Professional Documents
Culture Documents
Submitted by
BACHELOR OF ENGINEERING
in
MECHANICAL ENGINEERING
MARCH 2023
ERODE SENGUNTHAR ENGINEERING COLLEGE
(AUTONOMOUS)
PERUNDURAI, ERODE – 638 057
BONAFIDE CERTIFICATE
SIGNATURE SIGNATURE
Dr. J. Balaji., M.E., Ph.D. Dr. N. Saravanan, M.E., Ph.D.,
SUPERVISOR HEAD OF THE DEPARTMENT
Associate Professor
Department of Mechanical Department of Mechanical
Engineering, Engineering,
Erode Sengunthar Engineering Erode Sengunthar Engineering
College, College,
Perundurai, Perundurai,
Erode-638057. Erode-638057.
42
ABSTRACT
In this study, friction stir welding (FSW) technique was employed for joining AZ31
magnesium plates. Since SiC & Al2O3 particles had been injected along the joint line, AZ31/SiC
& AZ31B/ Al2O3 nano-composite joints was developed in the stir zone (SZ). The SiC and Al 2O3
mean size of the particles are 50 nm and 30 nm were used respectively. Towards this end,
friction stir welding was conducted by using a H13 hardened tool steel with cylindrical threaded
pin profile with tool rotational speed of 1240 rpm and tool travelling speed of 32 mm/min.
At the outset, tensile strength of the joints exhibits 224 MPa and 209 MPa of AZ31B/SiC
and AZ31B/Al2O3 nano composite joints respectively. the fracture morphology was examined in
the nano-composite joints that revealed a brittle fracture mode, which was observed in specimen
AZ31B/Al2O3. On the other hand AZ31B/SiC nano composite joint showed the ductile fracture
mode and hence it will produce more strength when compared to AZ31B/Al2O3 joint.
At the outset, the corrosion results showed better corrosion resistance of the produced
composite welded samples when compare to the AZ31B base metal alloy joints. From this
investigation, a significant enhancement was found in the weld nugget zone that the tensile
strength value was improved for both nano composite joints when compared to without nano
particles addition joint. The micro structure evaluation shows the good accordance with the
produced results.
KEYWORDS:
Friction Stir welding, AZ31B Magnesium alloy, SiC & Al2O3 nano composite, Tensile
Strength, corrosion resistance, Microstructure.
i
ACKNOWLEDGMENT
Behind every achievement lies an unfathomable sea of gratitude to those who actuated
it, without them it would never have into existence. To them we lay the word of gratitude
imprinted within us.
We expressed our sincere thanks to Honorable Founder Udyog Rattan Deiva Thiru.
J.SUDHANANDHEN who have provided excellent facilities for us to complete our project
as successful one.
We wish to express our sincere thanks to Dr.N.SARVANAN, M.E., PH.D Head of the
Department of Mechanical Engineering, for the Continuous help over the period of project work.
We are indebted to our internal guide Dr. J.BALAJI., M.E., PH.D, Asso Professor,
Department of Mechanical Engineering, for his constant help and creative ideas over theperiod
of project work
ii
TABLE OF CONTENT
3 PROPOSED SOLUTION/METHODOLOGY 28
3.1 INTRODUCTION 28
3.2 METHODOLOGY OF WORK
iii 29
3.3 VERTICAL MILLING CENTRE AS FSW MACHINE 30
3.4. WORK MATERIALS INVESTIGATION 31
3.4.1 Magnesium az31b 31
3.4.2. H13 hardened steel 32
3.4.3. Sic nano particle 34
3.5 AZ31B MAGNESIUM PLATE PREPARATON 35
3.5.1. Volume fraction calculation 35
3.5.2. Identifying important parameters 36
3.5.3 Making of volumes in az31b plates 39
3.6 SETTING OF PARAMETERS 40
3.7 CONSTANT WELDED PARAMETER 42
3.8 VARIABLE WELDING PARAMETER 43
3.9 PITTING CORROSION TEST 44
3.10 GENERAL CORROSION TEST 45
4 RESULT 46
4.1 INTRODUCTION MACROSTRUCTURE 46
PROPERTIES
4.2 SPECIMAN PRPARATION 47
4.3 RESULT & DISCUSSION 48
4.4 MICROSTRUCTURE STUDY(AZ31B/SIC) 50
4.5 MICROSTRUCTURE STUDY (AZ31B/ Al2O3) 51
5 STUDY OF PITTING CORROSION PROPERTIES 53
5.1Introduction 53
5.1.1Pitting corrosion properties 53
5.1.2Pitting corrosion test 54
5.2RESULT & DISCUSSION 55
5.2.1Pitting corrosion of az31b/sic 55
5.2.2Pitting corrosion of az31b/ al2o3 56
6 CONCLUSION 58
REFRENCE 60
iii
LIST OF FIGURES
vi
4.3 UNIVERSAL TESTING MACHINE 48
4.4 UTS & POE VALUES OF AZ31B/SIC & AZ31B/ Al2O3 49
4.5 OPTICAL & SEM MICROGRAPH OF AZ31B/SIC 51
4.6 OPTICAL & SEM MICROGRAPH OF AZ31B/ Al2O3 52
4.7 VARIOUS PITTING CORROSION PROFILES 53
4.8 DYNAMIC POLARIZATION CURVES OF FSW BETWEEN 56
AZ31B/SiC
vii
LIST OF TABLES
viii
CHAPTER-1
INTRODUCTION
1.1 INTRODUCTION
Frictions stir welding (FSW), initially developed by The Welding Institute (TWI) in 1991.
Is widely used in welding of magnesium and aluminum alloys .In recent year ,many researches
were carried out on surface composite fabrication with FSP .The surface composite were made
with various base materials and reinforcement .However ,the effect of rotational speed, pin profile
and particle size on surface composites behavior was never studied .In the cast aluminum alloys,
as a similar case, higher tool rotation speed and further FSP passes, were the most effective
parameters to refine coarse particles, heal the casting porosity, and consequently increase strength.
Therefore, with increase of rotation speed, the onion ring spacing reduces and the homogeneity of
stir zone is improved.
