stage (film boiling), nucleate boiling stage, and convective cooling stage
(Maniruzzaman, Fontecchio & Sisson, 2009) as shown in Fig. 3.7.

At vapor blanket stage, vapor/film blanket is composed around the surface in few
seconds. If different quenching mediums is used such as polymer, polymer film
formation is also seen on the surface. Then heat is transferred to the medium in
transition stage through this film. According to Möller, Govender & Stumpf (2010),
time of this stage determine the mechanical properties and fragmentation of film
must be homogeneous.

Leidenfrost Point

Figure 3.7 Quenching stages (Liscic et al., 2010)

26
 At the second stage (boiling or nucleate boiling), fluid starts to contact directly
with the hot surface and boiling regime developes. As illustrated in Fig. 3.8 the heat
transfer mechanism includes complex pyhsical phenomenas such as nucleation of
bubbles and growth, decomposition from the hot metal surface (Xiaoa, Wang,
Jadhavc & Li, 2010).

Figure 3.8 Heat transition phases and relation between surface, steam and fluid (Liscic, Tensi & Luty,
1992).

The transition temperature from the first phase to second phase is called the
Leidenfrost Point or Temperature (LFP). When the temperature goes down below
LFP, part begins contact directly and heat transfer increases. Non-uniform
fragmentation causes heterogeneous cooling and distortion risk increases (Alam,
2011). For example, in aluminium quenching, keeping the cooling process in the
Leidenfrost film boiling regime longer provides less distortionon the part (Huang &
Carey, 2007).

Convection stage starts if the temperature of the metal surface is goes down below
the liquid’s boiling point. The transition temperature from the boiling stage to the
convective cooling stage is depends on the boiling point of the quenchant. The metal
surface is completely wetted by the fluid therefore boiling stops at convection stage
and heat transfer occurs by direct contact between surface and liquid as shown in Fig.
3.9. The cooling rates in this stage are very low and heat removal is much slower
than in the boiling stage. Quench rate is determined by the rate of convection and the
viscosity of the quenching fluid (Sahay, Mohapatra & Totten, 2009).

27
 Figure 3.9 Wetting process during the quenching (Liscic et al., 2010)

Quench rate depends on; temperature, viscosity, surface tension, agitation rate,
additives (quenchant), vaporation heat of cooling medium, leidenfrost temperature
etc. (Huang & Carey, 2007).

Various coofficents are using to identify the quenching power such as;

 Grossmann H-value
 Heat-transfer coefficient W/(K.m2)
 Quench time
 The cooling curves to determine cooling behaviour.

Firstly, the cooling rate of water quenchant drops sharply with the increasing of
the temperature. Changing of cooling rate can be seen in Fig. 3.10 at different (19°C
to 65°C) temperatures. However, the cooling intensity of oil increases slightly with
the increase of temperature due to the decreasing of the viscosity of the oil.

28
Figure 3.10 Cooling rate of (1) 65°C (2) 53°C (3) 41°C and (4) 19°C water medium (Liscic et al.,
2010)

The higher flow rate provides better cooling. The uniformity of fluid flow around
component has great influence on distortion.

Thirdly, surface properties are important for quench rate. The smaller the surface
tension is, the less the stability of vapor film is, and the stronger the cooling
intensity. The cooling rate of rough surface is higher than smooth surface.

Finally, the larger the heat vaporization is, the stronger the cooling intensity. The
heat of vaporization of water at 100°C (212 F) is 2260 kJ/kg while the heat of
vaporization of mineral oil is about 210 kJ/kg. Therefore, the cooling intensity of
water is much more powerful than that of oil. The lower the vapor pressure is, the
more difficult the gasification, and therefore the lower the cooling intensity is
(Pan, 2002).

The cooling (quenching) rate is important for Al-Si casting alloys. especially in
interval between 200 °C and 450 °C. At these temperatures, due to the high level of
supersaturation and the diffusion rate, precipitation occurs quite rapidly. Above
450°C supersaturation is low and below 200°C diffusion rate is low for precipitation.
(Mohamed & Samuel, 2012). The critical cooling rate for AlSi7Mg0.3 alloy is

29
determined about 60 K/s in literature. Quenching with 3 K/s already significantly
suppresses precipitation during quenching. Hardness of alloy increases after aging
treatment with increasing quenching rate, due to the increasing content of
supersaturated solid solution (Milkereit, Fröck, Schick & Kessler, 2014).

3.2.2.1 Cooling Mediums and Quenchants

Water, water solutions with inorganic salt and alkali (brine), oil, aqueous polymer
solutions and different types of cooling mediums are used for immerse quenching.
Besides that, there are different type of quenching technique such as air forced,
spray, sand, fog etc. In this study immerse technique was used.

Water is widely used as traditionally quenching medium. Most important

advantages of water are cheaphness and easy usage. When bath temperature
increases, vapor phase extents, even tought the desire mechanical properties can not
obtain, distortion problems decreases. Genereally, 25°C, 65°C and 80°C waters are
commonly used for commercial quenching (Kaufman & Roy, 2004).

Salt addition in water (brine) is preferred for rapid cooling. The salt or borax
sticking to component surface can promote the burst of vapor film. Generally is
prepared with 10% NaCl or 3% NaOH. Salt crystalls accumulate on surface and then
disperse with time so vapor phase is scattered thus quench rate increases.
Disadvantage of brine is corrosion risk.

30
Figure 3.11 Illustration of the surface cooling mechanism of (a) water-quenched (Sahay, Mohapatra
& Totten, 2009) and (b) polymer quenchant (Liscic et al., 2010)

Conventional oils are espacially used for preventing distortion and crack
formation due to their low quenching rate. Burning and smoke makes the process
dangerous while decreasing the mechanical properties.

31
 Figure 3.12 Quenching severity coeffi cients H of typical quenchants

Polymer based quenchants are consist of organic polymers and water. Polymer is
reduced vapor blanket phase and provided homogeneous polymer layer on surface
that decreases heat transfer (Croucher, 2008). Constant heat regime is obtained with
this layer therefore distortion is controlled. Concentration, temperature and degree of
agitation of quenchant affect the vapor blanket stage (Liscic et al., 2010). There is no
burning and smoke problem in polymer quenchant (Pan, 2002).

Quenchant types affect the quenching severity considerably, therefore, the

selection of cooling medium becomes more of an issue. As seen in Fig. 3.12 there are
different types of quenchant with different cooling level from mild (0,2H) to good
(1,5H). While past oil quench systems have low quench rate, circulation makes the
system more effective as mentioned in section 3.2.2. Oil is accepted as the lowest
cooling medium on the other hand brine is accepted as the highest quenchant.
Property of polymer-based quenchant depends on polymer type and usage ratio.
Generally quenching severity of this type cooling medium between the oil and water,
The most commonly used quenchants are PAG, PVA, PSA, PVP, PAC, and PEOX.
Although there were many researches about time and temperature heat treatment,
few of them focused on quenching stage. So it is necessary to do deep research on
cooling medium and cooling behavior.

