Grain Size Effect on Softening Behaviour of Al-Mg Alloy due to Paint Bake Heat

Treatment

HEMALATHA NADARAJAH

A report submitted in partial fulfillment of the

requirements for the award of the degree of
Bachelor of Mechanical Engineering

Faculty of Mechanical Engineering I - --

Universiti Malaysia Pahang

NOVEMBER 2007
 ABSTRACT

Aluminium- Magnesium (Al-Mg) alloys have very good formability properties

and have been used extensively for interior structural components of automotive Body in
White (BIW). The alloys in an annealed temper achieve their strength through work
hardening mechanism during press forming process. The strengthening mechanism is
due to Mg atoms in solid solution exerting dislocation drag during low temperature
plastic straining. However at elevated temperatures, high diffusivity of Mg atoms allows
easy dislocations rearrangements which lead to reduction of mechanical strength. This
phenomenon is called softening. Furthermore, accumulation of stored energy in the
dislocations substructures due plastic straining during press forming process also serves
as a large driving force for thermal recovery. These two factors contribute Al-Mg alloy
sheet to be susceptible to softening during paint bake cycle. Al-Mg sheets for automotive
Body in White (BIW) applications are normally supplied in an annealed condition
known as "-0-" temper. The microstructure of an annealed sheet is characterized by
equiaxed recrystallized grains. Average size of grains depends on actual rolling
schedule and heat treatment stages on those particular sheets. This project investigates
the effect of varying grain size on softening characteristics of pre-strained sheets after
paint bake cycle. This is done by annealing Al-Mg H32 sheets in different temperatures
to obtain different grain size. Smaller grain size would have more softening than larger
grain size.

V
 ABSTRAK

Aioi Aluminium-Magnesium mempunyai ciri-ciri pembentukkan yang balk dan

telah digunakan untuk komponen struktur dalaman untuk rangka putih automotif (B1W).
Aloi dalam keadaaan 'anneal' mencapai kekuatan melalui proses pengerasan ketika
pemampatan berlaku. Mekanisem penguatan berlaku disebabkan atom Mg yang berada
dalam keadaan cecair pejal menghasilkan penolakan hang jetika ketegangan plastic pada
suhu yang rendah. Walau bagaimanapun, pada suhu berbeza, kehilangan atom Mg
mengakibatkan aturan atom bertaburan dan seterusnya menyebabkan kekuatan
mekanikal aloi itu menurun. Fenomena inilah yang dipanggil pelembutan('softening').
Tambahan pula, akumulasi tenaga simapanan dalam substruktur hasil daripada
ketegangan plastic ketika pemampatan berlaku juga menjadi :sebab untuk penyembuhan
tennal. Kedua-dua factor mi menyumbang kepada pelembutan Al-Mg ketika kala
pengeringan cat('paint bake cycle'). Kepingan Al-Mg di hantar dalam keadaan 'anneal'
yang juga dikenali sebagai -0-. Mikrostruktur kepingan mi mempunyai butiran yang
seragam. Saiz butiran bergantung kepada kepada pemprosesan dan haba. Projek mi
menyiasat kesan saiz butiran berbeza terhadap ciii pelembutan untuk Al-Mg yang telah
ditegangkan apabila melalui proses pengeringan cat. mi dilakukan dengan mambakar Al-
Mg dalam pelbagai suhu untuk rnenghasilkan saiz butiran berbeza. Butiran yang bersaiz
kecil akan menghasiikan nilai pelembutan yang lebili banyak daripada butiran yang
besar.

