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Magnesium Forged Components

for Structural Lightweight Transport


Applications

Contract #: COLL-CT-2006-030208
Document type: Deliverable report
Title: Deliverable D5.1.7; Quality assurance of magnesium forgings
Deliverable D5.2.3; Micro-structural and mechanical testing
Author Gabriela Popescu (UPB)
Issued by: I. Bădoi (INTEC; WP5 leader)
Dissemination level: RE

Collective Research Project funded by the European Community within the Framework of the
Specific Research and Technological Development Programme “Integrating and Strengthening
the European Research Area” (Sixth Framework Programme 2002–2006)
TABLE OF CONTENTS

1. Introduction to forgings quality of wrought magnesium alloy-extruded bar AZ80 T5


2. General process variables that influence 4.1. Verification/Determination of characteristic
forgings quality: the microstructure and curve to traction test of extruded bar AZ80 T5
mechanical properties 4.2. Verification/determination of mechanical and
2.1. Forging process variable: Billet quality elastic properties of extruded bar AZ80 T5
2.2. Forging process variable: Dies quality and 4.3. Compression test for verification/ determination
conditions at the die/billet interface the Ultimate strength of extruded bar AZ80 T5
2.3. Deformation zone and suitability equipment 5. Case study: Determination of mechanical
3. Technical conditions and applicable standards properties of die-closed forged component Fork
for quality assurance of wrought magnesium link (LEIBER)
alloys and quality assurance of forgings 5.1. Specimens/samples machining for determi-
3.1. Quality Conditions regarding to chemical nation the mechanical properties of Die-closed
composition of wrought magnesium alloys forged component Fork link (LEIBER)
3.2. Quality conditions regarding to physical 5.2. Determination of the mechanical properties of
properties of wrought magnesium alloys forged component Fork link (LEIBER)
3.3. Quality conditions regarding to mechanical 5.3. Analysis/evaluation of mechanical properties of
properties of AZ wrought magnesium alloys forged component Fork link (LEIBER)
3.4. Quality conditions regarding to mechanical 6. Case study: Determination of mechanical
properties of ZK wrought magnesium alloys properties of die-closed forged Shock absorber
head (INOFER)
4. Case study: Machining of test samples and veri- 6.1. Determination of YTS/UTS properties of forged
fication/ determination the mechanical properties component Shock absorber head (INOFER)
TABLE OF CONTENTS
6.2. Determination of elongation properties of forged the crack
component Shock absorber head (INOFER) 11.4. Case study: High forging temperature and the
7. Comparation of strength properties of cracks developing along the shear bands
ZK30,ZK60 and AZ80 forged magnesium alloys 12. Case study: Microstructure of AZ80 magnesium
8. Comparation of elongation properties of forged component. Fork link (LEIBER)
ZK30,ZK60 and AZ80 magnesium alloys 13. Microstructure pre-extruded bar of modified
9. Hardness and micro-hardness of the forged and ZK60 magnesium alloy
heat-treated parts 14. Microstructure of the cast AZ80 modified alloys
10. The metallographic examination of magnesium 15. Microstructure of the cast ZK60 modified alloys
alloys
16. Microstructures of the extruded AZ80 modified
10.1. The methods of etching alloys
11. Case study: Microstructure of AZ80 magnesium 17. Microstructures of the extruded ZK60 modified
alloy extruded bar and Shock absorber head alloys
(INOFER)
11.1. Case study: Influence of temperature on 18. Microstructure analysis of the extruded
internal cracks of manganese-rich phase and modified alloys
matrix of the Shock absorber head 19. Influence of heat treatment on microstructure of
11.2. Case study: Forging to high temperature and extruded and forged magnesium alloys
trans-crystalline crack in Shock absorber head 19.1. Recommended practice for heat treatment of
11.3. Case study: Phase distribution in the vicinity of magnesium forging alloys
TABLE OF CONTENTS

20. Influence of T5 heat treatment on microstructure of heat treatment T4/2 h and 4h @ 420C-individual
AZ80 forged bicycle part (LEIBER) grain size
21. Influence of T5 heat treatment on microstructure of 30. Grain size in modified AZ80-T4 alloys heat
ZK60 forged ring treatment T4/2h and 4h @ 420C
22. Influence of heat treatment on microstructure of 31. SEM microstructures and EDS analysis of AZ80-
extruded bar ZK+0,5 RE modified alloy T4 alloy. Heat treatment T4/2h @ 420C
23. SEM microstructures and EDS analysis of the 32. SEM microstructures and EDS analysis of az80-
az80 forged ring t4 alloy. Heat treatment T4/4h @ 420C
24. SEM microstructures and EDS analysis of the 33. SEM and EDS analysis of the modified ZK60
zk60 forged ring in T5 condition alloys
25. SEM microstructures and EDS analysis of white 34. Optical microstructures of ZK60 modified alloy,
particles of the AZ80 forged bicycle part heat treatment T6 individual grain size
26. SEM microstructures and EDS analysis of the 35. Optical microstructures of ZK60 alloy, modified
AZ80 forged ring with different quantities of RE. Heat treatment T6
27. SEM microstructures and EDS analysis of the 36. SEM and EDS analysis of the modified ZK60
ZK60 heat-treatment T/24 h @ 150°C alloys. Heat treatment T6/2 h @ 480C
28. SEM micrographs of extruded modified AZ80 37. Conclusions
alloys untreated and unetched 38. References
29. Optical microstructures of AZ80 modified alloy,
1. INTRODUCTION TO FORGINGS QUALITY