The FSW process is entirely solid state, giving it many advantages over conventional
welding process. conventional arc welding techniques all locally liquefy the work piece resulting
in large grain sizes and large residual stresses upon cooling, which greatly degrade material
properties. In addition, arc welding often necessitates the use of a filler material which changes the
joint composition and adds the weight of the filler used to joint.
In order to use FSW in critical components, a full understanding of the properties of friction
stir welds when subjected to static and dynamic loads is necessary. One very common magnesium
alloy that could benefit from use of FSW joints is the AZ31B alloy used in the transportation
industry. FSW offers a cost effective alternative, provided necessary research on FSW joints of
AZ31B is performed.
Friction stir welding (FSW) is a solid state welding process to join materials by
generating frictional heat between a rotating tool and materials being welded. FSW is a process
which involves the joining of metals without using any filler materials. It plasticizes the material
1
using a non-consumable tool which rotates and penetrates into the materials to be welded. The
central pin, followed by the shoulder, is brought into contact with the two parts to be joined as
shown in Figure 1. The material is plasticized by the rotation of the tool which heats the material
as the tool moves along the joint line. The material from the front of the tool is swept around this
plasticized annulus to the rear, the interface. Hence, the welds are created by the combined action
of frictional heating and mechanical deformation due to the rotation of the tool. High temperature
is generated to the order of 0.8 of the melting temperature. The tool consists of a circular section,
and at the end, there is a threaded probe or more complicated flute. This portion of the tool
excluding the probe is known as the shoulder. The probe, or the pin, penetrates the work piece
completely and the shoulder comes into contact with the surface, generating a force and rubbing
the top surface. The friction between the rotating translating tool and the work piece generates
heat. Also, there is adiabatic heating due to the large plastic deformation near the pin.
In FSW the interaction of a non-consumable and rotating tool with the work piece being
welded, creates a welded join through frictional heating and plastic deformation at temperatures
below the melting temperature of the alloys being joined.
2
The conventional joining processes for these alloys include gas metal arc welding
(GMAW), gas tungsten arc welding (GTAW), plasma arc welding (PAW) and electron beam
welding (EBW). However, the strength of joints using the conventional fusion welding only
reaches 50–70% of the parent metal and form flaws such as voids and hot cracks, usually present
in the weld. FSW can avoid these flaws and improve the mechanical properties of joints.
3
FIGURE 1.2 SCHEMATIC DIAGRAM FOR FSP PROCESS
❖ Plunging Stage
❖ Processing Stage
✓ A specially designed non-consumable cylindrical tool is rotated and plunged into the
selected area, to friction process the required location within a plate or sheet
4
✓ Tool has a small diameter pin with concentric larger diameter shoulder
✓ Tool shoulder and length of entry probe control the penetration depth.
✓ When tool descended to the part, the rotating pin contacts the surface, rapidly friction
produced between tool pin and metal surface heats and softens a small column of metal
❖ Plasticizing metal
❖ Transporting metal from the leading face of the pin to its trailing edge
✓ When the shoulder contacts the metal surface, its rotation creates additional frictional heat
and plasticizes a larger cylindrical metal column around the inserted pin.
✓ The shoulder additionally provides a forging force that contains the upward metal flow
caused by the tool pin.
Processing Stage…
✓ During FSP, work piece and the tool are moved relative to each other such that the tool
traverses, with overlapping passes, until the required area is processed.
✓ The processed zone cools, without solidification, as there is no liquid, forming a defect-
free recrystallized, fine grain microstructure.
5
1.2.3 PROCESS PARAMETERS OF FSW
A friction stir welding (FSW) tool is obviously a critical component to the success of the
process. The tool typically consists of a rotating round shoulder and a threaded cylindrical pin that
heats the work piece, mostly by friction, and moves the softened alloy around it to form the joint.
➢ A process parameter is the current status of a process under control. Accurate
measurement of process variables is important for the maintenance of accuracy in a
process.
➢ The following six important parameters are commonly measured variables in the FSP
process.
1. Tool Rotation Speed (or) Spindle Speed (rpm)
2. Tool Travel Speed (or) Feed Rate (mm/min)
3. Axial Load (KN)
4. Plunge Depth (mm/min)
5. Tool Tilt Angle (Degree)
6. Dwell Time(Sec)
6
1. Tool Rotation Speed (or) Spindle Speed (rpm)
• Spindle speed (or) Tool Rotation speed is the rotational frequency of the spindle of the
machine measured in Revolution per minute. It is important process parameter for
producing good defect free sample.
• The Excessive spindle speed will cause premature tool wear, breakages.
• This tool tilt angle action is mainly help as to proper mixing of the work
Material in the stirring zone. (Homogeneous mixture)
• Dwell time is the standby time of the tool penetration in the work material during the
processing.
7
• In this dwell period, Tool shoulder surface is penetrated at a certain depth like 0.2 mm to
0.4mm.This penetrated shoulder area (contact area) will give the better string action for the
surface of work material.
• Also it will avoid the overflow of the molted material from the working area to the exit.
1. Shoulder diameter:
The diameter of the tool shoulder is important because the shoulder generates most of the
heat, and its grip on the plasticized materials largely establishes the material flow field. For a good
FSW practice, the material should be adequately softened for flow, the tool should have adequate
grip on the plasticized material and the total torque and traverse force should not be excessive.
2. Pin (probe) geometry:
The shape of the tool pin (or probe) influences the flow of plasticized material and affects
weld properties. A tapered tool pin increases the material flow compared with a cylindrical pin
.The axial force on the work piece material and the flow of material near the tool are affected by
the orientation of threads on the pin surface.
8
1.2.5 STUDY OF FSW ZONES
During the welding or processing time various heating zones are formed around the tool
rotation. The following four zones are very important for microstructural study.
i) Stir Zone (SZ)
ii) Thermo Mechanically Affected Zone (TMAZ)
iii) Heat Affected Zone (HAZ)
iv) Un Affected Zone (UAZ)
The following Fig are clearly indicated the various zone in the cross sectional.
The strong grain refinement produced by the process leads the microstructure to the fine
dimensions offering the possibility to exhibit superplastic properties. The fine grain size of the
nugget zone and the solid state transformations acting in the TMAZ and HAZ lead to high tensile
strength and enhanced fatigue properties with respect to traditional fusion techniques.