32
 Fig. 3.13 shows that when polymer concentration increases medium behave like
oil so cooling rate decreases. Likewise, shows the difference between hot oil (200°C)
and cold quench oil (40°C). Using brine as quenchant shortens the cooling time and
also the fastest cooling is provide at 10% brine at 24°C.

Figure 3.13 Cooling rate comparasion between PAG and oil (Liscic et al., 2010)

As shown in Fig. 3.14, while PVP and PAG have almost the same properties,
cooling rate of polyacrylate based quenchant is lower due to its polymer structure.
Similarly, variance of cooling rate with different content of oil can be seen in Fig.
3.14. Types of quenchant does not only affect the cooling rate, depends on that, it
also affect the residual stresses and behavior of distortion as given in Table 3.2.

33
Figure 3.14 Cooling rate comparasion between different polymer quenchants and oil Liscic et al.,
2010)

3.2.2.2 Distortion and Residual Stress Problems

Distortion is a expression of the “lack of dimensional stability”. Distortion means

basically “twist awry or out of shape; to make crooked or deformed.” The term
distortion is commonly used in heat treating plants interchangeably with the term
“warpage” which is defined as “to bend or twist out of shape, especially from a
straight or flat form.” In this discussion, the generic term “distortion” will be used to
mean “part movement that can occur any time” while the term “warpage” will be
limited to mean “that distortion which occurs during the heat treating process.”
(Croucher, 2008).

“Cooling must therefore be fast enough to suppress precipitation. On the other

hand, cooling should be slow enough to avoid extensive residual stresses and
distortions (Rose, Kessler, Hoffmann & Zoch, 2006, p. 116).”

34
Table 3.2 Comparison of several commonly used quenchants in cooling rate and distortion
(Pan, 2002)

Quenchant Cooling Rate Distortion

10% NaOH water solution High

10% NaCl water solution High

10% Na2CO3 water solution High

50% NaOH water solution High

Water High

Polymer quenchants Moderate

25% NaNO3 + 20% KNO3 + 20% Increase Moderate

NaNO2 + 35% H2O

Accelerated quenching oil Low

Alkaline salt bath Very Low

Nitrate bath Very Low

Ordinary mechanical oil Very Low

Air Very Low

“Faster rates of quenching retain a higher vacancy concentration enabling higher

mobility of the elements in the primary Al phase during aging. An optimum rate of
quenching is necessary to maximize retained vacancy concentration and minimize
part distortion after quenching. A slow rate of quenching would reduce residual
stresses and distortion in the components, however, it causes detrimental effects such
as precipitation during quenching, localized over-ageing, reduction in grain
boundaries, increase tendencies for corrosion and result in a reduced response to
ageing treatment (Mohamed & Samuel, 2012, p. 62).”

35
3.2.3 Artificial Aging

Age-hardening is one of the most important strengthening methods aluminum

alloys. Through the aging coherent secondary phases precipitate into soft matrix and
causes the formation of dislocations. Aging time and temperature may changes the
mechanical properties significantly. Tensile properties can be enchanced and residual
stresses that occur in quenching can be reduced. In Fig. 3.15 mechanism of the T6
heat treatment and microstructural changes are shown schematically. The
precipitation can also occurs at room temperature it is called natural aging. However,
in industry, artificial aging at temperatures interval from 10°C to 300°C is applied to
accelarete the process (Mohamed & Samuel, 2012).

Figure 3.15 Illustration of the mechanism of T6 heat treatment and precipitation hardening

The precipitation series for Al-Si-Mg alloys can be shortened as follows;

36
 However, Zander & Sandström, (2008) define the series as;

Ogris (2002) was found that the following series;

“where α (SSS) is a supersaturated solid solution, and GP zones are coherent Guiner-
Preston zones (GP zones). The β’’ corresponds to precipitate associated with the
peak-aged condition; they are needle shaped and aligned along [100]Al directions of
the matrix. The seni-coherent β’ precipitate forms after coherent β’’ precipitates in
the aging sequence that are rod shaped and are aligned along [100]Al. The
equilibrium phase β forms as incoherent platelets lying in [100]Al planes. (Ceschini,
Morri & Morri, 2013).”

Figure 3.16 Hardness and Yield Strength curve for A356.0 aluinium alloy with DTAT and STAT with 150°C
and 180 °C (Abdulwahab et al., 2011)

37
 According to aging treatment temperature and time, obtained hardness, yield and
tensile strength alternates. As shown in Fig. 3.16 at high temperature(180°C), YS
value is higher at 2 hours comparing to low temperaure(150°C) and maximum
strength is obtained in shorter time however elongation is sacrificed. Long-aging
process at high temperature causes the grain growth and β’’ particles transforms to β
plate shape therefore mechanical properties (strength, hardness) decrease as seen in
Fig. 3.17 and 3.18. It is called over-aging.

Figure 3.17 GP Zones formation and overaging

Figure 3.18 Hardness curves at different aging temperature and overaging (Long et al., 2013)

38
 If strength is needed, higher artificial aging temperatures and shorter times should
be used to obtain the desired strength and hardness. However, at high temperature,
overaging can be seen and hardness values decreases sharply because of the
increasing precipitation size as shown in Fig. 3.19 (Paz, 2003).

Figure 3.19 Modified and unmodified A356 alloy hardness comparison at different aging parameters
(Paz, 2003)

In addition, quench rate also affect the aging results. TEM characterizations on
A356 alloy were indicated that after quench in water at 25°C, the α-Al matrix
includes in large quantaties needle-shaped and fine β″(Mg2Si) precipitates.
Characterization analysis were showed that the size of the β″(Mg2Si) phases are
roughly 3 to 4 nm in diameter and 10 to 20 in length. Contraraly, at 60°C water
medium, researchers observed that the volume of the precipitates decreases and the
size of the β″(Mg2Si) precipitate phases grows. In addition, a momentous quantity of
fine Si precipitates resulting from precipitation of excess Si can be seen in the
microstructure (Mohamed & Samuel, 2012).

39
3.3 Recent Researches on T6 Heat Treatment

Zhang, Zheng & StJohn (2002) researched that the short solution treatment effects
on tensile and impact properties of stronsium modified A356 alloy. Experiments
carried out in this study at 540°C and 550°C for 10, 30 and 60 min. They found that a
solution treatment at 540°C or 550°C for only 10 minutes is sufficient for the α-Al
phase to homogenise and attain the maximum level of Mg and Si solubility. They
also claimed that a solution treatment for 30 minitus provides spheroidization and
coarsening of the eutectic silicons thus ductility and impact resistance improves.

Rometsch & Schaffer (2002) researched that the relationship between

hardness(HB) and yield strength (YS) for different aluminium alloys. In this study,
aging treatments carried out at 150°C to 250°C for variety times following by
solution tratment at 540°C for 75 min. After the detailed study, they found the
formulas that can be expressed reletionship between HB and YS;

YS=2.95HB[0.065]n (3.1)

Where n is the strain hardening exponent calculated from the total true strain.

