CHAPTER I

INTRODUCTION

1.1 ENGINEERING MATERIALS

The knowledge of materials and their properties is of great significance for a design
engineer. The machine elements should be made of such a material which has
properties suitable for the conditions of operation. In addition to this, a design
engineer must be familiar with, how the manufacturing processes and heat treatment
affects the properties of the materials. The engineering materials are classified into
three types namely (a) Metals (b) Ceramics (c) Polymers.
Metals : Steels, wrought iron, cast iron, aluminium, copper, nickel etc...
Ceramics : Glass, brick, sand, cement, silicon carbide, tungsten carbide etc...
Polymers : Rubber, paper, fuel, wood, paints etc...

1.2 FINE GRAIN MATERIALS

Advanced materials, such as fine grained materials show promise for many industrial
applications including aerospace, automotive, biomaterials, sensor, construction,
electronics, metal-forming, storage and retrieval of information, optics. Reducing the
grain size of conventional super plastic alloys has been shown the lead to both an
increase in the elongation to failure and an optimal strain rate. These characteristics
are important for many industrial applications, including super plastic forming of
metals. The technology for the fabrication, characterization, modeling, design, and
application of fine structure materials is crucial for industrial competitiveness in the
worldwide market. Ultrafine materials are those materials exhibiting a grain-size
scale on the order of several (generally 100–1000) nanometers.
This size scale can include a particle diameter, width of a fiber or tube, layer
thickness, or grain dimension. A high strain rate and low-temperature super plastic
features have been observed in several fine structured materials. These materials

1
exhibit novel mechanical performance, such as asymmetry of compression and
tension, shear band formation, and elastic-perfectly plastic characteristics.

1.3 SEVERE PLASTIC DEFORMATION

Fine crystalline materials, consisting of large amount of grain boundary area, have
simulated considerable attention in the research field of advanced materials attributed
to their exceptional changes in mechanical, physical, and electronic properties. One of
the efficient methods to induce fine grain structure in materials is deforming it to
large strains below recrystallization temperature without intermediate thermal
treatment. Traditional techniques for introducing deformation of higher strains, such
as forging, extrusion, drawing, or rolling do have the inevitable limitation on required
equipments in exerting enough load or pressure to cause uniform submicron level
grain refinement. More recently developed techniques for producing fine grain
structure, viz. inert gas condensation and high energy ball milling are not yet capable
of producing large bulk samples of uniform dense structure. In recent years, various
severe plastic deformation (SPD) techniques have been practiced towards
synthesizing bulk fine structured materials attributed to the multifarious advantages of
these techniques with fine and uniform microstructure where the processed materials
contain no or very minimum porosity and impurity. Equal Channel Angular Pressing
(ECAP) is an efficient technique for grain refinement using severe plastic
deformation.

1.4 EQUAL CHANNEL ANGULAR PRESSING (ECAP)

Equal Channel Angular Pressing (ECAP) is a novel technique for producing fine
grain structures without change in the billet shape or dimensions. ECAP is capable of
producing fine grain structures. This progress related to the processing parameters,
die design, and micro structural features during equal-channel angular processing The
large sections of materials can be uniformly and intensively worked. It improves the
strength of the materials without any change in their chemical composition and
density. Due to the tremendous benefits and novelty of ECAP process, a lot of
research work is being initiated in India and abroad.

2
 CHAPTER II
LITERATURE REVIEW
2.1 MAGNESIUM

The weight of average family car has increased by 20% over the last
20 years. Most of the increased weight is a result of increased average engine size and
the additional safety features. On the other hand customer’s awareness of the fuel
efficiency has been made more acute by increasing fuel prices and the popularity of
environmental issues. So weight reduction is an imperative task for automobile
producer. The attractive benefit of reduction in automobile weight can be seen in
terms of improved fuel efficiency. The weight reduction have been made possible by
the replacement of steel by light metal alloys usually aluminum or magnesium.
Earlier most of steel or cast iron components in automobiles was replaced by
aluminum alloy. But at this moment the major aim and task of the researchers is to
find suitable materials which are more efficient than aluminum so as to reduce the
weight of automobile further. Magnesium and its alloy are one such promising
material whose light weight advantages could be used for the weight reduction
purpose.