A
 TABLE OF CONTENTS

CHAPTER TITLE PAGE

AKNOWLEDGEMENT iv
ABSTRACT v
ABSTRAK vi
TABLE OF CONTENTS vii - ix
LIST OF TABLES x
LIST. OF FIGURES xi— xii
LIST OF APPENDICES xiii
LIST OF SYMBOLS xiv

INTRODUCTION 1
1.1. Objective 3
1.2. Scopes 3
1.3. Project background 3
1.4. Gantt Chart 4
l.5. Flow Chart 4

2 LITERATURE REVIEW 5
2.1. Al-Mg Alloy 5
2.1.1. Aluminium 6-7
2.1.2. Production of Aluminium 6-7
2.1.3. Wrought Aluminium alloy series 7
2.1.4. Basic temper designation 8-9

vi'
 2.1.5. Non heat treatable and heat treatable
wrought aluminium alloys 10
2.1.6. Wrought Al-Mg alloys 10-11

2.2. Grain, Grain boundaries, and grain size 12

2.2.1. Structure of metals 12
2.2.2. Crystal structure of metals 13-14
2.2.3. Grains 15
2.2.4. Grain Boundaries 15-16
2.2.5. Grain Size 16-18

2.3. Recovery, recrystalization and grain growth 18-19

2.3.1. Recovery 19
2.3.2. Recrystalization 19-20
2.3.3. Grain growth 20

2.4. Defects in crystal structure and work hardening 21

2.4.!. Deformation and strength of a single
crystal 21
2.4.2. Crystal structure for alloys 21-22
2.4.3. Imperfection in the crystal structure
of metal 22-23

3 EXPERIMENTAL TECHNIQUE 24
3.1. Introduction 24
3.2. Specimen preparation 24-25
3.3. Hardness testing 26
3.4. Full Annealing 27-28

vii'
 3.5. Prestrain tensile testing 29-30
3.6. Recovery heat treatment and retest tensile test 31-32
3.7. Data Conversion 32-35
3.8. Metallography 36
3.8.1. Sectioning and cutting 36
3.8.2. Mounting 37
3.8.3. Planar grinding, fine grinding
and polishing 38
3.8.4. Etching 39
3.8.5. Microscopic analysis 40

4 RESULT AND DISCUSSION 41

4.1. Hardness test results 41-44
4.2. Prestrain tensile test results 45-49
4.3. Softening versus prestrain 49-52
4.4. Softening versus temperature 53-54