Forging offers potential savings in energy and material, especially in


medium and large production quantities, where tool costs can be easily
amortized.
Quality assurance of magnesium forgings is major influenced by quality
of wrought magnesium alloys, the technical level of technologies,
suitability of equipments and repeatability of technological parameters.
Magnesium parts produced by forging exhibit better mechanical and
metallurgical properties and reliability than do those manufactured by
casting or machining.
The magnesium alloys flow, the friction at the tool/material interface, the
heat generation and transfer during plastic flow, and the relationships
between microstructure/ properties and process conditions are difficult
to predict.
1. INTRODUCTION TO FORGINGS QUALITY

The key to a successful forging operation, to obtaining the desired


shape and properties and adequate quality of forgings is the
understanding and control of the metal flow in conditions of
magnesium anisotropy.
The direction of metal flow, the magnitude of deformation, and the
temperatures involved greatly influence the properties of the
formed components and forgings quality.
Metal flow determines both the mechanical properties related to
local deformation and the formation of defects such as cracks and
folds at or below the surface.
2. GENERAL PROCESS VARIABLES THAT INFLUENCE FORGINGS
QUALITY: THE MICROSTRUCTURE AND MECHANICAL PROPERTIES

The macro and micro-geometry, microstructure and mechanical properties of the


product, dimensions and surface finish, are influenced by the following process
variables:
 Billet-Tooling/Dies
 Conditions at the Die/Billet Interface
 Deformation Zone
 Equipment
The processing conditions (temperature, strain, strain rate) determine the micro-
structural variations taking place during deformation and often influence the final
product properties.
A realistic systems approach must include consideration of
(a) the relationships between properties and microstructure of the formed
material
(b) the quantitative influences of process conditions and heat treatment
schedules on micro-structural variations.
2.1. FORGING PROCESS VARIABLE:
BILLET QUALITY

Quality of initial conditions: composition, temperature and


history/prestrain.
Plastic anisotropy.
Billet size and thickness.
Flow stress as a function of chemical composition, metallurgical
structure, grain size, segregation, prior strain history, temperature of
deformation, degree of deformation or strain, and rate of deformation
or strain rate, and microstructure.
Forgeability as a function of strain rate, temperature, deformation rate.
Surface texture.
Thermal/physical properties (density, melting point, specific heat,
thermal conductivity and expansion, resistance to corrosion and
oxidation.
2.2. FORGING PROCESS VARIABLE:
DIES QUALITY AND CONDITIONS AT THE DIE/BILLET INTERFACE

Dies:
» Quality of tool geometry
» Surface conditions, lubrication
» Material/heat treatment/hardness
» Heating temperature

Die/Billet Interface:
» Lubricant type and temperature
» Insulation and cooling characteristics of the interface layer
» Lubricate and frictional shear stress
» Characteristics related to lubricant application and removal
2.3. DEFORMATION ZONE AND SUITABILITY EQUIPMENT

Deformation zone:
» The mechanism/mechanics deformation of wrought magnesium
alloys (slipping, twining)
» Metal flow, velocities, strain, strain rate (kinematics)
» Stresses (variation during deformation)
» Temperatures (heat generation and transfer)

Equipment:
» Speed/production rate
» Force/energy capabilities
» Rigidity and accuracy
3. TECHNICAL CONDITIONS AND APPLICABLE STANDARDS FOR
QUALITY ASSURANCE OF WROUGHT MAGNESIUM ALLOYS AND
QUALITY ASSURANCE OF FORGINGS

Applicable standards for verification and determination of the mechanical properties of


feedstock-wrought magnesium alloys and forgings:
DIN EN Magnesium alloy ingots and castings
1753:1997
ISO/FDIS Magnesium and magnesium alloys – wrought
3116:2007(E) magnesium alloys
DIN 9715:1982 Magnesium semi-finished products; Properties
ASTM Specification for Magnesium-Alloy Extruded Bars,
B107/B107M Rods, Profiles, Tubes, and Wire
ASTM B91 Specification for Magnesium-Alloy Forging
SAE J 466-1989 Magnesium Wrought Alloys
(SAE J466-1989)
3. TECHNICAL CONDITIONS AND APPLICABLE STANDARDS FOR QUALITY ASSURANCE OF
WROUGHT MAGNESIUM ALLOYS AND QUALITY ASSURANCE OF FORGINGS