Magnesium, with a density of 1.7 g/cm3 is the lightest of the structural

material. It is 2/3rd of its counterpart aluminum density (2.7 g/cm3) and 1/3rd of steel
density (7 g/cm3). So it has high specific strength properties over aluminum alloys.
However the total annual world consumption of magnesium at around 250 tones is a
fraction of the 20 million of aluminum used. Both metals were discovered in the early
19th century and industrial refining process for each metal was announced in 1886.
So the lower usage of magnesium is due to different complex of factors. However
developments in magnesium refining and processing technology have coincided with
new demands from many industries for high precision for light weight die casting.
Now the use of magnesium is growing at a faster rate than any other metals. While
there is no doubt that the maximum usage of magnesium in tonnage terms is the
automobile industry, there are newer high-tech industry which are beneficially

3
exploiting the properties of magnesium die casting. While the light weight is certainly
the major reason for the renewed interest in magnesium casting, and also there are
number of other properties, which make magnesium a preferred choice for
components in industrial application.

2.2 ADVANTAGES OF MAGNESIUM

Magnesium alloys has several advantages. The most important of these is light
weight. This lead to relatively high specific stiffness and specific strength for
magnesium alloys. Another very important advantage is flexibility and
manufacturability.

2.3 APPLICATIONS OF MAGNESIUM

Magnesium have various fields of applications.It may be used as alloying with

aluminum, iron and steel processing, as a structural metal, and electrochemical and
other uses. Some of the applications are discussed below.

2.3.1 Aircraft

Magnesium is employed extensively in aircraft engines, airframes and landing wheel.

The main factors dictating the use of magnesium have been strength/density ratio in
casting and stiffness/density ratio in the wrought forms, combined, as required, with
factors such as good elevated temperature, fatigue and impact properties, always with
good machinability. The alloys ZE41 (Mg-4.2Zn-0.7Zr-1.3MM), QE22 (Mg-0.7Zr-
2.5Nd- 2.5Ag), and particularly WE43 (Mg-4Y-3.25Nd-0.5Zr) are commonly used
for aircraft applications due to their improved corrosion and creep resistance[1].

2.3.2 Helicopter components

For military helicopters [1], the good ballistic tolerance of ZE41 has made it the most
common alloy used, although QE22 has been used where higher strength is required
at elevated temperatures. Currently both alloys are being replaced by WE43 and
WE54 (Mg- 5.1Y-3.25Nd-0.5Zr) alloys due to the excellent corrosion and creep
resistance of these latter alloys.

4
2.3.3 Cars and light trucks

Use of magnesium in automobiles despite its high cost compared to competing metals
(conventional steel and aluminum) is justified on the basis of component integration
and the near-net shape castability. The most promising applications for magnesium
are those where aluminum or plastic are not desirable substitutes for heavier materials
such as steel; i.e., substitution for either of these light-weight materials in existing
applications is unlikely [1,2]. This is borne out by the 1997 model cars in North
America in which increased use of magnesium has occurred largely at the expense of
steel. The use of magnesium in the new models ranges from about 1.4 to 9 kg per
vehicle giving an average of 2.9 kg per family car, about 16% more than for 1966
models. The dramatic benefit that reduced automobile weight can give in terms of
improved fuel consumption as shown in figure 2.1[1,2].

Figure 2.1. Fuel economy versus vehicle weight

For a New Generation automobiles such as the Ford stretched Mondeo/ Contour
P2000 which is expected to achieve nearly 80 mpg (3.4 l/100 km) [1,2]. In addition to
new power train requirements, this aggressive fuel efficiency goal requires that the

5
vehicles body weight and chassis must be reduced by nearly 50% and the total mass
be reduced by some 30% or 450 kg (from 1450 kg down to 950 kg) [1,2]. This has led
to extensive evaluation of the potential use of magnesium components to levels in
excess of 103 kg (10% magnesium) from a present 2.6 kg; a magnesium intensive
vehicle[1,2]. The magnesium industry has made great efforts to educate the
automotive industry on the benefits of utilizing magnesium to reduce vehicle weight,
cost, and/or complexity. Applications for magnesium in automobiles, using the die
casting approach, has been in components such as instrument panels, steering wheels,
steering columns and seat risers which take advantage of magnesium’s high strength-
to-density ratio, excellent ductility combined with attractive energy absorbing
characteristics. The most common automotive alloy today is AZ91D and AM60B
(Mg-6Al-0.3Mn). In addition, alloy AS41B (Mg-4Al-0.3Mn-1Si) has some North
American automotive applications. Magnesium parts in production include: accessory
drive brackets (AZ91D), automatic transmission clutch piston and stator (AS41B),
clutch housing (AZ91D), door mirror brackets (AZ91D), headlamp retainers
(AZ91D), upper and lower inlet manifolds (AM60B, AZ91D) oil filter adapter
housing (AZ91D), power window regulator housings (AZ91D), seat frames (AM60B)
as shown in fig 2.2, steering wheel armatures (AM50 [Mg-5Al-0.3Mn], AM60B) and
valve and cam covers(AZ91D).

Figure 2.2 Die cast magnesium alloy seat frame.