5 CONCLUSION AND RECOMMENDATION 55

REFRENCES 56-57
Appendixes A- K 58-69

ix
 LIST OF TABLES

TABLE NO TITLE PAGE

2.1 Numerical designation of aluminium alloys 7

2.2 Temper designation of aluminium alloys 9

2.3 Composition of commonly used BIW Al-Mg alloys 11

2.4 Mechanical properties of commonly used BIW Al-Mg alloys 11

2.5 Atomic arrangements 14

3.1 Heat treatment for grain size 1 27

3.2 Different grain size tested with different prestrain 30

3.3 Different grain size tested with 1% strain after paint bake cycle 31

3.4 Softening of specimen with different temperature

and prestrain 35

3.5 Stages in etching process 39

4.1 Hardness test results for AA5083 42

4.2 Softening value for AA1 100 1.5 mm 50

4.3 Softening value for AA1 100 2.0 mm 51

x
 LIST OF FIGURES

FIGURE NO TITLE PAGE

1.1 Effect of varying grain size on the softening behavior 4

2.1 Bayer process - Aluminium production 6

2.2 Crystal production 12

2.3 Grains 15

2.4 Grain boundaries 16

2.5 Effects of recovery, recrystalization on mechanical properties

size of grain 19

2.6 Edge dislocation 22

2.7 Defects in a single crystal lattice 23

3.1 Turret punch machine 25

3.2 ASTM E8 tensile test specimen 25

3.3 Furnace used for heat treatment and its controller 27

3.4 Annealing 28

3.5 Air cooling 28

3.6 1NSTRON tensile test machine 29

3.7 Tensile test results for GS I with 5%,1 0%,1 5%,

and 20% prestrain 30

3.8 Process of testing 32

3.9 Conversion of force and displacement to stress and strain 33

xi
 3.10 Conversion of stress strain to graph 34

3.11 Stress difference of before and after paint bake cycle 34

3.12 Cutting machine 36

3.13 Chemical and equipment for epoxy 37

3.14 Pressure vessel 37

3.15 Grinding and polishing equipment 38

3.16 Microscopic analysis 40

4.1 Hardness (HV) versus temperature for AA5083 43

4.2 Comparison of different temperature for AA 1100 1.5mm with

different prestrain 46

4.3 Comparison of different temperature for AA 1100 2.0 mm with

different prestrain 47

4.4 Softening calculation 49

4.5 Softening versus prestrain for AM 100 1.5mm 51

4.6 Softening versus prestrain for AA1 100 2.0mm 51

4.7 Different grain size due to annealing 53

4.8 Softening versus temperature for AA 1100 1.5mm 54

4.9 Softening versus temperature for AA1 100 2.0mm 54

XII

E.
 LIST OF APPENDICES

APPENDIX TITLE PAGE

A Gantt chart 58

B Flowchart 59

C 350°C with 5% - 20% prestrain for AA1 100 1.5mm 60

D 400°C with 5% - 20% prestrain for AAI 100 1.5mm 61

E 450°C with 5% - 20% prestrain for AA 1100 1.5mm 62

F 500°C with 5% - 20% prestrain for AA1 100 1.5mm 63

G 550°C with 5% - 20% prestrain for AA1 100 1.5mm 64

H 350°C with 5% - 20% prestrain for AA 1100 2.0mm 65

I 400°C with 5% - 20% prestrain for AAI 100 2.0mm 66

J 450°C with 5% - 20% prestrain for AA1 100 2.0mm 67

K 500°C with 5% - 20% prestrain for AA1 100 2.0mm 68

L 550°C with 5% - 20% prestrain for AAI 100 2.0mm 69

xlii
 LIST OF SYMBOLS

ay - Yield strength of metal

a0,k - Hall Patch constants

d - Grain diameter

n - Number of grain

N - Size of grain

F - Force

- Stress

c - Strain

xiv
 CHAPTER 1

INTRODUCTION

Aluminium is well known for its high strength to weight ratio. Aluminium is
a nonferrous metal whereby it has important properties such as corrosion resistance,
high thermal and electrical conductivity. Aluminium and aluminium alloys posses a
unique combination of properties, making them versatile materials of construction for
many applications, from wrapping foil to aerospace components.

Like other metals, aluminium is identified by various designation systems.

The principle alloying elements in aluminium are copper, manganese, silicon,
magnesium, and zinc. Aluminium alloys are wrought or cast and can be strengthened
by cold working or precipitation hardening. Aluminium alloys are formed machined
and joined using variety of processes.

Work-hardening wrought Al-Mg alloys which are also known commercially

as the 5000 series aluminium-based alloys are currently being used as automotive
BIW material. Magnesium is the principal alloying element and is added for solid-
solution strengthening. Generally Al-Mg alloys used in BIW applications have very
good formability; relatively low yield stress and work harden during cold working.
 2

A finished assemble automotive 131W complete with its exterior closure panel
would have to primed, coated and painted; followed by a paint baking cycle. The
cycle is nominally being carried out at 175 °C for 30 minutes (Bryant, 1999). This
set of conditions is adequate to start the thermal recovery process which leads to
softening of the material.

Initial study by Burger et al. (Burger et al., 1995) has shown that the
softening process Is influenced by both heat treatment time and pre-straining. At
about 10% pre-strain, the material softens by 50 MPa. This drop can be translated to
almost 20% reduction of strength since the material would work harden to about 250
MPa after 10% straining. The softening phenomenon should be considered because
in sheet metal forming operations, strain level of between 10%-20% is common In
production of stretch-drawn components.

Al-Mg sheets for automotive BIW applications are normally sent in —0-
temper whereby the sheet has been annealed and recrystallized. This process is done
by heating a number of coils in a large batch furnace. These sheets have equiaxed
recrystallized grains. The more heat is supplied the bigger the grain size gets. Grain
size affects the softening behaviour of the pre-strained sheets after paint bake cycle.