ASTM B557-06 Standard Test Methods for Tension Testing


Wrought and Cast Aluminium and Magnesium-Alloy
Products
ASTM E8M-04 Standard Test Method for Tension Testing of
Metallic Materials [Metric]
ISO 6892 Tensile tests
ISO 31-0:1992 International standard of rounding of numbers
ASTM E 10 Standard Test Method for Brinell hardness of
Metallic Materials
ASTM E 21 Standard Test Method for Elevated Temperature
Tension Tests of Metallic Materials
ASTM E 23 Standard Test Method for Notched Bar Impact
Testing of Metallic Materials
ASTM E4 Practices for Force Verification of Testing Machines
3.1. QUALITY CONDITION REGARDING CHEMICAL COMPOSITION OF
WROUGHT MAGNESIUM ALLOYS
The chemical composition of wrought magnesium alloys/magnesium forgings will be in
accordance with ISO/FDIS 3116:2007(E) or ASTM E35 Test Methods for Chemical
Analysis of Magnesium and Magnesium Alloys
[%]
Magnesium
Al Zn Ca Cu Fe Mn Ni Si Zr Mg
alloy
2.50 ÷ 0.60 ÷ < max. max.
AZ31B < 0.040 < 0.050 0.0050 - 97
3.50 1.40 0.0050 0.20 0.10
5.80 ÷ 0.40 ÷ < max. max.
AZ61A - < 0.050 0.0050 - 92
7.20 1.50 0.0050 0.15 0.10
7.80 ÷ 0.20 ÷ < max. max.
AZ80A - < 0.050 0.0050 - 91
9.20 0.80 0.0050 0.12 0.10

ZK31 - 3.0 - - - - - - 0.60 96.4

5.50 ÷ max. max. 0.60 ÷


ZK61A - - - - 93.2
6.50 0.10 0.010 1.00

4.80 ÷ max.
ZK60A - - - - - - 94
6.20 0.45
3.2. QUALITY CONDITION REGARDING TO PHYSICAL PROPERTIES OF
WROUGHT MAGNESIUM ALLOYS
The physical properties of wrought magnesium alloys will be in accordance with
ISO/FDIS 3116:2007(E) and are presented in the below table
Minimum physical properties of wrought magnesium alloys
Coefficient of
Thermal Electrical Specific heat
Specific thermal
conductivity resistivity Jkg-1K-1
Alloy gravity expansion
-6 -1 Wm-1K-1 n m (200C to
(200C) 10 K
0 0 (200C) (200C) 2000C)
(20 C to 200 C)
AZ31 1.77 26.0 96 100 1040

AZ61 1.80 27.3 79 143 1000

AZ80 1.80 26.0 78 145 1050

ZK30 1.80 27.1 125 70 960

ZK60 - - - - -
3.3. QUALITY CONDITION REGARDING TO MECHANICAL PROPERTIES
OF AZ WROUGHT MAGNESIUM ALLOYS
Mechanical properties of AZ wrought magnesium alloys will be in accordance with values
presented below tables
Mechanical properties of AZ61; Alloy ISO-MgAl6Zn1

0.2% Proof stress,


Thickness Tensile strength, Rm Elongation, A
Temper Rp0,2
(mm) (N/mm2), min (%), min
(N/mm2), min

Bars and solid sections t = D for solid round bars

1 ≤ t ≤ 10 260 160 6
F 10 < t ≤ 40 270 180 10
40 < t ≤ 65 260 160 10

Forgings

F All 270 152 6

Note: Values for separately forged test pieces must be agreed between the manufacturer and customer
3.3. QUALITY CONDITION REGARDING TO MECHANICAL PROPERTIES OF AZ
WROUGHT MAGNESIUM ALLOYS

Mechanical properties of AZ80; Alloy ISO-MgAl8Zn

0.2% Proof stress,


Thickness Tensile strength, Rm Elongation, A
Temper Rp0,2
(mm) (N/mm2), min (%), min
(N/mm2), min

Bars and solid sections t =D for solid round bars


t ≤ 40 295 195 10
F 40 < t ≤ 60 295 195 8
60t ≤ 130 290 185 8
t ≤6 325 205 4
T5* 6 < t ≤ 60 330 230 4
60t ≤ 130 310 205 2
Forgings
F All 290 200 6
Note: Values for separately forged test pieces must be agreed between the manufacturer and customer
* Conditions of heat treatment for T5 temper are presented in table
3.4. QUALITY CONDITION REGARDING TO MECHANICAL PROPERTIES
OF ZK WROUGHT MAGNESIUM ALLOYS
Mechanical properties of ZK wrought magnesium alloys will be in accordance with values
presented below tables
Mechanical properties of ZK30; Alloy ISO-MgZn3Zr
0.2% Proof stress,
Thickness Tensile strength, Rm Elongation, A
Temper Rp0,2
(mm) (N/mm2), min (%), min
(N/mm2), min
Bars and solid sections t = D for solid round bars
t ≤ 10 870 200 8
F
10 < t ≤ 100 300 225 4

T5* All 275 255 4

Forgings

F All 290 205 7

Note: Values for separately forged test pieces must be agreed between the manufacturer and customer
* Conditions of heat treatment for T5 temper are presented in table
3.4. QUALITY CONDITION REGARDING TO MECHANICAL PROPERTIES OF ZK
WROUGHT MAGNESIUM ALLOYS