6
 Fig 2.3 Applications of Mg alloys in automobile
The fig 2.3 tells the important parts that have been made by magnesium alloys in
automobiles.
2.3.4 Missiles and space exploration

Strength and rigidity at minimum weight, coupled with ease of fabrication are
important for missile and space applications. However, the designer of missiles and
space probes needs other properties in his materials of constructions[1].

Conditions in space flight are rigorous, involving extremes of temperature from

aerodynamic heating, sudden immersion in shadows, and proximity of some
components to liquefied fuels: ozone and free radicals in the upper atmosphere:
bombardment by short wave electromagnetic radiation, high energy particles and
micrometeorites: vacuum down to 10-11 mmHg. EZ33 (Mg-2.7Zn-0.7Zr-3.2MM)
sand casting are used in the “Skylark” research rockets[1]. Limited information is
available on British missiles, but it is known that ZK51 (Mg-4.5Zn- 0.7Zr) and ZE41
castings have been used extensively for structural parts [1].

7
 Magnesium-based materials have a long history
of applications in the aerospace industry. Over the years, magnesium based materials
are extensively used in both civil and military aircraft. Some applications include the
thrust reverser (for Boeing 737, 747, 757, 767), gearbox (Rolls-Royce), engines and
helicopter transmission casings.

Figure 2.4. Thin-walled magnesium case and chassis for a hand-portable cellular
telephone .

2.3.5 Appliances and sporting goods

The trend has been for an increase in the use of magnesium die castings and examples
are computer housings and mobile telephone cases as shown in figure 2.4 where
lightness, suitability for thin wall casting and the characteristic of electromagnetic
shielding are particular advantages[1].

8
2.3.6 Nuclear energy industry

With natural uranium as a fuel, it is essential to conserve neutrons by only using

materials in the reactor which will not absorb them readily. Natural uranium plants
with operating temperatures suitable for power production essentially determine the
general reactor design and limit the canning material to magnesium and the coolant
gas to magnesium dioxide.
The advantages of magnesium over competing materials are: (a) low tendency to
absorb neutrons, (b) does not alloy with uranium, (c) adequate resistance to carbon
dioxide up to the highest service temperatures envisioned, and (d) good thermal
conductivity.

2.4 ALLOYS OF MAGNESIUM

Magnesium alloys are mixtures of magnesium with other metals (called an alloy),
often aluminium, zinc, manganese, silicon, copper, rare earths and zirconium.
Magnesium is the lightest structural metal. Magnesium alloys have a hexagonal
lattice structure, which affects the fundamental properties of these alloys. Plastic
deformation of the hexagonal lattice is more complicated than in cubic latticed metals
like aluminum, copper and steel. Therefore magnesium alloys are typically used as
cast alloys, but research of wrought alloys has been more extensive since 2003.
Cast alloys
AZ63, AZ81, AZ91,AM50,ZK51,ZK61, ZE41, ZC63, HK31,HZ32, QE22,
QH21,WE54,WE43,Elektron 21

Wrought alloys

AZ31, AZ61, AZ80, Elektron 675, ZK60,M1A,HK31,HM21, ZE41, ZC71

2.5 AZ 91

Among the various magnesium alloy systems, Mg-Al alloys are the most important
alloy systems since aluminum provide better castability.AZ 91 alloy contains 9%
Al,1% Zn,0.2% Mn ,is the most widely and commercially used Mg alloy in

9
automotive industries. This alloy provides very good tensile properties at room
temperature, excellent casting properties and corrosion resistance. Aluminum in this
alloy offer better castability, strength and corrosion properties. Zinc improves the
solid solution strengthening whereas Mn provides corrosion resistance. Comparison
of AZ 91 with other materials is given below[3].

Table 2.1 Comparison of properties of AZ 91 magnesium alloy with Al, Cast

iron, Plastic and steel materials

2.6 EFFECT OF ALLOY COMPOSITIONS IN AZ91

2.6.1 Aluminum

Aluminum is one of the major alloying elements to magnesium. Aluminum has very
good solubility in magnesium. The yield strength increases with addition of Al
whereas UTS increases up to 6% and then decreases. However the ductility increases
initially up to 3% of Al addition and then start to decrease steeply. The solid
solubility of Al in magnesium at room temperature is around 2%.So the excess Al

10
forms Mg17Al12 inter metallic with Mg. This phase is hard and brittle and hence,
acts as a strengthening element at room temperature Al in this alloy also improves the
castability .However ,Al also increases the tendency for shrinkage micro porosity up
to 9% can be related to the worst combination of mushy zone size, inter dendritic
feeding, permeability and eutectic volume friction.