The softening behaviour is also influenced by heat treatment time. After

applying heat treatment at 177 °C for 30 minutes (1800 seconds), the material that
has been 15% pre-strain has soften by almost 50 MPa. This study which was carried
out by Burger et al. (Burger et al., 1995) has shown that significant softening could
occur under normal paint bake heat treatment. Therefore a more extensive
investigation should be initiated in order to thoroughly understand the softening
behaviour of pre-strain Al-Mg alloys subjected to paint bake treatment.
 3

1.1 Objective

i) To study to the effect of varying original material grain size on

softening characteristics of pre-strained sheets after paint bake cycle.

1.2 Scopes

i) The research is limited to commercially pure aluminium AAI 100,

AA5052 (2.3% Mg) and AA5083(4.5% Mg) 5xxx series wrought
aluminum ahoy.
ii) Heat treatment cycle is limited to ±50°C of the average paint baking
temperature which is 175°C- 177 °C for 30 minutes.
iii) Grain size varies from 350°C to 550 T.

1.3 Project Background

Al-Mg alloy sheets for automotive BIW applications are normally supplied in
an annealed condition known as '-0' temper. The annealing stage for '-0' temper is
performed after the final gauge has been achieved in a cold rolling schedule by
heating a number of coils in large batch furnace (batch annealing). The
microstructure of an annealed sheet is characterised by equiaxed recrystallized
grains. Average size of grains of Al-Mg alloy sheet depend on the actual rolling
schedule and heat treatment stages of that particular sheet. The size of the grain
effects the softening characteristics of pre-strained sheets after paint bake cycle.
 4

30 minutes 175C
(Grain Size (GS))

GSI

I
GS2

GS3

GS4

0 5 10 10
Pro-strain (%)

Figure 1.1: Schematic graph showing the effect of varying grain size on softening
behavior

1.4 Gantt Chart

The Gantt chart is illustrated in Appendix A

1.5 Flow Chart

The flow chart is illustrated in Appendix B

 CHAPTER 2

LITERATURE REVIEW

2.1 Al-Mg Alloy

2.1.1 Aluminium

Metal have played an important role in the development of human

civilization. In this development, there has not been a metal, apart from steel as
versatile as aluminium because of its unique intrinsic characteristics which are in
Interest :f scientist and engineers (Murakami, 1985). The density of alumInIum Is
only 2.7 g1cm3, about one third of steel which makes it a useful material for
transportation manufactured product (Kalpakjian and Steven, 2001). Since Its
lighter, it reduces the cost per pound and increases the specific strength of
aluminium. 5- 10% fuel savings are realized for every 10 0/o reduction in vehicle
weight (Studied by Ford, BMW, Argonne, Ross, EAA, International Aluminium
Institute, 2000). An aluminium Body in White (BIW) is typically 40-45% lighter
than an equivalent steel structure (R.W.Cahn et al, 2005).

Aluminium has good corrosion resistance, non toxic, and has good electrical
properties. Because aluminium has low strength it is alloyed for greater strength.
Aluminium offers rapid and economical machinability. Hence, aluminium is very
favorable for designing a safer and cleaner car without adding too much weight for
 6
various construction part and engines. Moreover with growing environmental
pressUre to reduce' noxious fume emissions and also to achieve maximum recycling
of all car materials together with the increasing importance of oil, aluminium seems
to attractive as lighter vehicle consume less oil.

2.1.2. Production of Aluminium

Aluminium is the most abundant metallic element, which is 8% of the earths

crust (Kalpakjian, 2001). Aluminum is found in earth's crust always combined state
with other elements such as iron, oxygen, and silicone. Bauxite, which consists of
mainly hydrated aluminum oxides, is the main source of aluminum. This is produced
by Bayer process as Figure 2.1.

Aluminum in the ore

(Crushed into powder)

Hot sodium hydroxide

(To remove impurities)
Sodium aluminate

Precipitated from aluminate

solution
Aluminum hydroxide

Thickened and calcined

Aluminum oxide, Al203

Dissolved in molten bath of

cryolite (Na3A1F6) at 940°C -
980°C and this mixture is
electrolyzed in electrolytic cell
Aluminum

Figure 2.1: Bayer process - Aluminum production

 7

Aluminum metal forms at the cathode (negative pole), while oxygen is

released at the anode (positive pole). The production process consumes a great deal
of electricity which leads to the high cost of aluminium.