Mechanical properties of ZK60; Alloy ISO-MgZn6Zr

0.2% Proof stress,


Thickness Tensile strength, Rm Elongation, A
Temper Rp0,2
(mm) (N/mm2), min (%), min
(N/mm2), min

Bars and solid sections t =D for solid round bars

F t ≤ 50 300 210 5

T5* t ≤ 50 310 230 5

Forgings

T5* t ≤ 75 290 180 7

T6* t ≤ 75 295 220 4

Note: Values for separately forged test pieces must be agreed between the manufacturer and customer
* Conditions of heat treatment for T5 temper are presented in table
4. CASE STUDY:MACHINING OF TEST SAMPLES AND
VERIFICATION/DETERMINATION THE MECHANICAL PROPERTIES OF
WROUGHT MAGNESIUM ALLOY-EXTRUDED BAR AZ80 T5

 If the pre-extruded magnesium bars not are accompanied by


documents of mechanical tests, before the closed-die forging
of components, producer of magnesium forgings will proceed
to determine of the mechanical properties.
 Case study: pre-extruded bar Ø28 mm AZ80 T5 of which
were machined out five specimens with shape and
dimensions presented below.

Applicable standards:

 ASTM B557-06: Standard Test Methods for Tension Testing


Wrought and Cast Aluminum and Magnesium-Alloy Products;
 ASTM E8M-04: Standard Test Method for Tension Testing of
Metallic Materials [Metric].
4. CASE STUDY: MACHINING OF TEST SAMPLES AND
VERIFICATION/DETERMINATION THE MECHANICAL PROPERTIES OF
WROUGHT MAGNESIUM ALLOY-EXTRUDED BAR AZ80 T5

Normal Proportional specimens of smaller


Dimensions specimens dimensions
Dimensions, mm
D 12.5 9 6 4
L0 50 36 24 16
L 58 44 32 19
R 9 6 5 4
Dl (min) 19 13.5 9 6
4.1. VERIFICATION/DETERMINATION OF CHARACTERISTIC CURVE
TO TRACTION TEST OF EXTRUDED BAR AZ80 T5

Material feedstock: pre-extruded bar AZ80 T5/Ø28 mm


4.2. VERIFICATION/DETERMINATION OF MECHANICAL AND ELASTIC PROPERTIES
OF EXTRUDED BAR AZ80 T5

Material feedstock:
pre-extruded bar Ø28 mm
4.3. COMPRESSION TEST FOR VERIFICATION/DETERMINATION THE ULTIMATE
STRENGTH OF EXTRUDED BAR AZ80 T5

Material feedstock: pre-extruded bar AZ80 T5 Ø28 mm


5. CASE STUDY: DETERMINATION OF MECHANICAL PROPERTIES OF
DIE-CLOSED FORGED COMPONENT FORK LINK (LEIBER)
Die-closed forging data:
Equipments:
» screw press (440 t); estimated ram speed: vR≈0.45−0.5 m/s
» slug heating in gas furnace; direct flame
» production forging die (#5054), normally used for EN AW 6082; pre-heating by torch
» miscellaneous: temperature measurements by IR radiation pyrometer
(range 260−600⁰C) or contact thermometer
Feedstock: AZ80-T5 (Ø30×50 mm) with additional heat treatment (2h/430⁰C, cooling
in ambient air)
Forging conditions:
» one forging stroke
» lubricant Acheson ADS72-2 (graphite-based compound, alu pigmented)
» tooling temperature range 85−180⁰C
» slug temperature range 180−340⁰C
Current alloy/temper: aluminum EN AW 6082-T6
5.1. SPECIMENS/SAMPLES MACHINING FOR DETERMINATION THE MECHANICAL
PROPERTIES OF DIE-CLOSED FORGED COMPONENT FORK LINK (LEIBER)

Machining scheme for test samples out of forged components will comply
with technical documentation

Mechanical evaluation:
machining of tensile test bars from the samples
5.2. DETERMINATION OF THE MECHANICAL PROPERTIES OF FORGED COMPONENT
FORK LINK (LEIBER)