The flow arm is on the upper surface of the weld and consists of material that is dragged
by the shoulder from the retreating side of the weld, around the rear of the tool, and deposited on
the advancing side.
For example schematic diagram will shows the detailed view of various zones in aluminum
matrix .The microstructure will shows equal distribution of material and the strength of the
material will be increased.
9
FIGURE 1.7 SCHEMATIC FOR MICROSTRUCTURE OF FSW ZONE
1. Weld nugget:
The weld nugget is characterized by severely deformed and dynamically recrystallized
region. Weld nugget composed of fine – equated recrystallized grains. The fine recrystallized zone
at the weld nugget is due to heavy plastic deformation followed by dynamic recrystallization
occurred during thermo mechanical processing.
10
4. Unaffected Zone:
The unaffected zone is also called as base metal .The unaffected zone thus not is affected
by heat generated during the welding process .The properties of this region thus not changed
compared to the TMAZ,HAZ.
FSW has become a major joining process in the aerospace, railway and ship building
industries especially in the fabrication of magnesium alloys. FSW process offers numerous
advantages over the conventional fusion welding process such as better weld strength, lesser
residual stresses, absence of filler material/shielding gas, relatively easier mechanism, possibility
of joining difficult-to-weld dissimilar materials. Joining of panels and large extruded profiles is
also an interesting application for FSW and it is used now in series in ships, bridge and wagon
building and in off shore industry.
FSW has been shown as an effective technique in following applications
✓ To fabricate surface composites
✓ To refine microstructure of cast light alloys
✓ To produce fine-grain microstructure, this exhibits super plasticity.
Aerospace:
✓ Potential applications of FSW in aerospace industry are in the fields of fuselage structural
parts and cryogenic tanks.
✓ One of the first implementations of FSW in the aerospace industry for use on the space
shuttle external tank (ET). In addition to weight savings, the use of FSW leads to a
reduction in parts, reduced cycle times, greater joint strength, and lower manufacturing
costs
Automotive:
✓ These are attractive processes for manufacturers seeking to reduce body weight by
integrating light weight magnesium alloys into their assemblies and reduce the energy
consumption of their joining processes.
✓ FSW concepts applied to magnesium tailored blanks for door panels, drive shafts, and
space frames.
11
Cam and mobile phone bodies
Aerospace applications
FIGURE 1.8 SCHEMATIC FOR APPLICATION OF AZ31B MG ALLOY
12
Navy:
✓ Current applications are in materials joining however forming and materials processing
operations are being investigated for applications on future vessels.
✓ Using FSW, fabricators are able to provide large components for Navy vessel construction
which have a reduced dimensional distortion. The result is a reduction in the total cost from
fabrication to assembly of the component without a reduction in quality.
13
CHAPTER-2
LITERATURE REVIEW
1. Abachi et al (2010) has investigated the effect of the probe profile, rotation speed and particle
size on the microstructures and hardness of the AZ31/Al2O3 was investigated. AZ31 Mg-based
Nano composite with nano-Al2O3 particles were successfully fabricated by FSPwith threaded
probe tool. Cavities and micro void were seen in non-threaded and three-fluted specimens due to
low material flow of stir zone.
2. Mohsen Bahrami et al (2013) have fabricated AA1050/SiC Nano-composite layer, the lowest
average microhardness value, was 111HV, as well as the most uniform particle distribution was
achieved in threaded tapered specimen. It also ensured the uniform micro hardness in the profile.
3. Mohsen Bahrami et al (2013) gives detailed information about the cluster size plays the
key role in determination of UTS. Smallest clusters in threaded tapered specimen confirms its
highest UTS.
4. Mohsen Bahrami et al (2013) found that the tool shoulder is responsible for material
consolidation. Interestingly, material consolidation is appropriately done only if the materialhas
previously been plasticized enough.
6. I Dinaharan et al (2012) have explored that friction stir welding and processing both take
place at the center while only friction stir processing takes place away from the center. Therefore,
the center may experience less deformed compared to the sides. This may also be responsible for
the hardness drop at the center.
17
7. A.somireddy et al (2014) gives detailed information about the higher rotational speed also
causes expensive release of stored materials to the upper surface. Which produces micro- voids
in the stir zone and this may be of one reasons for lower tensile properties of the joints.
8. A.somireddy et al (2014) investigated that the joint fabricated with the rotational speed of
1120rpm, welding speed of 40mm/min, recorded higher hardness (75Hv) in the stir zone, and this
is also one of the reasons for superior tensile properties of these joints compared to other joints.
9. A.somireddy et al (2014) gives detailed information about the higher tool rotational speed
resulted in higher heat generation and this lead to the excessive release of stirred material to the
upper surface which results in lower hardness.
10. Balasubramanian et al (2008) have discussed welding is carried out around 70-90% of
the material melting point. So it is important that the tool material should have sufficient strength
at this temperature otherwise the tool can twist and break.
11. Padmanaban et al gives (2008) detailed about the magnesium alloys have many attractive
properties, such as low density and high specific strength. It is predicted that the application of
magnesium alloys will grow rapidly in the near future, especially in the transport industry.
12. Kamran Dehghani et al (2013) have explored at 800 rpm, increase in travelling speed,
resulted in larger grain sizes. This result suggests the key role of stirring action in controlling
the grain size. On the contrary, at 1250 rpm, finer grains obtained at higher travelling speeds. This
phenomenon reflects the domination of heat input factor to stirring action of the pin. At 1000
rpm, grain size values have not any particular correlation with travelling speed.
14. Nader parvin et al (2013) was found an onion ring structure in the specimen friction stir
processed by threaded pin. Triangular, square, & four flute square specimens showed partial
onion ring pattern. No evident onion ring, however, was observed in FFC specimen. While
heat input is not adequate, the material flow is low & therefore, no onion rings could be
18
formed. Thus, it could be inferred that TT & FFC specimens had received the maximum &
minimum heat input, respectively.
2.2.1 INTRODUCTION
Magnesium is normally melt in mild steel crucibles for the alloying, refining or cleaning
stage due to very slow reaction with the steels. Magnesium is very soft. It is necessary to add
either alloy elements or reinforcements to make it stronger.