2.1.3 Wrought Aluminum Alloys series

An alloy is composed of two or more chemical elements, at least one of

which is metal. Aluminum alloys produced in the wrought form such as sheet, plate,
extrusions, rod and wire are classified according to the major alloying element they
contain. A four digit numerical designation is used to identify aluminum wrought
alloys. The first digit indicates the alloy group that contains specific alloying
elements. The second digit indicates modification of the original alloy or impurity
limits. The last two digits identify the aluminum alloy or indicate the aluminum
purity.

Table 2.1: A four digit numerical designation is used to identify aluminum wrought
alloys. (Source: Handbook of Aluminium, Marcel Dekker.Inc)

Alloying elements

lxxx series Pure aluminum with a minimum 99% aluminum content by

weight and can be work hardened

2 xxx series Copper, high strength to weight ratio; low resistance to

corrosion

3 xxx series I Manganese, and can be work hardened

4 xxx series I Silicon, lower melting point

5 xxx series Magnesium, derives most of their strength from solution

hardening.

6 xxx series Magnesium and silicon, are easy to machine, and can be
precipitation hardened, but not to the high strengths that 2000,
5000 and 7000

7 xxx series Zinc, and can be precipitation hardened to the highest

strengths of any aluminum alloy

8 xxx series Miscellaneous category (other element)

 8

2.1.4 Basic temper designations

Aluminium and aluminium alloy products are identified by various

designation systems, standards, and specifications. Aluminium products are covered
by standards produced by American Society for Testing and Materials, the Society of
Automotive Engineers, and the Aerospace Materials Specification.

Wrought and cast aluminium alloys are identified by various assignation

systems, which include the Aluminium Association (AA) numbering system and
Unified Numbering System for metals and alloys. Aluminium Association
designation for wrought aluminium alloys consist of four digits as indicated in Table
2.1.

Temper designations are letters that indicate the final condition of cold
worked (H) or heat treated (1) material. The temperature designation is separated
from the alloy with a hyphen. For example, 3003-H2 designates a quarter hard
aluminium manganese alloys, and a 2014 —T4 designates an aluminium copper alloy
that is solution treated, quenched and allowed to age at room temperature.

The Unified Numbering System for metals and alloys identifies wrought and
cast aluminium alloys with the uppercase letter A followed by five numbers that
identify a composition range for a specific alloy. For wrought aluminium alloys, the
first number is 9 followed by the Aluminium Association number for the alloy. For
example, alloy 3003 is equivalent to UNS A93003.
Table 2.2: Temper designations that are used to indicate cold worked or heat treated
aluminium alloy (Source: Metallurgy, B.J. Moniz, Alp)

Designation Condition

F As fabricated
0 Annealed and reciystallized(from cold worked or cast state)
HI Strain hardened only
H2 Strain hardened and partially annealed
H3 Strain hardened and thermally stabilized
W Solution heat treated
TI Cooled from elevated temperature shaping process, and
naturally aged
T2 Cooled from elevated temperature shaping process, cold
worked and naturally aged
T3 Solution heat treated, cold worked, and naturally aged
T4 Solution heat treated and naturally aged
T5 Cooled from an elevated temperature shaping process and
T6 then artificially aged
T7 Solution heat treated and then artificially aged
T8 Solution heat treated and stabilized
T9 Solution heat treated, cold worked and artificially aged
TIO Solution heat treated, artificially aged, and then cold worked
Cooled from elevated temperature shaping process, cold
worked and then artificially aged.
 10