Paz (2003) found that well-modified A356 alloy shows very similar hardness
values solution treated for 2, 4 and 6 hours after artificial aging at 155°C. He showed
that 2 hours are enough to obtain similar properties. The artificial aging temperature
and time should be chosen depending on the desired properties. If strength is needed,
higher artificial aging temperatures and shorter times should be used to obtain the
desired strength (236°C-30min). At low temperatures elongation values increases
(155°C-6h). And also he indicated that higher temperatures provide more hardness
only if stay in non-over aging temperatures.

40
 Shabestari & Shahri (2004) researched the effects of cooling rate, Sr and Sb
addition in alloy, the heat treatment and their relationship with microstructure and
mechanical properties of A356 alloy in their study. They said that heat treatment is
more effective on tensile properties than solidification rate and modification.

Kuntongnum et al. (2008) carried out T6 as follows: solution treatment at 520°C

and 540°C for 4 hour before quenching and artificially aging at 135°C, 165°C and
195°C for 4, 8,12 and 16 hr. They found that as the aging temperature increase the
optimum aging time is shorter and the maximum value of hardness decrease.
Likewise Paz (2003) and Fracasso (2010) found the same results in his study.

Long time treatment (535°C-4 h + aging at 150°C- 15h) and short time treatment
(550°C-2h + aging at 170°C-2h) were compared in Ji-hua et al. (2011) study and
they found that “the solution at 535 °C for 4 h and the solution at 550°C for 2 h can
reach full spheroidization of Si particle, over saturation of Si and Mg in α(Al) matrix.
The heat treatments of T6 and ST produce almost the same microstructure of A356
alloy.”

Abdulwahab et al. (2011) used modified A356 alloy with 0.01 Sodium(Na) in
their study, single thermal aging treatment (STAT) and double thermal aging
treatment (DTAT) was applied. Solution treatment carried out at 540°C for 1 hour
and quenched in water followed by an artificial ageing temperatures at 150°C,
180°C, 210°C and ageing time of 1–5, 18, 20 h. Peak hardness value was obtained at
180°C for 20 hours aging (134.9 HVN) and they claimed that the most economic
aging treatment is DTAT at 180°C for 2 h.

In their study Zhu et al. (2012) performed SHT at 535°C for 8 hours followed by
quenching rapidly in water at 25°C, and then artificial aging applied at 160°C for 6 h
followed by air cooling. They mentioned that “the YS-UTS and elongation of the T6-
treated A356 alloys with and without modification are improved due to the
speroidization of eutectic silicon particles and Mg2Si precipitation hardening.”

41
 Long et al. (2013) researched the effect of solution treatment on the age hardening
of an A356 alloy. They showed that prolonged solution treatment has a detrimental
influence on age hardening due to the porosity in the cast A356 alloy. “The diffusion
of Mg atoms toward porosities during solution treatment may lead to a significant
reduction of the Mg solutes available to form Mg–Si-containing strengthening
precipitates in the Al-matrix upon aging treatment. The Mg enrichment around
porosity becomes more severe with the increase of solution treatment time.”

Lee (2013) investigated the T6 heat treatment conditions for low pressure die
casting in order to optimize fatigue properties therefore the solution treatment was
carried out at 540°C for 3,6 or 12 hours and the artificial aging was applied at 160°C
for 4, 8 hours. He claim that “a prolonged solution treatment has a negative influence
on the age hardening due to the existence of porosity in the cast A356 alloy similar
with Long, et al. (2013).” Also one was mentioned that “apart from the
spheroidization of the Si particles during solution treatment, thermally activated Mg
atoms can diffuse out from the Al-matrix and enrich near the porosity pre-existed in
the alloy. The Mg enrichment around porosity becomes more severe with the
increase of solution treatment time." Researcher suggested 540°C for 6 hours and
160°C for 16 hours heat treatment for increasing the number of cycles to failure for
A356 alloy at alternating stress amplitudes of less than 200 MPa.

In order to determine the effect of heat treatment on impact strength Akhil,

SanjiviArul & Sellamuthu (2014) used different size cast components as 20-40-60-80
mm. Parts were heat treated at 537°C for 12 hours followed by a temperature of 155º
for 5 hours. They indicated that “the as-cast condition impact strength increases with
reduction in section size due to grain refinement in smaller section size caused by
fast cooling rate”.

42
 In an other study, A356 and A357 alloys were compared. Solution treatment
experiments were carried out at 520°C, 530°C and 540°C for 5 minutes to 5 hours
and quenched in water then artificially aged at 160°C, 170°C and 180°C. They
concluded that solution heat treatment of A356 and A357 alloys for 15 minutes and
at 540°C, quenched at 25°C and aged for 3h at 180°C, has shown similar hardness
results (Menargues, Martín, Baile, & Picas, 2015).

Tarkun (2015) has reported the mechanical properties and microstructures of

A356 alloy wheels which is produced in CMS Jant ve Makine Sanayi A.Ş. In thesis,
as cast and T6 treated mechanical values are given as following YS 126-201 MPa,
UTS 209-267 and elongation is given 5.7 - 4.3.

There are a quite few research studies on solution treatment and artificial aging.
However, studies on quencing are rare to find in literature espacially aluminium
alloys. Researcher focused on polymer solutions for steel heat treatment and
literature about polymer quenchants is given below.

Kakhki et al. (2009) used PAG type polymer, oil and water for comparing
hardness after quenching and claim that, with using polymer solution desired
properties can be obtained together reducing distortion risk. On the other hand,
according to Liscic et al. (2010) above 74°C PAG loses its effectiveness into water,
PVP shows similar properties with oil because of its density and with adding 10%
PVP can be reach to desired mechanical properties without cracking (Pan, 2002).
10% ACR usage as quenchant equals to oil medium so usage ratio above the 10%
decreases the mechanical properties. Besides that, best mechanical properties obtain
with 16% PAG concentration, medium properties obtain with 22-28% PAG and to
achive optimum distortion control 32-40% PAG should add into water solution
(Croucher, 2008).

43
Figure 3.20 Transition stage with (a) Polymer quenchant (b) Polymer quenchant with surfactant
additive (Liscic et al., 2010)

Liscic et al. (2010) mentioned that some chemical additives into polymer-water
solution may increase the fragmentation time and accelerate the transition to second
stage of cooling. Explotion effect or ligth of foaming can be seen in Fig. 3.20.
Cooling graphs of different polymers are also shown in section 3.2.2.1.

It appears from the aforementioned investigations that most attention has been
paid to quenching of steel parts. Although polymers have been widely used on the
new quenching technologies, there are microbiological problems of their uses in
industry. Quench tanks must be cleaned frequently and circulation must be obtained.
Otherwise, it creates a bad smell in the quench tank and causes environmental risks
and human healthy.

Due to this problem, the surfactant which similar to polymer chemical structure
can be used as quenching medium instead of polymer quenchants.

44
3.4 Surfactants

“Surfactants are the similar chemicals with polymers which are added to the water
for decreasing its surface tension and enhancing the wettability of fluid so that it can
have a better contact with the solid surface (Alam, 2011).” The term surfactant is
a blend of ‘surface active agent’. There are three main type of surfeactant as
following; ionic, non-ionic, anionic.