❖ Magnesium is the third most abundant element and constitutes about 2 % of the
Earth’s crust. Found 2.8% in sea water and other forms, i.e.,
❖ The Basic Raw Materials are,
✓ Dolomite (CaMg(CO3)2),
✓ Magnesite (MgCO3)
✓ Carnallite (KMgCl3.6H2O).
19
higher welding speed utilized. This is not a factor in the base metals that are welded in the
soft condition.
ALLOY CHARACTERISTICS
Tough, leak tight castings with 0.0015 Be, used for pressure die-
AZ81 casting
20
Pressure-tight, weldable, good creep resistance and proof stress to
QH21
300ºC
21
2.2.3 INTRODUCTION AZ31B MAGNESIUM ALLOY
Magnesium alloys have recently received considerable attention due to their excellent
properties such as light weight, high specific strength and stiffness, Mach inability and
recyclability. These advantages make magnesium alloy make very attractive materials in a wide
variety of applications, where weight reduction is extremely important. At room temperature
magnesium and its alloys are difficult to deform due to the crystal structurewhich is hexagonal
close packed.
However magnesium alloys are still not as popular as aluminum alloys in structural
application and a major technical challenge is the development of reliable and inexpensive joining
methods to produce high quality welds.
Friction Stir Welding (FSW) is a capable of joining magnesium alloys without melting
and thus it can eliminate problems related to the solidification. As FSW done not require any
filter material, the metallurgical problems associated with it can also be reduced and good quality
weld can be obtained.
In AZ31, AZ60 and AZ80 grades of wrought magnesium alloys were welded using FSW
process and their mechanical & metallurgical properties were evaluated.
22
2.2.4 CHARACTERISTICS AND METALLURGY OF MG ALLOY
Magnesium is the lightest metal that can be used in structural applications when alloyed
with other elements. Magnesium is the lightest of all light metal alloys and therefore is an
excellent choice for engineering applications when weight is a critical design element. It is
strong, has good heat dissipation, good damping and is readily available.
Magnesium has a moderately low melting temperature making it easier to melt for casting.
Additionally it is relatively unstable chemically and extremely susceptible to corrosion in a
marine environment. It is thought that the corrosion is due more to impuritiesin the metal
versus an inherent characteristic.
Magnesium can also be alloyed with rare earth elements, which increase the strength of
magnesium especially at high temperatures. The key properties of magnesium alloys arethat
they are light weight, with low density (two thirds that of aluminum), and have good high
temperature mechanical properties with good to excellent corrosion resistance.
In particular cast magnesium alloys have specific design and manufacturing advantages:
1. Castings can be made with thinner walls than aluminum (1-1.5mm versus2-2.5mm).
2. Castings cool more quickly due to a reduced latent heat of fusion per unit volume.
3. High gate pressures can be achieved using moderate pressures due to the low density of
magnesium.
4. Iron from casting dies has low solubility in magnesium alloys, which reduces any tendency
to die soldering.
Magnesium alloys used for automotive applications is based on the combination of high
strength properties and low density. In automotive applications weight reduction will improve
the performance of a vehicle by reducing the rolling resistance and energy of acceleration, thus
reducing the fuel consumption and moreover a reduction of the greenhouse gas CO2 can be
achieved.
23
Magnesium alloys should be used in applications where low mass and high specific
properties are required. Low creep resistance, high coefficient of thermal expansion (CTE), low
Young’s modulus, insufficient ductility and crash energy consumption in car body structures, low
fatigue stability, low corrosion and wear resistance are deficits which have to overcome by further
alloy and/or process developments.
The following attractive properties are widely suitable for more applications.
❖ Ability to die cast at high productivity rate.
❖ Good creep resistance to 120°C.
❖ High damping capacity due to ability to absorb energy elastically.
❖ High thermal conductivity permitting rapid heat dissipation.
❖ Good machinability.
Automotive Application:
✓ 20,000 standard type cars with 6 and 8 cylinders were produced with the following
mass production magnesium parts: disk wheels, gear box cases, gear box covers, rear
suspension gear box cases ,chain locker, chain locker cover, crank cases, fly wheel
cases and various bearings, slide guiding and covers.
✓ It’s used for their winning racing cars a great number of electron parts such as crank,
compressor and gear box cases, brake shoes, timing, differential and camshaft cases
and various smaller parts.
✓ Highly loaded electron engine parts have also contributed .Altogether many magnesium
parts have already been used by all major car manufacturers inautomotive applications
until (engines, gears, clutch, rear suspension, starter, ignition, steering, breaks, car body,
seats, wheels (rims), etc.) and the application was not only restricted to cast parts.
24
FIGURE 2.3 SCHEMATIC FOR APPLICATION OF MG
25
particles. In contrast, the hardness of the FSP AZ31 without the Sic particles was
significantly decreased due to the abnormal grain growth.
2. AZ31/Al2O3 NANOCOMPOSITE:
Fabricate AZ31/Al2O3 Nano composites by friction stir processing (FSP). Due to severe
plastic deformation, dynamic recrystallization, and grain growth retardation by nanoparticles
during the FSP processing, ultrafine grained microstructures with homogeneous distribution of
the nanoparticles were produced.
The Al2O3 powder was fed into a groove of a width and depth of 1.2mmand 5mm,
respectively, which was located on theAZ31 plate before FSP. Then, the tool was insertedinto
the groove and composite fabrication has been processed, a constant travel speed of 45 mm/min
was adopted. Then, tool rotational speeds of 800, 1000, and 1200 rpm were applied. The
distribution Al2O3 of the particles and the grain size of the etched sample were evaluated by
optical microscopy (OM) and micro hardness was measured using a Micro-Vickers hardness
tester with a load of 200 g.
3. CU/B4C NANOCOMPOSITE:
The B4C particles significantly influenced the area, dispersion, grain size, micro hardness
and sliding wear behavior of the Cu/B4C surface composite .Boron carbide has excellent chemical
and thermal stability, high hardness and low density and is used for manufacturing of armor tank,
neutron shielding material etc., When the content of B4C particle increase, it leads to increase
in flow stress of the plasticized composite.
Micro hardness increased when the volume fraction of B4C is increased .The composite
demonstrated a reduction in the average grain size .When the volume fraction of B4C particles
was increased, the area of the surface composite decreased.
26
Initially UTS values decrease with the addition of TIC from 3% .This may be due to de-
cohesion of particles at the surface which led to decrease in UTS. After 5% SiC addition the
UTS values are found to be increasing stability.