Tensile testing properties of the forged parts


5.3. ANALYSIS/EVALUATION OF MECHANICAL PROPERTIES OF FORGED
COMPONENT FORK LINK (LEIBER)

The aluminum reference alloy for this component is EN AW6082


Standards for this alloy prescribe a minimum yield stress of
YS=260 MPa, a minimum ultimate tensile strength of UTS=310
MPa and a minimum elongation of 6% for forged parts
The results show that the ultimate tensile strength and
elongation of forged AZ80 exceed these requirements for the
longitudinal as well as for the transverse direction
The yield stress, however, does not meet this requirement and
especially for the transverse direction is notably lower
Literature data for the longitudinal tensile properties of AZ80A-
F forgings at room temperature are as follows: typical yield
stress YS=215 MPa, typical ultimate tensile strength UTS=315
MPa and typical elongation of 8% (minimum values: 180 MPa,
290 MPa and 5%, respectively
The results exceed these values
6. CASE STUDY: DETERMINATION OF MECHANICAL PROPERTIES OF
DIE-CLOSED FORGED SHOCK ABSORBER HEAD (INOFER)
Die-closed forging data:
Equipments:
» screw press (550 t); estimated ram speed: vR≈0.45−0.5 m/s
» slug heating in gas furnace; direct flame
» production forging die (#5054), normally used for EN AW 6082; pre-heating by torch
» miscellaneous: temperature measurements by IR radiation pyrometer
(range 260−600⁰C) or contact thermometer
Feedstock: AZ80-T5 (Ø47×140 mm) with additional heat treatment (2h/430⁰C, cooling
in ambient air)
Forging conditions:
» one forging stroke
» lubricant Acheson ADS72-2 (graphite-based compound, alu pigmented)
» tooling temperature range 85−180⁰C
» slug temperature range 180−340⁰C
Current alloy/temper: aluminum EN AW 6082-T6
6.1. DETERMINATION OF YTS/UTS PROPERTIES OF FORGED COMPONENT
SHOCK ABSORBER HEAD (INOFER)

Influence of slug temperature on strength properties of forged component


6.2. DETERMINATION OF ELONGATION PROPERTIES OF FORGED COMPONENT
SHOCK ABSORBER HEAD (INOFER)

Influence of slug temperature on elongation properties of forged component


7. COMPARATION OF STRENGHT PROPERTIES OF
ZK30, ZK60 AND AZ80 FORGED MAGNESIUM ALLOYS
Influence of slug temperature on elongation properties of forged component
8. COMPARATION OF ELONGATION PROPERTIES OF
ZK30, ZK60 AND AZ80 FORGED MAGNESIUM ALLOYS
Influence of slug temperature on elongation properties of forged component
9. HARDNESS AND MICRO-HARDNESS OF
THE FORGED AND HEAT-TREATED PARTS

MICRO-HARDNESS
ALLOY/PART TREATMENT HARDNESS
Transversal Longitudinal
Untreated – 33 33
AZ80 18 h @ 180 C – 110 114
LEIBER part 21 h @ 180 C – 112 110
24 h @ 180 C – 109 111
Untreated 258 83 96
18 h @ 180 C 270 112 98
AZ80
TNO ring 21 h @ 180 C 258 114 98
24 h @ 180 C 219 95 98
Untreated 212 67 71
18 h @ 150 C 223 104 101
ZK60
TNO ring 21 h @ 150 C 228 89 107
24 h @ 150 C 232 – –
10. THE METALLOGRAPHIC EXAMINATION OF MAGNESIUM ALLOYS
Specimen Preparation
In general specimens of magnesium alloys are normally prepared
metallographic in the same way as specimens of aluminium or
steel, but a number of particular points must be taken into account
Cutting: ensure good cooling and use low cutting speed
Mounting: use cold mounting; temperatures in excess of 150ºC can
cause micro-structural changes to occur which may produce
erroneous results.
Grinding: 320 to 1200 grade papers; ≈ 90 s; 300 rpm; 6-8 N/specimen;
intermediate rinsing with water; the reaction of the water with the
surface of the specimen is not significant at this stage in the
preparation;
as magnesium is a relatively soft metal the grinding process should
be started on as fine a grade of paper as possible;
10. THE METALLOGRAPHIC EXAMINATION OF MAGNESIUM ALLOYS

in the case of fully automated grinding good results can be achieved


using a maximum specimen; grinding with 1200 and 2400 grade
papers and Ethanol; intermediate rinsing with Ethanol.
Polishing: Diamond suspension (not water based), diamond lubricant
(not water based), 4 - 5 min., 250 - 300 rpm; available diamond
abrasive suspensions (3 μm and 1 μm); Ethanol should also be
used for the fine polishing operation using an oxide polishing
suspension (OPS neutral).
Etching: The specimens can be etched with a number of different etching
solutions. The specimens are then rinsed with Ethanol and
immediately dried with dry compressed air or hot air.
10.1. THE METHODS OF ETCHING

Nital 1–8% (Nitric acid solution) / Hydrofluoric acid solution /


Etchant: 100 ml Ethanol 98%+1-8 ml Etchant: 90 ml distilled water+10 ml
Nitric acid 65%; Hydrofluoric acid;
Etching time: 1 to 5 min; Etching time: 3 – 60 s;
Effect: Forms an etch film, no Effect: Intermetalic Mg17Al12 phase
microstructure apparent, intermediate attacked.
polishing produced no improvement.
Oxalic acid solution 2-10% /
Etchant: 100 ml distilled water+2-10 g
Picric acid solution for micro-etching / Oxalic acid;
Etchant: 100 ml Ethanol+18 ml distilled Etching time: 6 to 10 s;
water+6 ml Glacial acetic acid+12 g Picric Effect: Grain boundaries etched.
acid 98%;
Etching time: 20 - 25 s;
Picric acid/ Etchant:100 ml distilled
Effect: Etchant for as-cast and wrought
water+100 ml Ethanol+5 g Picric acid;
Magnesium alloys, and pure Magnesium;
Etching time: 30 s;
reveals the microstructure of the metal
Effect: Grain boundaries visible, etch
(grain boundaries and twinning.
film or slightly milky surface remains.
11. CASE STUDY:MICROSTRUCTURE OF AZ80 MAGNESIUM ALLOY
EXTRUDED BAR AND SHOCK ABSORBER HEAD (INOFER)
Pre-extruded slugs (AZ80, Ø45 mm):
influence of heat treatment on microstructure