In earlier investigations on surfactants are generally gives information about the

surface tension that effect the boiling phase but recent studies show that additives
also effect the pool boiling similarly without do not change the surface tension.
Besides, some researchers used the definition of dynamic surface tension instead of
surface tension. Furthermore, Shah & Darby (1973) studied the heat transfer
coefficients for various surfactant mediums. They found that improvement of heat
transfer with increasing surfactant concentration may not caused by surface tension
but by foaming. These results were explained with the phenomenon of light in their
study. Light of foaming can be seen at Fig. 3.20.

Qiau & Chandra (1998) researched the cooling behavior of hot copper with SDS
(Sodium Dodecyle Sulphate) quenchant with a concentration of 100 ppm. They
analyzed the influence of addition of surfactant on boiling curve under the surface
temperature of 240 °C and they found that addition of surfactant enhances the
nucleate boiling heat flux by up to 300 %. Nevertheless, SDS addition reduced the
transition boiling. Alam (2011) used a different surfactants known as Ethoxylated
ester with concentration of 50-100-200-500 ppm.

According to previous studies in literature, it seems that addition of a small

amount of surfactant into cooling medium enhance the heat transfer coefficients and
change the quenching behavior extremely.

45
 CHAPTER FOUR
EXPERIMENTAL STUDIES

4.1 Study of Current Situation

Understanding the current situation is the basis of this study. For this reason,
firstly, the heat treatment of A356 aluminum wheel parts produced by low pressure
casting was studied. Process steps were carried out under standard heat treatment
conditions (temperature and time) applied at CMS Jant ve Makina Sanayi A.Ş. To
study the current situation, solution treatment was performed at 540°C for 240 min.
before quenching at 80°C. After that, artificial aging was performed at 150°C for 180
min. Finally, the painting was applied to the wheels at 180°C for 30 min. and parts
were cooled at room temperature. In this study, different heat treatment procedures
were also applied to understand the effect of each step of heat treatment. These
procedures were given below;

 Only solution treatment

 Solution treatment + painting
 Solution treatment + artificially aging (T6)
 Solution treatment + artificially aging + painting (T6 + painting)
 Only artificially aging (T5)
 Only artificially aging (T5) + painting

4.2 Design of Experiment (DOE) and Heat Treatment Experiments

In order to evaluate the results of the experimental studies systematically, an

experimental design (DOE) was made based on the temperature and time parameters
applied in the literature studies. The experimental studies consist of three steps;
solution treatment tests, solution treatment and aging optimization tests and
quenching tests. For solution treatments, general full factorial 2 factor 5 level design

46
was used and 25 experiments were planned. For solution and aging optimization
tests, 4 factor 3 level 1/2 factorial design was used and 19 experiments were planned.
For the last step, 4 experiments were performed in four different quenching media.
Heat treatments were performed in laboratory type Protherm furnace. Heat treatment
parameters were given in Table 4.1 and 4.2.

According to Minitab results; main effect plots and interaction plots were drawn.
In order to obtain prediction and optimization plots, multiple regression model was
used.

 A main effect is present when different levels of a categorical variable

affect the response differently. For a variable with two levels, one level
can increase the mean compared to the other level. This difference is a
main effect.
 Interaction plots are used in order to assess two-way interactions. Lines is
evaluated to understand how interactions affect the response. If the lines
are parallel, there is no interaction.
 Regression investigates the relationship between a response (Y) and
predictor(s) (X). Multiple regression analyze is an examination of the
linear relationships between one continuous response and two or more
predictors.

Solution treatment experiments were carried out respectively at 510°C, 520°C,

530°C, 540°C, 550°C for 80 min., 160 min., 200 min., 240 min., 280 min. followed
by quenching immediately in water at 80°C for 120 second. The effect of these
parameters on mechanical properties was evaluated in Minitab program.
Microstructures of the samples were also investigated.

Optimization experiments were carried out respectively at 480°C, 510°C, 540°C

for 80 min., 160 min., 240 min. followed by quenching immediately in water at 80°C
and artificially aged at 120°C, 150°C, 180°C for 60 min, 120 min, 180 min..

47
 In the last step of experimental studies, the effect of quenching medium (Table
4.3) on mechanical properties was studied. Different type of surfactants (Triton X-
100, Tween 20, SDS) were used at same amount and other parameters were also kept
constant.

Table 4.1 Design of solution treatment experiments

Solution Treatment Solution Treatment Time

Experiment No
Temperature (°C) (min.)

1 80
2 160

3 510 200

4 240

5 280

6 80
7 160

8 520 200

9 240

10 280

11 80
12 160

13 530 200

14 240

15 280

16 80
17 160

18 540 200

19 240

20 280

21 80
22 160

23 200

24
550 240

25 280

48
Table 4.2 Design of optimization experiments

Solution Solution Artificially Artificiall

Quenhing
Experimen Std Run Treatment Treatment Aging y Aging
Center Pt Blocks Temp.
t No Order Order Temp. Time Temp. Time
(°C)
(°C) (min.) (°C) (min.)

26 15 1 1 1 480 240 80 180 180

27 6 2 1 1 540 80 80 180 60

28 5 3 1 1 480 80 80 180 60

29 13 4 1 1 480 80 80 180 180

30 12 5 1 1 540 240 80 120 180

31 4 6 1 1 540 240 80 120 60

32 17 7 0 1 510 160 80 150 120

33 8 8 1 1 540 240 80 180 60

34 1 9 1 1 480 80 80 120 60

35 16 10 1 1 540 240 80 180 180

36 3 11 1 1 480 240 80 120 60

37 14 12 1 1 540 80 80 180 180

38 18 13 0 1 510 160 80 150 120

39 19 14 0 1 510 160 80 150 120

40 10 15 1 1 540 80 80 120 180

41 2 16 1 1 540 80 80 120 60

42 9 17 1 1 480 80 80 120 180

43 7 18 1 1 480 240 80 180 60

44 11 19 1 1 480 240 80 120 180

49
Table 4.3 Design of quenching experiments

Experiment No Quenchant Amount of Addition

45 Water -

46 SDS 1000 ppm

47 Triton X-100 1000 ppm

48 Tween 20 1000 ppm

In order to determine cooling behavior of the parts at different quenching

mediums, termocuples were attached into the wheels as shown in Fig. 4.1. Datas
collected by using datalogger and computer. Maximum cooling rate, Leidenfrost
points and mechanical properties were examined.

Figure 4.1 Termocupl placed into the wheel (Personal archive, 2019)

50
4.3 Mechanical Testing

In order to determine the mechanical properties, tensile testing was applied and
hardness measurement was performed to the samples. Samples taken for
microstructure examination and mechanical tests were taken from the regions
indicated in the schematic cross-sectional view of the wheel given in Fig. 4.2.

Figure 4.2 Area number of obtained testing specimen

4.3.1 Tensile Testing

Tensile test specimens were prepared as shown in Fig. 4.3 with dimension; 5.64
mm do, 28 mm Lo, 24.98 mm2 So and test was performed according to TS EN ISO
6892-1 standard with Zwick Roell Z100 tensile testing device with 5 N/mm2 pre-
load, 5 N/mm2 test speed and 100 kN Load-cell.