The aim of this project was to fabricate AZ31B/SiC Nano composites by FSW and to
propose a new route producing a satisfactory distribution of nanoparticles accompanying fine
grain structure. We also investigated the effect of volume fraction and single passes on the welded
joints on metallurgical properties such as macrostructure, microstructure, cluster analysis, grain
measurement values.
FSP is a simple, affordable and productive technique for modifying the grain structureof
sheet metals. It is a solid-state process in which a specially designed tool is plunged intothe
sheet rotated and moved thereby causing intense plastic deformation through a complex stirring
action. This yields a dynamically recrystallized material having a fine grain microstructure. Some
of the main advantages of FSP over other refinement techniques are
27
CHAPTER-3
EXPERIMENTAL WORK
3.1. INTRODUCTION
In this chapter the experimental setup and welding conditions are discussed in detail
from machine to instrumentation facility. This chapter describes the steps that were taken to
achieve the objective of this study. The produced Magnesium Metal matrix (MMC) composite
welded joints by vertical milling Centre (VMC) and validate the optimum results.
The aim of this project was to fabricate AZ31B/TiC Nano composites by FSW
and to propose a new route producing a satisfactory distribution of nanoparticles accompanying
fine grain structure.
Commercially available SIC Nano powder (< 200 nm particle size) and AZ31B
Magnesium alloy plates are used in this work. The thickness of the plate is 6mm.The Tic powders
were filled into a groove machined on the AZ31B cast plate. The H13 HARDENED TOOL
STEEL was used in this work. The constant tool rotational and traverse speeds wereused in
this work 1250 rpmand 40mm/min, respectively. The tilt angles were 0°.
To study the microstructure and the micro hardness, the FSPed specimens were cut in
traverse direction. Microstructure evaluation of the FSPed zone and the distribution of the Tic
particles in stirred zone (SZ) were carried out by scanning electron microscopy. Microhardness
of the specimens was measured in the cross section using Vickers micro hardness testing
machine. In all the tests, a load of 200 g was applied for 15s.
28
3.2. METHODOLOGY OF WORK
OBSERVATIONS
MICROSTRUCTURE
TENSILE STRENGTH RESULTS
PERCENTAGE OF
ELONGATION
CORROSION
RESISTANCE
CONCLUSION
29
3.3 VERTICAL MILLING CENTRE AS FSW MACHINE
30
FIGURE 3.2 FIXTURE SETUP
A pilot hole of smaller diameter than the probe was drilled between the abuttingsheets
at the start of the process seam. Touches down conditions were set to minimize the stress on
the tool. Traversing was initiates after a sufficient time period to plasticize the work piece material
in contact with the shoulder and probe. The friction stir processing operation was carried out at
ambient temperature and the specification of the FSW machine.
AZ31B magnesium-alloy plate (hot-rolled and soft-annealed) has the nominal chemical
composition in weight percent are given in table 2. Friction stir processing (FSP)has been
developed by several researchers to produce an upper surface modification of metallic materials.
31
FIGURE 3.3 RECEIVED AZ31B MAGNESIUM PLATE
The chemical composition of the AZ31B Magnesium Plate are given below.
TABLE 3.1 CHEMICAL COMPOSITION OF MG ALLOY PLATE
They mostly used tool materials are H13 hardened steel, HSS. High-quality
Weld can be created by this process with e. g. a milling machine because using same movement
conditions but the tool is different. Basically other tool design is needed because the goal
isn’t the material removing but the material mixing and heating by frictional heat.The tool
must be meet several important requirementsOn the one hand in the course of mixing the
material flow conditions specifically affect the quality of the weld, so the tool geometry is very
important.
Non-consumable High Speed Steel (HSS) tool steel with flat shoulder is chosen as tool
material to fabricate the joints, because of its high strength at elevated temperature,thermal
fatigue resistance and low wear resistance. The diameter of the shoulder and pin used were 18
mm, 6 mm respectively and length of the pin is 5.7 mm.
32
Therefore, the good tool materials have the following properties:
❖ good wear resistance,
❖ high temperature strength, temper resistance,
❖ Good toughness.
Tool wear is the important considerations in the selection of tool material.The tool profile
nomenclatures are listed below the tabulation in Table.2.
TABLE 3.2 TOOL PROFILE NOMENCLATURES
SD:18mm;
1250 rpm
H13 Hot working Taper Threaded PL:5.7mm
40 mm/min
PD:6mm
Materials Composition
Carbon 0.85%
Tungsten 6.00%
Molybdenum 5.00%
Chromium 4.00%
Vanadium 1.90%
Hardness 63-65
33
FIGURE 3.4 SCHEMATIC DIAGRAM OF TOOL
FIGURE 3.5 AS RECEIVED SIC MICRO POWDER & TEM IMAGE OF NANO
PARTICLE
34
TABLE 3.4 PROPERTIES OF SIC
The volume fraction (percentage by volume, Vol %) is one way of expressing the
composition of a mixture with a dimensionless quantity,
Where,
Here,
Groove width=0.4mm
Groove depth=5mm
Pin diameter=6mm
Pinlength=5.7mm
35
3.5.2. IDENTIFYING IMPORTANT PARAMETERS
A) VARIABLE PARAMETERS
In this project, majorly discussed about four variable process parameters. The four
variable process parameters are rotational speed, traverse speed, size of particles and groove
width.
Rotational Speed
Rotary speed has an important influence on the steady state temperature reached in the
process. The rate of heat generation and heat dissipation balance each other at a steady value
which depends on the process settings, particularly the rotary speed. The best procedureto lower
the peak temperature would be to adopt lower speeds of rotation.
Traverse Speed
Travel speed is the velocity at which the tool is fed that is advance against the work piece.
During the process the material will be flow into the both the sides of tool like advancing side
and retracting side.
Size of Particles
The effect of particle size and amount of reinforcement component on the properties
of AZ31B-Sic & Al2O3nano and micro composites were investigated. The various size of
particles can be influence the properties of welded joints.
36
Figure 3.6. TEM micrograph of as-received nano particles (a) SiC nano particles
(b)Al2O3 nano particles
b) CONSTANT PARAMETERS
Axial Force
Axial force is the vertical force of tool on the base material in FSW process. At lower
axial force (2 kN), the tensile strength of FSW joints is lower.