Process windows (AZ80):


influence of slug temperature on microstructure
11.1. CASE STUDY: INFLUENCE OF TEMPERATURE ON INTERNAL CRACKS OF
MANGANESE-RICH PHASE AND MATRIX OF THE SHOCK ABSORBER HEAD
11.2. CASE STUDY: FORGING TO HIGH TEMPERATURE AND TRANS-CRYSTALLINE
CRACK IN SHOCK ABSORBER HEAD
11.3. CASE STUDY: PHASE DISTRIBUTION IN THE VICINITY OF THE CRACK
11.4. CASE STUDY: HIGH FORGING TEMPERATURE AND THE CRACKS
DEVELOPING ALONG THE SHEAR BANDS
12. CASE STUDY: MICROSTRUCTURE OF AZ80 MAGNESIUM
FORGED COMPONENT FORK LINK (LEIBER)
13. MICROSTRUCTURE PRE-EXTRUDED BAR OF MODIFIED ZK60
MAGNESIUM ALLOY

Pre-extruded slugs (ZK60, Ø240 mm): cross-sectional differences in microstructure

Initial condition:T5 (T=177oC/16-24) After heat treatment: 400o C /2h


After heat treatment : 400o C /3h After heat treatment: 400o C /6h
14. MICROSTRUCTURE OF THE CAST AZ80 MODIFIED ALLOYS
15. MICROSTRUCTURE OF THE CAST ZK60 MODIFIED ALLOYS
16. MICROSTRUCTURE OF THE EXTRUDED AZ80 MODIFIED ALLOYS
17. MICROSTRUCTURE OF THE EXTRUDED ZK60 MODIFIED ALLOYS
18. MICROSTRUCTURE ANALYSIS OF THE
EXTRUDED MODIFIED ALLOYS

The microstructures of the modified alloys AZ80+0.5 RE and


AZ80+0.7 RE look similar and the grain sizes of 12 and 14
µm were also quite similar
The microstructure of the AZ80+0.7 RE+0.6 Y is more
inhomogeneous than microstructure of the alloys AZ80+0.5
RE and AZ80+0.7 RE
In contrast to the AZ80 alloys, the modified ZK60 alloys is
more inhomogeneous
In micrographs of ZK60+0.5 RE and ZK60+0.7 RE inhomogeneous
microstructures are grains with a wide variation of sizes; very small
grains with 2–4 µm coexist with large un-recrystallized grains
The average grain size of the modified alloy ZK60 + 0.5 RE
is about 13 µm and 18 µm for ZK60 + 0.7 RE alloy
19. INFLUENCE OF HEAT TREATMENT ON MICROSTRUCTURE OF
EXTRUDED AND FORGED MAGNESIUM ALLOYS

Solution heat treatment consists in heating the magnesium alloy


to a temperature at which certain constituents go into solution and
then quenching so as the hold these constituents in solution during
the cooling
Quenching is done in still or moving air, liquids not
ordinarily being used. It gives maximum hardness and yield
strength, but sacrifice toughness
Generally solution heat treatment lies between 340–565°C,
and exposure time may be from 16 to 24 hours
Stabilization is used mainly for the purpose of preventing or
minimizing the growth of grain size in service at elevated
temperatures. The stabilization treatment produces much or most
coalescence of constitutes precipitated form of solid solution
19. INFLUENCE OF HEAT TREATMENT ON MICROSTRUCTURE OF EXTRUDED AND
FORGED MAGNESIUM ALLOYS

Precipitation or ageing treatment follows solution heat treatment:


For wrought magnesium alloys, extruded bars and forgings,
result in retaining alloy constituents in solid solution in
concentrations substantially greater than the equilibrium
solubility at the room temperature
Ageing treatment or precipitation consists in heating the
quenched alloy at a moderately elevated temperature to
effect the precipitation of the constituents held in solid
solution
The temperature of treatment may be in the range 150 to
260 °C, with 3 to 16 hours of exposures.
Annealing consists in heating the magnesium alloy at a moderate
temperature to effect recrystallization, agglomerate precipitate, or remove
internal stress
Wrought magnesium alloys in various conditions of strain
hardening or temper can be annealed by being heated at
290 to 455 °C, depending on alloy, for one or more hours
19.1. RECOMMENDED PRACTICE FOR HEAT TREATMENT OF
MAGNESIUM FORGING ALLOYS

Solution heat treatment (T4) of AZ80 magnesium alloy:


- Temperature: 410–425 C
- Time: 2 and 4 hours
- Cooling in air
- Even if the temperature is increased at 540C, the in-
homogeneity will be present
- Hardness can be increased with 20-30%
- Grain size decreases around 35%
- At addition of RE, the microstructures and mechanical
properties can be improved significantly (case of AZ80
modified with 0.7%RE)