51
 Figure 4.3 Tensile test specimen dimensions

Tensile testing results are shown as elastic module(E), yield strength (Rp0,2),
ultimate tensile strength (Rm) and elongation(A28). Four tests was applied to each
experiments and average was calculated.

4.3.2 Hardness Test

Heat treatment is directly related with hardness due to the homogenation of

matrix, Mg and Si dissolution in alloy and their precipitation behavior. In this study,
Brinell measurement was carried out according to TS EN ISO 6506-1 standard with
Innovatest Nemesis 9000 machine. Specimens were prepared by using milling
machine and grinding with 180 grit. Three tests was applied to each experiments and
average was calculated.

4.4 Microstructure Analysis

After samples were cut from the wheel, samples were grinded with 180, 800,
1000, 1200 grit sand papers. After grinding, samples were polished with diamond
paste. In order to observe the Microstructure, the samples were etched using 3% HF
and the surface cleaned with alcohol. The microstructures were investigated using
Nikon Epiphot 200 in different magnifications.

52
 CHAPTER FIVE
EXPERIMENTAL RESULTS AND DISCUSSION

5.1 Tensile Testing Results

5.1.1 Tensile Testing Results of Current Situation

In order to understand the current situation and determine the effect of different
heat treatment stages on mechanical properties, tensile testing was applied to low
pressure die cast A356 aluminium wheels. Yield strength (YS), ultimate tensile
strength (UTS), and elongation (ε%) results after different heat treatment procedures
are shown in Fig. 5.1 and 5.2 in detail.

Figure 5.1 YS (Rp) and UTS (Rm) results after different heat treatment procedures

Original Equipment Manufacturers (OEM) require the specific yield-ultimate

tensile strength (YS-UTS), elongation (ε%) and hardness (HB) values. The desired

53
mechanical properties must be achieved in the final product. These desired values are
indicated by red dashed lines on the graphs.

There is no significant change in YS and UTS values after solution treatment.

However, as a result of the change in eutectic silicon morphology from acicular to
fibrous shape, elongation value increased from 6 % to 10 %. This results are similar
with Azadi & Shirazabad (2012) study. After artificial aging applied on the as-cast
sample, YS value increased from 97 MPa to 126 MPa with a significant change 26
%.

Figure 5.2 ε% (A28) results results after different heat treatment procedures

Whereas T5 (only aging) enhanced the YS-UTS, elongation values decreased

from 6.0 % to 4.2 %. The results show that artificial aging temperature is not enough
high to change the eutectic silicon morphology and homogenization of the
microstructure.

According to the results, painting process applied after solution treatment and
artificial aging is quite effective on YS and UTS and increased the YS and UTS
values approximately 30 %. The lowest elongation value was obtained after aging

54
and painting. Because of the process condition (temperature and time) are similar,
aging and painting process together is like double aging and has negative effect on
elongation.

Compared to as-cast samples, after T6 heat treatment YS and UTS values of the
samples increased by 93 % and 30 %, respectively. However, elongation decreased
from 6.0 % to 4.4 %. The highest YS and UTS values were obtained after T6 and
painting process. A sharp decrease in mechanical properties was not observed.
Results shows that it was not achieved to over-aging point.

At painting stage, YS and UTS values enhanced 23 % and 10 % respectively on

average. On the other hand, elongation value was decreased approximately 2 %.

Applying the solution treatment is essential to meet the elongation values that are
requested by customers. In addition, artificially aging should be applied to meet YS
and UTS values. For these reasons, the optimization study of heat treatment becomes
important.

5.1.2 Tensile Testing Results of Solution Treatment Experiments

The examination of current situation showed that the solution treatment stage of
T6 is the most important stage for elongation, non-arguably. Therefore, in order to
understand the effect of this stage on mechanical properties, the solution treatments
performed at different temperatures and times as described in Table 4.1.

Yield strenght (YS) values are given in Table 5.1 as Rpmax, Rpmin and Rpaverage.
Each experiment was performed four times and the average was calculated.

55
Table 5.1 YS (Rp) values after solution treatment experiments

Experiment Rpmax Rpmin Rpaverage

Temp.(°C) Time(min.)
No MPa MPa MPa
1 80 77 76 76
2 160 85 84 85
3 510 200 88 81 85
4 240 91 89 90
5 280 92 90 91

6 80 88 83 86
7 160 96 93 94
8 520 200 95 93 94
9 240 101 99 100
10 280 103 100 101

11 80 91 87 88
12 160 99 93 94
13 530 200 99 92 95
14 240 104 101 98
15 280 100 98 96

16 80 94 90 92
17 160 97 97 97
18 540 200 103 95 99
19 240 105 104 104
20 280 110 103 106

21 80 93 89 91
22 160 101 97 99
23 550 200 106 102 103
24 240 106 105 105
25 280 105 103 104

56
 Figure 5.3 YS (Rp) values after solution treatment experiments

In the second part of the study, according to the tensile testing measurement
results after solution treatment experiments, all yield strength (YS) values were
obtained between the as-cast condition and T6 treatment condition.

As it is known from the literature, homogenization of the microstructure and

dissolution of Mg and Si create vacancies during the solution treatment, which leads
to distortionof Al matrix crystals and increase in YS (Lados, Diana, Apelian, Diran,
2011). As can be seen in Fig. 5.3, the increase in time and temperature was observed
with the increase in YS values and the maximum YS value was determined at 550°C
for 280 minutes. It can be said that there is no significant difference between the YS
values obtained at different temperatures and times.

Ultimate tensile strenght (UTS) values are given in Table 5.2 as Rmmax, Rmmin and
Rmaverage. Each experiment was performed four times and average was calculated.

57
Table 5.2 UTS (Rm) values after solution treatment experiments

Experiment Rmmax Rmmin Rmaverage

Temp.(°C) Time(min.)
No MPa MPa MPa
1 80 178 158 168
2 160 192 177 185
3 510 200 191 183 187
4 240 197 176 189
5 280 203 168 190

6 80 192 168 181

7 160 206 181 195
8 520 200 206 169 186
9 240 218 211 214
10 280 218 201 210

11 80 192 171 180

12 160 200 177 186
13 530 200 200 163 186
14 240 214 174 193
15 280 205 171 191

16 80 205 176 190

17 160 198 172 189
18 540 200 210 169 190
19 240 221 206 215
20 280 226 216 221

21 80 192 153 174

22 160 210 173 190
23 550 200 21 186 204
24 240 223 199 212
25 280 219 198 209

58
 Figure 5.4 UTS (Rm) values after solution treatment experiments

Ultimate tensile strength (UTS) shows non-lineer behavior but similar with YS,
UTS values between as-cast condition and T6 treatment condition because of the
homogenization and Mg dissolution into Al matrix. Artificial aging which is the
main strengthening stage, increases the YS and UTS however, in the solution
treatment process, enhancing the mechanical properties must not be expected. To
obtain above 200 MPa UTS, least 200 min. solution treatment must be applied to
aluminium casting part as shown in Fig. 5.4.