When the axial force is increased from 2 kN, the tensile strength also increases, reaching a
maximum at 3 kN. However, if the axial force is increased beyond 3kN, the tensile strength
of the joint decreases. Heat is generated by the rotating tool under the application of axial force;
this heat is the primary source for welding.
37
Tool Pin Profile
The influence of pin geometry on particle incorporating in the welded joints. In this
investigation the cylindrical threaded pin profile to give the to give the good particle distribution
on the welded zone.
Tilt Angle
A suitable tilt of the spindle in the trailing direction ensures that the shoulder of the tool
holds the stirred material by a threaded pin and moves material efficiently from the front to
the back of the pin. This tool tilt angle action is mainly help as to proper mixing of the work
material in the stirring zone.
Tool shoulder diameter is constant. Tool shoulder to give the heat energy on the travel of toolon
the base metal by the friction between tool shoulder and base material.Tool Pin Diameter
Tool pin diameter is constant. Pin profile is cylindrical threaded. It is majorly influence the
particle distribution in welded zone. The list of the constant parameters are tabulated in Table
3.5.
38
Table 3.5 Constant Parameters
The AZ31B magnesium alloy plate was cut by the wire cut Electrical Discharge
Machining. The below diagram showed that the prepared sample for process.
By using spark erosion EDM process the necessary dimension of groove was
produced.
39
The below diagram was showed the volume prepared sample
FSW involves complex material movement and plastic deformation. Welding parameters,
tool geometry and joint design exert significant effect on the material flow pattern and
temperature distribution, thereby influencing the micro structural evaluation of material.
In this section, a few major factors affecting FSW process, such as tool geometry, welding
parameters, joint design are addressed. The strength of friction stir welding dependson the
following three process parameters. They are
Spindle speed
Feed rate
Depth of penetration
SAMPLE-1:
PARAMETER SETTING
40
Discussion:
This is our first sample to weld the AZ31B Mg alloy plate. In this sample we have
find the defect as tool pin length will be increase when we have weld at the speed of 1250rpm.
Error:
Surface is various thickness in magnesium plate and tool is various in length pin tool.
PARAMETER SETTING
Speed =1600rpm
Discussion:
This is our second sample to weld the mg alloy plate. In this sample we have find the
defects as tool pin length slightly altered with respect to the plate thickness we have weld at the
speed of 1400rpm and feed rate 40 mm/min.
Error:
The weld is tool travelling speed is high and removing ship and melting metal increase.
SAMPLE-3
41
Photo image
PARAMETER SETTING
Discussion:
In this weld sample producing no defect from the surface and it will produce the tunnel defect
in the crass section view.so we have to reduce the spindle speed with the correct feed rate
condition.
Error:
In this weld samples load high and plate thickness various dimensions and not proper
weld samples.
Therefore we finally conclude the welding speed and the feed rate of the variouswelding
sample based on the theory of the following statement. It is stated that the when the welding speed
is maximum and then the feed rate is to minimum compared to the weld speed. Then become a
good quality welding samples we produce. According to this we finalize the parameter
importantly welding speed is 1250 rpm and welding feed rate is 40 mm/min. It will produce
defect free weld sample. The following tables are produced constant process parameters and
variable process parameter to list.
Table no 3.5 is show the constant welding parameters to be welded in the AZ31B/Tic
plate for good welding condition.
42
TABLE 3.6 CONSTANT WELDED PARAMETER
In FSW, the non-consumable tool plays vital role in generating heat by means of friction
to plasticize the materials to be welded on the magnesium plates. Though the tool has three
different portions such as pin, shoulder and shank. The pin diameter and the shoulder diameter
decide quantinum oh heat generated during FSW.
43
TABLE 3.7VARIABLE WELDING PARAMETERS
3 AZ31B/Al2O3
A software based PAR basic electrochemical system (Figure 3.7) was used for conducting
potentio dynamic polarization tests to study the pitting corrosion behavior the of welded zone.
The standard calomel electrode (SCE) and carbon electrode were used as the reference and
auxiliary electrodes respectively. All the experiments were conducted in 3.5% NaCl solutions,
with the pH adjusted to 10. The potential scan was carried out at 0.166 mV/sec with an initial
potential of – 0.25 (OC) SCE to the final potential of pitting. The exposure area for these
experiments was 1 cm2 . The potential at which the current increases drastically was considered
as the critical pitting potential (Epit). Specimens exhibiting relatively more positive potential,
(or less negative potential) were considered as those with better pitting corrosion resistance
Figure 3.12 (a) Basic electrochemical (b) Electrochemical flat cell system
44
3.10 GENERAL CORROSION TESTS
The salt fog apparatus (Figure 3.12) was used for testing the corrosion behavior of the welded
zone. The experimental set up is shown in Figure 3.12. This apparatus consists of an enclosed
glass chamber with square 49 plastic rods to hang the specimens. Two nozzles, viz., one for
air and one for water, are present within the chamber. The air nozzle is connected to the air
compressor and the water nozzle is connected to a can containing the NaCl solution. The air
compressor supplies the air to the salt fog apparatus at the required working pressure. The nozzles
are placed 90o apart from one another, such that a NaCl fog is created within the chamber. The
specimens were tied up in the chamber with a non-corrosive polymer thread and hung in such
a way that they were held at an angle of 7 to 14o parallel to the flow of the fog from the nozzles.
The constant flow rate is set within few minutes the cloud of fog is created, and all the specimens
are be subjected to a constant flow of NaCl droplets striking their surfaces. Every 16 hours (for
48 hours) the specimens, depending upon their batch were removed from the chamber, and
cleaned with acetone to remove any rust that may have been formed on the surface of the
specimens.
45
CHAPTER 4
4.1. INTRODUCTION
Uniaxial tensile test is known as a basic and universal engineering test to achieve material
parameters such as ultimate strength, yield strength, % elongation, % area of reduction and
Young's modulus. These important parameters obtained from the standard tensile testing are
useful for the selection of engineering materials for any applications required.