Aging treatment (T5) of AZ80 Annealing of AZ80


magnesium alloy: magnesium alloy (F, T5, T6)
- Temperature: 177C Stress relieving in case of - Temperature: 385C
- Time: 16–24 h - Time: 1 h to more hours
AZ80 magnesium alloy
forging (F, T5)
- Temperature: 205C
- Time: 1 h
19.1. RECOMMENDED PRACTICE FOR HEAT TREATMENT OF
MAGNESIUM FORGING ALLOYS

Solution heat treatment (T6) of ZK60 magnesium alloy:


- Temperature: 475–490C
- Time: 4 hours
- Protective atmosphere necessary (used mixture of gases 0.5%
SF6+99.5% Ar)
- Cooling in air
- Aging: 24 h @ 175C
- Hardness can be increased with 15-20%.

Aging treatment (T5) of ZK60 Annealing of ZK60


magnesium alloy: magnesium alloy (F, T5, T6)
- Temperature: 150 C - Temperature: 290 C
- Time: 24 hours. Stress relieving in case of ZK60 - Time: 1 h to more hours
magnesium alloy forging (F, T5)
- Temperature: 150C
- Time: 1 h
20. INFLUENCE T5 HEAT TREATMENT ON MICROSTRUCTURE OF
AZ80 FORGED BICYCLE PART (LEIBER)

(a) (b)

(c) (d)
Optical micrographs of AZ80 forged bicycle part:
(a) as forged; (b) 18 h / 180°C; (c) 21 h / 180°C; (d) 24 h / 180°C (undetached) [20]
21. INFLUENCE T5 HEAT TREATMENT ON MICROSTRUCTURE OF
ZK60 FORGED RING

(a) (b)

(c) (d)
Optical micrographs of ZK60 forged ring:
(a) as forged; (b) 18 h / 150°C; (c) 21 h / 150°C; (d) 24 h / 150°C (etched with 5% Nital solution) [20]
22. INFLUENCE OF HEAT TREATMENT ON MICROSTRUCTURE OF
EXTRUDED BAR ZK + 0.5 RE MODIFIED ALLOY

Initial condition: T5 (T=177oC/16-24 h)

After heat treatment: 400oC/2 h After heat treatment: 400oC/3 h After heat treatment: 400oC/6 h
23. SEM MICROSTRUCTURES AND EDS ANALYSIS OF
THE AZ80 FORGED RING

18 h @ 180 °C 24 h @ 180 °C
24. SEM MICROSTRUCTURES AND EDS ANALYSIS OF
THE ZK60 FORGED RING IN T5 CONDITION

grey particles white particles


25. SEM MICROSTRUCTURES AND EDS ANALYSIS OF WHITE
PARTICLES OF THE AZ80 FORGED BICYCLE PART

18 h@180 °C

24 h@180 °C
26. SEM MICROSTRUCTURES AND EDS ANALYSIS OF WHITE
PARTICLES OF THE AZ80 FORGED RING

18 h@180 °C

24 h@180 °C
27. SEM MICROSTRUCTURES AND EDS ANALYSIS
OF THE AZ80 HEAT TREATMENT T/24h @ 150⁰C

forged bicycle part forged ring


28. SEM MICROGRAPHS OF EXTRUDED MODIFIED AZ80 ALLOYS
UNTREATED AND UNETCHED
MgzAlyMnxCev

MgzAlyZnΣREv
Mg32(Al,Zn)49 at
Zn/Al>1/3

AZ80 + 0.5%RE, white compounds – AZ80 + 0.7%RE, 500x, white and grey
MgzAlyZnxREw compounds on the extrusion direction

Mg

Mg32(Al,Zn)49

AZ80+0.7%RE+0.6%Y, 500 x, rows of white precipitates on


the extrusion direction and compounds Mg32(Al,Zn)49
29. OPTICAL MICROSTRUCTURES OF AZ80 MODIFIED ALLOY,
HEAT TREATMENT T4/2 h AND 4h @ 420C
Heat treatment T4/2 h @ 420C
AZ80 Cer 1 AZ80 Cer 2 AZ80 Cer Y

Heat treatment T4/4 h @ 420C


30. GRAIN SIZE IN MODIFIED AZ80-T4 ALLOY,
HEAT TREATMENT T4/2 h AND 4h @ 420C
31. SEM MICROSTRUCTURES AND EDS ANALYSIS OF
AZ80-T4 ALLOY HEAT TREATMENT T4/2h @ 420C

1 1
2
1 3
2
3
2

AZ80+0.5%Ce AZ80+0.7%Ce AZ80+0.5%Ce+0.6%Y

EDS analysis of white particles in point 2 EDS analysis of white particles in point 1
32. SEM MICROSTRUCTURES AND EDS ANALYSIS OF
AZ80-T4 ALLOY HEAT TREATMENT T4/4h @ 420C