ε% values are given in Table 5.3 as A28max, A28min and A28average. Each
experiment was performed four times and average was calculated.

As it is known, in solution treatment stage, the morphology of eutectic silicon

phase changes through the thermal modification. Spheroidization of the eutectic
silicon phase provides ductility and better fracture toughness.

59
Table 5.3 ε% (A28) values after solution treatment experiments
Experiment A28max A28min A28average
Temp.(°C) Time(min.)
No MPa MPa MPa
1 80 13.58 6.50 9.79
2 160 16.33 8.40 12.62
3 510 200 11.44 10.54 10.99
4 240 14.69 7.66 11.27
5 280 14.58 5.43 11.15

6 80 11.95 5.08 9.16

7 160 15.25 7.66 11.50
8 520 200 13.85 5.51 9.18
9 240 21.07 17.15 18.96
10 280 21.85 10.78 15.93

11 80 13.24 4.35 8.45

12 160 14.33 4.77 8.85
13 530 200 14.14 4.12 8.83
14 240 13.23 6.93 9.61
15 280 11.32 4.49 9.99

16 80 14.03 6.39 10.32

17 160 10.25 5.03 8.34
18 540 200 13.85 4.59 8.25
19 240 18.48 10.85 15.40
20 280 19.85 16.50 18.58

21 80 9.77 3.12 6.60

22 160 13.67 5.48 8.88
23 550 200 15.43 6.58 11.00
24 240 17.16 8.97 12.84
25 280 15.58 8.59 11.79

60
 Figure 5.5 ε% (A28) values after solution treatment experiments

In addition, as mentioned in literature, solution treatment homogenizes the

microstructure by dissolving the as-cast plate shape Mg2Si precipitates, inclusions
and by transforming the β-Al5FeSi intermetallic phases into the rounded phase
(Zedan et al., 2010; Zander & Sandström, 2008). It reduces the segregation and
elongation improves. Hence, test results as given in Fig. 5.5 show that elongation
increases up to 19 % when parts treated at 520°C and 540°C for 240 min (Zhu et al.,
2012).

Low elongation values were obtained at 530°C for all test time. Microstructure of
the sample is shown in Fig. 5.26. It was observed that Fe-rich intermetallic phases
exist in α-Al matrix. These phases are formed because of the low solidification rate
at casting process. Fe intermetallic exists in α-Al matrix in two forms: α-Fe and β-Fe
forms. α-Fe is also known as Chinese script. Comparing to the α-Fe phase, β-Fe
effects the elongation and toughness more in negative way (Mohamed, Samuel,
Samuel & Doty, 2009). In this case, obtained low values can be explained by these
brittle Fe-rich intermetallic phases.

61
5.1.3 Tensile Testing Results Of Optimization Experiments

Results of optimization experiments (Rp, Rm, A28) were given in Table 5.4.

Table 5.4 YS (Rp), UTS (Rm) and ε% (A28) values of optimization experiments

Quenhi
SHT SHT Aging Aging Rp Rm A28
Exp. Std Run Center ng
Blocks Temp. Time Temp. Time average average averag
No Order Order Pt Temp.
(C°) (min.) (C°) (min.) MPa MPa e MPa
(C°)

26 15 1 1 1 480 240 80 180 180 81 153 5.49

27 6 2 1 1 540 80 80 180 60 132 202 3.40

28 5 3 1 1 480 80 80 180 60 73 148 6.15

29 13 4 1 1 480 80 80 180 180 77 146 4.69

30 12 5 1 1 540 240 80 120 180 170 227 3.03

31 4 6 1 1 540 240 80 120 60 133 186 2.43

32 17 7 0 1 510 160 80 150 120 114 186 3.94

33 8 8 1 1 540 240 80 180 60 184 242 3.21

34 1 9 1 1 480 80 80 120 60 70 149 5.96

35 16 10 1 1 540 240 80 180 180 198 244 2.19

36 3 11 1 1 480 240 80 120 60 79 159 6.32

37 14 12 1 1 540 80 80 180 180 171 222 1.87

38 18 13 0 1 510 160 80 150 120 120 192 3.99

39 19 14 0 1 510 160 80 150 120 120 192 3.99

40 10 15 1 1 540 80 80 120 180 135 198 2.90

41 2 16 1 1 540 80 80 120 60 110 184 3.97

42 9 17 1 1 480 80 80 120 180 71 146 5.99

43 7 18 1 1 480 240 80 180 60 81 159 6.27

44 11 19 1 1 480 240 80 120 180 76 152 5.82

62
 5.1.3.1 Statistical Analysis of Yield Strength Results

According to the main effect analysis, it was found that solution treatment
temperature is the most effective parameter on the YS values, but the values obtained
at 480°C were the same as the casting state (80 MPa) and this temperature was not
sufficient to provide the solubility of the Mg2Si phase in the structure and to form a
supersaturated solid solution which gave the precipitation hardening ability to
material. Besides that YS is affected positively by solution treatment time, aging
time and temperature in linear proportional as given in Fig. 5.6.

In order to obtain desired YS, solution treatment and aging must be carried out at
least 516°C for 240 min. and 180°C for 180 min., respectively. Similar results might
be obtained at 540°C for 80 min. and 180°C for 180 min. Interactions between
parameters were given in Fig. 5.7. A gray background represents a term that was
removed from the model because it is not statistically significant. Detailed
optimization parameters and five different options were settled in Fig. 5.8.

Figure 5.6 Main effects screener for yield strength

63
 Figure 5.7 Interaction plots for yield strength

According to multiple regression analysis, the formulation of the YS value

depending on the variables was given.

Figure 5.8 Prediction report and five alternative parameters for yield strength (Target 155MPa)

64
 5.1.3.2 Statistical Analysis of Elongation Results

According to main effect analysis, it was found that solution treatment

temperature is the most effective parameter on ε% value but the values obtained at
480°C were the same as the casting state (6 %) and this temperature is not sufficient
to spherozation of acicular shape eutectic silicons in the microstructure. However, as
the solution treatment temperature increases, obtained ε% values decreases after T6
treatment. Besides that ε% is affected negatively by aging temperature and time in
linear proportional as given in Fig. 5.9.

In order to obtain the maximum value for ε%, solution treatment temperature,
aging time and temperature must be minimize as much as possible however
parameters must be adjusted to reach desired YS and HB at the same time. Hence,
solution temperature must be 516°C at least. Detailed optimization parameters were
settled in Fig. 5.11.

Figure 5.9 Main effect screener for elongation

65
 Figure 5.10 Interaction plots for elongation

According to multiple regression analysis, the formulation of the ε% value

depending on the variables was given.

Figure 5.11 Prediction report and five alternative parameters for elongation (Target 4.5 ε%)

66
5.1.4 Tensile Testing Results of Quenching Experiments

Results of quenching experiments (Rp, Rm, A28), maximum cooling rates and
Leidenfrost points were given in Table 5.5.