The tensile testing is carried out by applying longitudinal or axial load at a specific
extension rate to a standard tensile specimen with known dimensions (gauge length and cross
sectional area perpendicular to the load direction) till failure. The applied tensile load and
extension are recorded during the test for the calculation of stress and strain. A range of universal
standards provided by Professional societies such as American Society of Testing and
Materials (ASTM), British standard, JIS standard and DIN standard provides testing are selected
based on preferential uses. Each standard may contain a variety of test standards suitable for
different materials, dimensions and fabrication history. For instance, ASTM E8: is a standard
test method for tension testing of metallic material sand ASTM B557 is standard test methods of
tension testing wrought and cast aluminium and magnesium alloy products
A standard specimen is prepared in a round or a square section along the gauge length
as shown in figures no- respectively, depending on the standard used. Both ends of the
specimens should have sufficient length and a surface condition such that they are firmly
gripped during testing. The initial gauge length Lo is standardized (in several countries) and
varies with the diameter (Do) or the cross-sectional area (Ao) of the specimen as listed in table
1. This is because if the gauge length is too long, the % elongation might beunderestimated
in this case. Any heat treatments should be applied on to the specimen prior
to machining to produce the final specimen readily for testing. This has been done to prevent
surface oxide scales that might act as stress concentration which might subsequently affect the
final tensile properties due to premature failure. There might be some exceptions, for examples,
surface hardening or surface coating on the materials. These processes should be employed after
specimen machining in order to obtain the tensile properties results which include the actual
specimen surface conditions.
46
Figure 4.1: Standard tensile specimens
The testing Dimensions are clearly indicated in the following figure with our testing
component image.
TESTING FACILITY
Machine no : MI UTME 19
47
Accuracy, % :± 1.00
The ultimate requirement of FSW process is to produce required amount of heat during
welding, which in turn could facilitate the matrix metal flow around the tool pin in the plasticized
state and generate enough amount of shearing force to act along the line of weld which would
produce welded joints of sound quality (Heurtier et al 2006). The amount ofheat generation
during FSW process mainly depends on the friction force and plastic deformation which tend to
form recrystallized grain growth in the SZ (Afrin et al. 2008). In addition to this, the ceramic
reinforcements also play an important role in grain refinement during FSW. The hard nature of
ceramic particles performs a shearing action between the parent metals during welding process
and hence the bigger sized grains are converted intosmall grains. At the same time, the
production of heat energy and grain refinement of nugget zone mainly depend on the process
variables of FSW process such as tool rotational speed,tool travelling speed, axial force, type
of reinforcements and amount of particles addition inthe SZ during welding.
48
and homogenous dispersion of nano particles in the stir zone. The detailed comparison of all the
optimized welded joints (AZ31B/SiC and AZ31B/Al2O3) is explained below.
Table 4.1 Comparative analysis of FS Welded composite joints with base metal welded
joint (without reinforcement)
From the Table 6.1, it could be inferred that the values of UTS, POE and microhardness
of AZ31B/SiC FS welded composite joint are higher compared to AZ31B/Al2O3 and base metal
welded joints and the values are presented as bar chart in Figure 6.15.
Figure 4.4 UTS and POE values of (a) AZ31B/SiC FS welded composite joint
(b)AZ31B/Al2O3 FS welded composite joint (c) base metal welded joint
(without reinforcement).
From the property values shown in Figures 6.1 (a) & (b) it can be observed that when compared
to the base metal welded joints (without reinforcement), the properties of the joints prepared with
reinforcements (the addition of nano particles in the weld nugget zone during
49
welding exhibit enhanced properties at the optimum welding conditions. When compared to
the base metal FSW joint without reinforcement, the percentages of property enhancement of
the nano-SiC particles reinforced FSW joint are 12.13 % and 52% for UTS and POE. Similarly,
when compared to the base metal FSW joint without reinforcement, the percentages of property
enhancement of the nano- Al2O3 particles reinforced FSW joint are
10.5 % and 45% for UTS and POE respectively. However, among the FSWed composites the
nano-SiC incorporated FS welded composite joint has exhibited more enhanced properties
compared to nano-Al2O3 incorporated FS welded composite joint.
Figure 4.2 contains the optical micrographs (a & b) of AZ31B/SiC FS welded composite
joint obtained from stir zone (SZ) and transition zone (SZ & TMAZ) with 100× magnification
along with SEM micrograph (c). From the Figure 6.2 (a), it could be inferredthat the SiC
nano particles are uniformly dispersed in the magnesium matrix within the SZdue to dynamic
recrystallization caused by pinning effect of tool pin (Sabbaghian et al. 2014; Azizieh et al. 2011).
Also Figure 6.2 (b) presents the transition zone which reveals the SiC particles free zone and SiC
particles dispersed zone which are identified in TMAZ and SZ respectively. Figure 6.2 (c)
presents the higher magnification (SEM micrograph) view of composite joint and it gives an
excellent conformity for SiC particles dispersion in the SZ. Very few clusters and
agglomerations are observed in the SZ. Moreover, the presence of SiC particles in the SZ were
confirmed through EDS peak points which is presented in Figure 6.3.
50
Figure 4.5 Optical & SEM micrograph of AZ31B/SiC FS welded composite joint (a) Stir
zone micrograph (b) Transition zone (c) SEM micrograph.
51
Figure 4.6 Optical & SEM micrograph of AZ31B/Al2O3 FS welded joint (a) stir zone
micrograph (b) Transition zone (c) SEM micrograph.
52
CHAPTER 5
STUDY OF PITTING CORROSION PROPERTIES
5.1 INTRODUCTION
Pitting corrosion is a type of corrosion that attacks a local area of the metal and eventually
leads to the formation of holes in the metal. Pitting corrosion can lead to stress corrosion cracking,
an example of which collapse of the Silver Bridge in West Virginia, USA happened in 1967.
This type of corrosion generally occurs when a small area is affected bythe environment and
becomes anodic. Meanwhile, another area in the metal acts as a cathode. This leads to a type of
galvanic corrosion which begins at the surface of the metal but canspread downwards and
eventually lead to the structural failure of the metal.
Pitting corrosion can lead to the formation of pits on the metal. The shape of these pits
can vary from shallow and wide to deep and narrow. An illustration depicting the different shapes
that a cavity formed on the metal due to pitting corrosion can take. The ratio between the deepest
pitting corrosion-formed cavity and the average penetration of the metal (which can be
calculated from the total loss in weight of the metal) is given by the pitting factor.