2
1
3
1 1
3 2
2

AZ80+0.5%RE AZ80+0.7%RE AZ80+0.5%RE+0.6%Y

EDS analysis in point 1 – needle particles EDS analysis in point 1 – white particles EDS analysis in point 2 – white particles
33. SEM AND EDS ANALYSIS OF THE MODIFIED ZK60 ALLOYS

needle phases and blocks prismatic phases brittle phases

Mg20Zn5ΣRE

ZK60+0.7%RE ZK60+0.7%RE ZK60+0.7%RE+0.6%Ca


34. OPTICAL MICROSTRUCTURES OF ZK60 MODIFIED ALLOY,
HEAT TREATMENT T6 INDIVIDUAL GRAIN SIZE
ZK60 Cer 1 ZK60 Cer 2 ZK60 CerCa

100x 150x 200x

7,63 7,85
8

7
ASTM E112 Grain Size "G"

5,94
6
5,56

Grain size in modified ZK60-T6


5
4,28
4

3
4,28 alloys heat treated for 2 h @
2 480C in SF6+Ar atmosphere
ZK60-
1 Ca
ZK60-
0 Cer2
ZK60-
Forged Cer1
Heat
treated
35. OPTICAL MICROSTRUCTURES OF ZK60 ALLOY, MODIFIED
WITH DIFFERENT QUANTITIES OF RE.HEAT TREATMENT T6
ZK60 + 0.7 %Ce ZK60 + 0.7 %Ce ZK60 + 0.7%Ce + 0.6%Y
36. SEM AND EDS ANALYSIS OF THE MODIFIED ZK60 ALLOYS
HEAT TREATMENT T6/2 h @ 480

1
1 2

ZK60+0.5%Ce ZK60+0.7%Ce ZK60+0.5%Ce+0.6%Y

Metallic base MgZn; Intergranular compounds; EDS analysis in point 1


EDS analysis in point 1 EDS analysis in point 1
37. CONCLUSIONS
The microstructures of AZ80 and ZK60 magnesium alloys show
homogenous morphology of the secondary phases distributed in
inter-dendritic spacing and along with grain boundary.
Addition of rare earth elements is an effective grain refiner for both
AZ and ZK alloys and improves the microstructure.
The addition of Ce and Y to the AZ80 alloy decreases grain size and
increases dispersed precipitates within the grains.
The addition of rare earth elements and Ca to the ZK60 alloy works
out similarly, with a refining degree almost double and leading to
grain stability at high temperature.
The MgZn2 phase is a strengthening phase, especially in ZK alloys.
Further, the microstructures present phases like MgCaZn or
MgxYyZnz compounds (most probably Mg3Y3Zn3), distributed in
the magnesium matrix.
The microstructures present phases like MgCaZn or MgxYyZnz
compounds (most probably Mg3Y3Zn3), distributed in the
magnesium matrix.
Heat treatment of magnesium alloys results in a homogenization of
cast structures and thus will improve the mechanical properties of
the alloys.
38. REFERENCES

I. Bădoi (INTEC), W.H. Sillekens (TNO); Deliverable D5.1.4; Forging Practice of


Magnesium Alloys, June 1, 2009
I. Bădoi (INTEC), W.H. Sillekens (TNO); Deliverable 5.1.7 Quality assurance of forging
process, June 1, 2009
Gabriela Popescu (UPB); Deliverable D5.7.2; Procedure Quality Assurance of Wrought
Magnesium Alloys CODE MagForge - 01 - QAWMA, September, 2009
T. Pepelnjak (UL–FME), M. Erjavec (UL–FME), G. Popescu (UPB); Deliverable D2.2.1;
constitutive relationships and physical property data for state-of-art feedstock,
February, 2008
W. Sillekens (TNO), G. Kurz (GKSS), B. Clauw (INOFER), G. Cortese (FORGIA), G.
Kemmler (LEIBER), D. Kobold (TECOS), R. Andersson (SVT); Deliverable D 2.3.1 (rev
1), August 2008
W.H. Sillekens (TNO), Forging of Magnesium Alloys: Current Status and Prospects for
Development, Congress Materials Science and Engineering – Symposium Light Metals
2008 DGM MGE presentation.
38. REFERENCES

G. Kurz, D. Letzig (GKSS); Deliverable report/presentation Deliverable D1.1.3, learning


module 1
G. Popescu (UPB); Deliverable D2.4.2 - Heat-treatment procedures for wrought alloys,
December, 2009
G. Popescu (UPB); Deliverable D2.7.2 - Heat-treatment procedures for magnesium
forgings, December, 2009
D. Letzig, G. Kurz (GKSS); Deliverable D1.3.2; Process route for casting, pre-extrusion
and homogenisation of modified feedstock, September, 2009
G. Popescu (UPB), P. Moldovan (UPB), D. Bojin (UPB), W.H. Sillekens (TNO),
Influence of Heat Treatment on Magnesium Alloys Meant to Automotive Industry, UPB
Scientific Bulletin, Series B, vol.71, Issue 2, 2009, p.1454-2331
D. Letzig, G. Kurz (GKSS); Presentation, Progress WP1 “Material development”,
Plenary Meeting, May, 2008

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