Table 5.5 YS (Rp), UTS (Rm), ε% (A28) values of quenching experiments

Maximum
Rp Rm A28
Experiment Cooling Leidenfrost
Quenchant average average average
No Rate Point (°C)
MPa MPa MPa
(°C/s)

45 Water 85 442 140 230 7.5

46 SDS 61 385 135 229 8.2

47 Triton X-100 68 448 135 229 8.2

48 Tween 20 70 453 129 225 8.2

According to results, quenching with water displays higher YS than the surfactant
quenchants. Nevertheless, YS values were obtained similar between 129-140 MPa as
seen in Table 5.5. It found that critical cooling rate was provided to suppress
precipitation in all quenching mediums and 61°C/s (Tween 20) was enough to obtain
supersaturated solid solution. In both water and surfactant quenchant cooling
mediums, obtained the same elongation values and standard deviations were equal.

Cooling behavior of A356 wheel parts at four different mediums were given in
Fig. 5.12. Experiment results show that the shortest (10 second) and the fastest
(85°C/s) cooling was obtained with water. Triton X-100 and Tween quenchants
slowed down the cooling rate to approximately 70°C/s. The longest (20 second) and
the slowest cooling (61°C/s) was obtained with SDS quenchant.

67
 Cooling Behavior at Different Quench Mediums
600
Variable
Water
SDS
500 Triton X-100
Tween
Temperature °C

400

300

200

100

0,0 3,0 6,2 9,4 12,6 15,8 19,0 22,2 25,4 28,6
Time (second)

Figure 5.12 Cooling behavior at different quench mediums

Low cooling rates with SDS, Triton and Tween, can be explained by surfactant
layer that composed on the surface at the beginning of cooling when part immersed
into surfactant quenchants. This layer slows down the cooling rate like polymer or oil
quenchants as mentioned in literature before. Fragmentation of layer and direct
contact with aluminium surface begins when Leidenfrost point surpass. It was
determined that surfactant layer fragmentation occurs in 4 seconds as illustrated in
Fig. 5.13. In water medium, nucleate boiling phase was began directly after reaching
Leidenfrost point.

Vapor blanket (film boiling), nucleate boiling and convection cooling phases can
be seen on Fig. 5.12. and 5.13. Maximum cooling rate and Leidenfrost points of each
quenchant were determined for the first time for A356 alloy by using surfactant
addition.

68
 Cooling Rate at Different Quench Mediums
90 Variable
Water Δ
80 SDS Δ
Triton X-100 Δ
70 Tween 20 Δ
Cooling Rate (°C/s)

60

50

40

30

20

10

540 500 450 400 350 300 250 200 150 135 100 50
Temperature (°C)

Figure 5.13 Cooling rate at different quench mediums

69
5.2 Hardness Test Results

5.2.1 Hardness Test Results of Current Situation

In order to analyze current situation and determine the effect of different heat
treatment stages on mechanical properties, hardness testing was applied to low
pressure die cast A356 aluminium wheels as indicated section 4.4.2.

Figure 5.14 HB results at different heat treatment stages

There is no significant change in hardness values after solution treatment as

shown in Fig. 5.14. Otherwise, hardness value increased after T5 treatment in which
only only artificial aging. It can be explained by precipitation theory of Mg2Si,
formation of Mg-Si clusters and GP zones. Compared to as-cast samples, after the
entire T6 heat treatment hardness values of casting parts increased by 40% from 66
HB to 91,42 HB. The highest hardness values were obtained after T6+painting
process as 95HB. It was also determined that painting process, after only solution
treatment or only artificially aging, increased the hardness value approximetely 12%

70
however after T6 heat treatment increased only 4% because of the majority of
secondary hardening phases was already precipitated into Al matrix.

5.2.2 Hardness Test Results of Solution Treatment Experiments

Brinell hardness values are given in Table 5.6 as Brinell. Mean datas was obtained
from three hardness measurement of each specimen.

Table 5.6 Hardness(HB) values of solution treatment experiments

Experiment
Temp.(°C) Time(min.) Hardness (HB)
No
AS-CAST 66
T6 91
1 80 57
2 160 62
3 510 200 56
4 240 62
5 280 53
6 80 63
7 160 65
8 520 200 65
9 240 65
10 280 60
11 80 57
12 160 63
13 530 200 60
14 240 64
15 280 65
16 80 63
17 160 63
18 540 200 66
19 240 63
20 280 64
21 80 63
22 160 60
23 550 200 68
24 240 65
25 280 64

71
 Figure 5.15 HB values of solution treatment experiments

Distribution of hardness values shows that soft aluminium matrix was hardened
through the Mg-Si dissolution but there is no meaningful differences between low
and high temperatures. As mentioned in section 3.2.3. hard Mg2Si phase disperse
into matrix homogeneously after aging proecess as fine β” and thus hardness of
material increase. However, in solution treatment stage, hardness improvement was
seen up to only 5 HB (Fig. 5.15). Hardness results are compatible with hardness of
low pressure die cast wheels and it measured approximately 60-65 HB. With this
study, it is understood that the solution treatment has no significant effect on
hardness without any aging or painting process.

72
5.2.3 Hardness Test Results of Optimization Experiments

Hardness(HB) results of optimization experiments are given in Table 5.7.

Table 5.7 Hardness(HB) values of optimization experiments

Quenh
Exp. Std Run Center SHT SHT Aging Aging Hardness
Blocks Temp.
No Order Order Pt Temp.(C°) Time(min.) Temp.(C°) Time(min.) (HB)
(C°)

26 15 1 1 1 480 240 80 180 180 54

27 6 2 1 1 540 80 80 180 60 71

28 5 3 1 1 480 80 80 180 60 49

29 13 4 1 1 480 80 80 180 180 50

30 12 5 1 1 540 240 80 120 180 78

31 4 6 1 1 540 240 80 120 60 79

32 17 7 0 1 510 160 80 150 120 66

33 8 8 1 1 540 240 80 180 60 82

34 1 9 1 1 480 80 80 120 60 48

35 16 10 1 1 540 240 80 180 180 86

36 3 11 1 1 480 240 80 120 60 51

37 14 12 1 1 540 80 80 180 180 84

38 18 13 0 1 510 160 80 150 120 68

39 19 14 0 1 510 160 80 150 120 68

40 10 15 1 1 540 80 80 120 180 68

41 2 16 1 1 540 80 80 120 60 61

42 9 17 1 1 480 80 80 120 180 47

43 7 18 1 1 480 240 80 180 60 49

44 11 19 1 1 480 240 80 120 180 49

73
 According to the main effect analysis, it was found that solution treatment
temperature is the most effective parameter on HB values, but the values obtained at
480°C are the same as the hardness of the sample after casting (50 HB) and similarly
with YS value assessment in section 5.1.3.1 this temperature was not sufficient to
provide supersaturated solution for catalyzing the precipitation hardening. Therefore,
hardness of the material was seen steady. On the other hand, HB increases to a
certain limit value with increasing aging temperature and time (Fig. 5.16). This
results reflects the findings of Fracasso(2010) and Menargues et al. (2015).

In order to obtain desired hardness, solution treatment and aging must be applied
following at least 522°C for 240 min. and 180°C for 180 min. Similar results might
be obtained, independent from aging time, at 540°C for 80 min. solution and 180°C
aging or 540°C for 240 min. solution and 120°C aging. Detailed optimization
parameters and five different options were settled in Fig.5.18.