In the mechanism of pitting corrosion, the oxidation of the metal occurs, resulting inan
acidity which is localized. The generous separation of the cathodic half-reaction and the anodic
half-reaction helps maintain this localized acidity. The acidity leads to the electro
53
migration of anions towards the pit which is formed. A potential gradient is also formed by
localized acidity. The pits that are formed on the surface of the metal are often filled with the side
products formed in the corrosion process.
There are various distinct methods to test a steel grade’s pitting resistance. They are:
• ASTM G48, practice A and E- Since the acidic solution combines with oxidising ability
and chlorides, it is one of the toughest pitting corrosion tests conducted for stainless steel.
54
5.2RESULT AND DISCUSSION
The pitting potential values of the friction stir welds AZ31B/SiC are presented in Table
4.5. It has been found that the weld nugget exhibits better pitting corrosion resistance than the
base aterial as can be seen from typical dynamic polarization curves presented in Figure 4.7. In
case of weld metals only the eutectic is present at grain boundaries and dendrite boundaries.
Eutectic has much lower level of Mg content (32% against 52% in ) and also is large in size.
When corrosion starts, the matrix around SiC particles would dissolve and the SiC particle is
knocked out. Something to happen around a larger Mg particle would take more time as these
particles cannot be removed easily from the matrix owing to their size and non-rounded shape.
The difference in the pitting potential values of the AZ31B base metal (advancing side Epit = -
720.57, retreating side Epit = -709) and the friction stir weld AZ31B/SiC nugget (Epit = -684)
is noticeable and the reason for the absence of precipitatesas well as phase in the weld nugget.
It is clear that the SiC particles are present in the weld metal seem to be not as harmful as the
particles due to the much lower magnesium content inthe SiC particles.
Table 5.1 Pitting potential values of FSW AZ31B/SiC magnesium alloy joint
There is noticeable improvement in the pitting corrosion resistance of the weld nugget,
as shown by the lesser negative Epit values. The typical dynamic polarization curves presented
in Figure 4.7 show that the weld zone exhibited better pitting corrosion resistance.The pitting
potential values indicate the potential at which the onset of pitting takes place,and the smaller
negative values indicate better pitting corrosion resistance.
55
Figure 5.2 Dynamic polarization curves of FSW between AZ31B/SiC
5.2.2 Pitting Corrosion of FSW Magnesium Alloys of AZ31B/Al 2O3 composite joint
The pitting potential values of the friction stir welds AZ31B/Al2O3 are presented in Table
4.2. The difference in the pitting potential values of the AZ31B base metal and the friction stir
weld AZ31B/Al2O3 composite joint nugget is significant. The nugget exhibits lesser resistance
to pitting corrosion. This could be due to the larger number of Mg-Mn inter metallic particles.
Fragmentation of these particles occurs during stirring and hence the nugget contains larger
number of particles which are smaller in size resulting in lower pitting potentials. Severely
deformed and stressed grain structure in the TMAZ on both sides of the nugget exhibit further
reduction in pitting corrosion resistance.
56
Table 5.2 Pitting potential values of FSW AZ31B/Al2O3 magnesium alloy joint
There is noticeable improvement in the pitting corrosion resistance of the weld nugget, as shown
by the lesser negative Epit values. The typical dynamic polarization curves presentedin Figure
4.8 show that the weld zone exhibited better pitting corrosion resistance. The pitting potential
values indicate the potential at which the onset of pitting takes place, and the smaller negative
values indicate better pitting corrosion resistance.
57
CHAPTER 6
CONCLUSIONS
6.1 INTRODUCTION
This chapter first summarizes the main aspects of the present work and then elaborates on
the major conclusions arrived from the experiments which involved the fabrication of AZ31B/SiC
and AZ31B/Al2O3 FS welded composite joints and evaluating their mechanical properties and
pitting corrosion properties were examine the microstructures.
The friction stir welding (FSW) process of AZ31B/SiC and AZ31B/Al 2O3 were carried out
using vertical milling center (VMC) to produce FS welded composite joints for investigating the
performance of the welded joints. The constant tool rotational speed and tool travelling speed were
the important process variables in the present work. The primary output quality characteristics of
the composite welded joints are Ultimate tensile strength (UTS), Percentage of Elongation (POE)
and pitting corrosion which were examined on the FSW processed specimens fabricated by the
incorporating nano sized SiC (~50 nm) and Al2O3 (~30 nm) ceramic particles into the preplanned
grooves of the welding specimens. The effect of various input parameters wereevaluated through
microstructure analysis, tensile strength analysis and pitting corrosion for both the cases
(AZ31B/SiC and AZ31B/Al2O3) were determined using standard testing technique.
Following are the major conclusions drawn from the present investigation on friction stir
welding of AZ31B magnesium alloy with the reinforcement of SiC and Al 2O3 nano particles.
• The FSW process parameters considered in this research are tool rotational speed 1240
rpm, tool travelling seed 32mm/min. The quality characteristics considered to evaluate
performance are ultimate tensile strength, percentage of elongation and pitting corrosion.
The experiment was conducted followed for friction stir welding of AZ31B/SiC and
AZ31B/Al2O3 composite joints and base metal alloys.
58
• FSW can be effectively used to synthesis AZ31B/SiC and AZ31B/Al 2O3 MMCs without
any kind of defects. SiC and Al2O3 particles were distributed uniformly throughout the
magnesium matrix along the weld joint.
• From the macroscopic observation it was observed that, the FSW joints reinforced with
SiC and Al2O3 were not identified with any defects like tunnel defect, pin defect, piping
defect, solidification cracks and kissing bonds etc, at the optimized condition. From the
metallurgical inspection through optical and SEM analysis, it was observed that
homogeneous dispersion of nano particles (SiC & Al2O3) was achieved within the weld
nugget zone in this process.
• When the performance characteristics were analyzed, the SiC nanoparticles added weld
joints exhibited better property values compared to Al2O3 added weld joints.
• At the outset, the particles reinforced FS welded composite joints (SiC and Al 2O3) exhibits
better mechanical, metallurgical and corrosion properties than the base metal (AZ31)
welded joint without reinforcement.
59
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