2.1.5 Non heat treatable and heat treatable wrought aluminum alloys

Wrought aluminum alloys can be divided into two groups; non heat treatable
and heat treatable alloys. Non heat treatable aluminum alloys cannot be precipitation
strengthened but only can be cold worked to increase their strength. Three main
groups of this type are lxxx, 3xxx and Sxxx series. Cold work is the plastic
deformation which is carried out in a temperature region and over a time interval. In
the early stage of plastic deformation, slip is essentially on primary glide planes and
the dislocations from coplanar arrays. As deformation proceeds cross slip takes place.
this increases the strength of the material. Magnesium is the principal alloying
element in 5xxx series aluminum alloy and is added for solid solution strengthening
in amounts up to about 5 %( Source: Foundation of Material Science, McGraw Hill).
Some aluminum alloy can be precipitation strengthened by heat treatment (heat
treatable). These series are 2xxx, 6xxx and 7xxx.

2.1.6 Wrought Al - Mg alloys

Work-hardening wrought Al-Mg alloys which are also known commercially

as the Sxxx series aluminium-based alloys are currently being used as automotive
BIW material. Magnesium is the principal alloying element and is added for solid-
solution strengthening. Generally Al-Mg alloys used in B1W applications have very
good formability; relatively low yield stress and work harden during cold working.
Alloy grades that have been used extensively as automotive BIW material are listed
in Table 2.3. Nominal values of their mechanical properties are shown in Table 2.4.
The alloys are supplied to the BIW press shop in an annealed temper, designated as -
0 temper.
 11

Table 2.3.: Composition of commonly used Al-Mg alloys used for automotive BIW
components in weight percent with Al as remainder (Source: Handbook of
Aluminium; Alloy production and Materials manufacturing)

Alloy Mg Si Cu Fe Mn Zn Cr Ti
5251 1.7-2.4 0.40 0.15 0.50 0.10-0.50 0.15 0.15 0.15
5052 2.2-2.8 0.25 0.10 0.40 0.10 0.10 0.15-0.35 -
5754 2.6-3.6 0.40 0.10 0.40 0.50 0.20 0.30 0.15
5182 4.0-5.0 0.20 0.15 0.35 0.20-0.50 0.25 0.10 0.10
5083 4.0-4.9 0.40 0.10 0.40 0.40-1.00 0.25 0.05-0.25 0.15

Table 2.4.: Mechanical properties of commonly used Al-Mg alloys used for
automotive BIW components (Source: Handbook of Aluminium; Alloy production
and Materials manufacturing)

Alloy Yield stress, Ultimate Tensile Strength Maximum

0.2% (MPa) (UTS) (MPa) Elongation %

5251 80 180 25
5052 90 195 24
5754 100 215 24
5182 135 290 22
5083 145 300 22
 12

2.2. Grain, grain boundaries, and grain size

2.2.1 Structure of metals

Metal structure is the arrangement of atoms within metals. The arrangement

influences the behavior and properties of certain metal. Others that influence
properties and behavior of metal are composition of the metal, impurities and
vacancies, grain size, grain boundaries, and environment.

Solidification Single crystal I

Liquid metUnit cell Crystal

Polycrystals

Figure 2.2: The flow of crystal production.

 13

2.2.2 Crystal structure of metals

When metals solidify from a molten state, the atoms arrange themselves into
various orderly configurations, called crystals. The arrangement of atoms within the
crystal is called crystalline structure. Crystal structure is the configurations of atoms
as they add to one another in an orderly and repeating three dimensional pattern.
Amorphous solids are solid that do not exhibit a crystal structure. They posses the
random arrangement that commonly occur in liquids. Examples of these are nickel-
zirconium and molybdenum-rhenium.

Crystal structure may be present with any of the four types of bonding which
is metallic, covalent, and ionic or Van de Waals bonding. A space lattice and unit
cell help to illustrate crystal structures. A space lattice is a regular array of points
produced by lines connected through the points. A unit cell is the smallest
arrangement of atoms tat repeats itself through the space lattice. As the number of
atoms per lattice increases, the unit cell becomes more complex.

Although 14 types of unit cell types are possible, most metal exhibit one of
three types. The three basic atomic arrangements are as shown in Table 2.5.