Figure 5.16 Main effect screener for hardness

74
 Figure 5.17 Interaction plots for hardness

According to multiple regression analysis, the formulation of the HB value

depending on the variables was given.

Figure 5.18 Prediction report and five alternative parameters for hardness (Target 75HB)

75
5.2.4 Hardness Test Results of Quenching Experiments

Hardness measurement of optimization experiments (HB) were given in Table

5.8. According to the hardness results, it was determined that 61°C/s cooling rate is
enough to supress solute atoms into supersaturated solid solution (SSS) and critical
rate for A356 alloy was similar with Milkereit et al. (2014) study. Hardness values
were obtained at range of 61-85°C/s cooling rate as seen in Fig. 5.19.

Table 5.8 Hardness(HB) values of quenching experiments

Maximum Leidenfrost
Hardness
Experiment No Quenchant Cooling Rate Point (°C)
(HB)
(°C/s)

45 Water 85 430 77

46 SDS 61 415 78

47 Triton X-100 68 438 76

48 Tween 20 70 459 75

Interval Plot of Hardness

95% CI for the Mean
90

85

80
78
Hardness (HB)

77
76
76
75

70

65

60
SDS TritonX-100 Tween20 Water
Quenchant
Individual standard deviations were used to calculate the intervals.

Figure 5.19 HB values of quenching experiments

76
5.3 Microstructure Analysis Results

Microstructures of the wheel parts after heat treatment are given in Fig. 5.20.
Lamellar eutectic silicon phases and plate-shape intermetallic phases are seen in as-
cast sample. After T6 treatment, spherodatization is occured and plate-shape Mg2Si
and other intermetallic phases disappared. Changes on phases directly effect the
mechanical properties so microstructural analyze must be done adequately. After
solution treatment experiments, all parts was examined with optical microscopy and
micrographs were taken at 200x and 500x magnifications.

Figure 5.20 Microstructures of as-cast (a)200X, (b)500X and T6 heat treated (c)200X, (d)500X
samples

77
Figure 5.21 Microstructures of solution treated parts at 510°C at 200X and 500X for (a)(b)80 min,
(c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min

78
Figure 5.22 Microstructures of solution treated parts at 520°C at 200X and 500X for (a)(b)80 min,
(c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min

79
Figure 5.23 Microstructures of solution treated parts at 530°C at 200X and 500X for (a)(b)80 min,
(c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min

80
Figure 5.24 Microstructures of solution treated parts at 540°C at 200X and 500X for (a)(b)80 min,
(c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min

81
Figure 5.25 Microstructures of solution treated parts at 550°C at 200X and 500X for (a)(b)80 min,
(c)(d)160min, (e)(f)200min, (g)(h)240min, (i)(j)280min

82
 Figure 5.26 Fe-intermetallics in the microstructure of solution treated part at 530°C

Effect of solution treatment temperature and time on eutectic silicon phase

formation and homogenization of the microstructure were given in Fig. 5.21-26.
Spheroidization can be seen even at 510°C however degree of roundness increased
gradually with the increasing temperature. At 540°C and 550°C silicon phases
become fully rounded and larger.

The microstructure is more affected by time change than the solution treatment
temperature variation. Intermetallics, plate shape Mg2Si phases and half-
rounded/rounded eutectic silicon phase were detected in the microstructure of
solution treated sample at 510°C for 80 min. However, longer time as 240-280 min
was appropriate to change the silicon morphology and diffuse intermetallic phases
totally (Fig. 5.27).

83
Figure 5.27 Microstructure of the Sr-modified A356 alloy samples after (a) 510°C for 80 min and (b)
510°C for 280 min solution treatment

84
 CHAPTER SIX
CONCLUSION

In this thesis, effect of;

 Each of current heat treatment and painting stages on mechanical properties,

 Time and temperature of solution treatment on mechanical properties and
microstructure,
 Different solution treatment and artificial aging conditions on mechanical
properties,
 Quenching medium on cooling rate mechanical properties

of Sr modified-A356 low pressure die cast wheels was investigated and the main
finding can be summarized as follow.

According to current situation analysis;

 Depending on the desired mechanical properties, different stages of the heat

treatment can be applied to as-cast parts separately or in combination. The
yield-ultimate tensile strength and hardness were enhanced by applying
artificially aging and painting without solution treatment however desired
elongation values were not obtained.

 It was shown that elongation predominantly depends on solution treatment

and increases the elongation up to 40% due to the spheroidization of eutectic
silicon and homogenization of microstructure. Besides that intermetallic
phases that exist in microstructure because of low solidification rate,
decreases elongation sharply.

 Solution treatment has no effect on yield-ultimate tensile strength and

hardness by oneself. Whereas it was determined that values vary considerably
when the same aging or painting process applied after different solution
treatments.

85
 Artificially aging increases the yield strength respectively 46% and 23%,
likewise, it hardened the material respectively 27% and 8%, with and without
solution treatment.

 Painting increases the yield strength respectively 22% and 8%, likewise, it
hardened the material respectively 12% and 4%, before and after T6
treatment.

According to solution treatment experiments and optimization plots;

 510°C is quite enough to change the microstructure and after only solution
treatment, same mechanical properties were obtained at 510°C for 80 min
(Fig. 6.1). On the other hand, in microstructure, it was detected half rounded
and lamellar eutectic silicons.

Figure 6.1 Optimization plot for (a) target elongation, (b) maximum elongation

86
According to optimization experiments;

 As a result of multiple regression analysis, formulas of mechanical properties

related to heat treatment variables were formed.

 It was understood that 480°C is not sufficient to provide supersaturated

solution for catalyzing the precipitation hardening and changing the
morphology of acicular eutectic silicons.

 Although 510°C and 80 or 200 minutes solution treatment seems to be

enough to obtain same mechanical properties (comparing only solution
treated parts) and low solution treatment temperature causes more elongation,
it was found that after the artificial aging, desired yield strength and hardness
cannot be obtained at 510°C and temperature must be increased. (Mechanical
properties of final product, excluding paint process, was accepted as 155MPa
YS, 4.5 ε%, 75HB)

 Also it was found that solution treatment temperature must be least 516°C in
order to obtain desired YS value (155MPa) and must be least 522°C in order
to obtain desired HB value (75HB) after T6 treatment.

 Alternative heat treatment parameters were calculated and given in prediction

reports.

According to quenching experiments;

 Cooling rate and leidenfrost points were determined for the first time for
A356 alloy at water-surfactant quenchant medium.

 It was found that maximum cooling rate values of surfactant quenchants are
between the water and polymer quenchants and calculated as 61-70°C/s.
Maximum cooling rate was observed in water as 85°C/s.

87
 Critical cooling rate was determined as 61°C/s.

 Leidenfrost points of water and surfactant quenchants were determined and it

was found that after reaching this point cooling rate increases dramatically in
water. However, in surfactant quenhing medium, cooling rate increased after
decomposition of surfactant layer.

88
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