2.6.2 Zinc
Zinc has very good solubility in Mg. The role of Zn in AZ91 alloy is to improve the
strength of alloy by solid solution strengthening. Zn also improves the fluidity of the
alloy. But higher amount of Zn to Mg-Al can lead to hot cracking problem. It is
further reported that the addition of Zn reduces the ductility of the alloy. Zn strongly
affects solidification pattern of AZ 91 alloy and there by forming micro porosity.
Studies report that addition of 2 % Zn increases micro porosity in sand cast Mg alloy
containing 2,4,8 and 10% Al. The presence of Zn decides the type of eutectic
(completely or partially divorced)during final stage of solidification.

2.6.3 Manganese

The main purpose of addition of Mn to AZ 91 alloy is to improve the corrosion

properties. The role of Mn in the improvement of corrosion resistance is two
fold.1.When Mn is added to Mg-Al alloys several types of AlMnFe intermetallic
particles are formed. These particles settle at the bottom of the melt, by which the
iron content in the melt is reduced.2.Mn also renders the iron containing particles left
in the melt during solidification less harmful by making them less efficient as
cathodes, compared to the Al-Fe intermetallics which are formed in Mn free MgAl
alloys.

2.7MECHANICAL PROCESSING METHODS

Fine crystalline materials, consisting of large amount of grain boundary area, have

simulated considerable attention in the research field of advanced materials attributed

to their exceptional changes in mechanical, physical, and electronic properties. One of

the efficient methods to induce fine grain structure in materials is deforming it to

11
large strains below recrystallization temperature without intermediate thermal

treatment. Traditional techniques for introducing deformation of higher strains, such

as rolling, forging, extrusion, tube and wire drawing, deep drawing do have the

inevitable limitation on required equipments in exerting enough load or pressure to

cause uniform submicron level grain refinement[4].

2.7.1Rolling

Figure 2.5. Rolling .

12
The material to be rolled is drawn by means of friction into the two revolving roll gap
The compressive forces applied by the rolls reduce the thickness of the material or
changes its cross sectional area In rolling the crystals get elongated in the rolling
direction. In cold rolling crystal more or less retain the elongated shape but in hot
rolling they start reforming after coming out from the deformation zon
2.7.2 Forging

Forging is basically involves plastic deformation of material between two dies to

achieve desired configuration. Depending upon complexity of the part forging is
carried out as open die forging and closed die forging. In open die forging, the metal
is compressed by repeated blows by a mechanical hammer and shape is manipulated
manually[4]. In closed die forging, the desired configuration is obtained by squeezing
the work piece between two shaped and closed dies. The schematic diagram of open
and closed die forging are illustrated in fig 2.7 and 2.8.

On squeezing the die cavity gets completely filled and excess material comes out
around the periphery of the die as flash which is later trimmed. Press forging and
drop forging are two popular methods in closed die forging. In press forging the
metal is squeezed slowly by a hydraulic or mechanical press and component is
produced in a single closing of die, hence the dimensional accuracy is much better
than drop forging. Both open and closed die forging processes are carried out in hot
as well as in cold state. In forging favorable grain orientation of metal is obtained[4]

Figure 2.6. Open Die Forging

13
 Figure 2.7. Closed Die Forging .

2.7.3 Extrusion
In extrusion, the material is compressed in a chamber and the deformed material is
forced to flow through the die. The die opening corresponds to the cross section of the
required product. It is basically a hot working process, however, for softer materials
cold extrusion is also performed[4].

2.7.3.1 Direct and Indirect Extrusion

In direct extrusion metal flows in the same direction as that of the ram as shown in
fig 2.8(a). Because of the relative motion between the heated billet and the chamber
walls, friction is severe and is reduced by using molten glass as a lubricant in case of
steels at higher temperatures. At lower temperatures, oils with graphite powder are
used for lubrication. In indirect extrusion process, metal flows in the opposite
direction of the ram. Fig 2.8(b) indicates the process of indirect extrusion. It is more
efficient since it reduces friction losses considerably. The process, however, is not
used extensively because it restricts the length of the extruded component[4].

14
 Figure 2.8 Extrusion types (a) Direct Extrusion (b)Indirect Extrusion
2.7.4 Drawing
Large quantities of wires, rods, tubes and other sections are produced by drawing
process which is basically a cold working process. In this process the material is
pulled through a die in order to reduce it to the desired shape and size. In a typical
wire drawing operation, once end of the wire is reduced and passed through the
opening of the die, gripped and pulled to reduce its diameter[4].A typical drawing
operation is illustrated in fig 2.9.

15
 Figure 2.9. Drawing .

2.8 SEVERE PLASTIC DEFORMATION

Severe plastic deformation (SPD) is a powerful technique for forming and controlling
materials and their properties. In SPD, large strains are applied to the material and
consolidation occurs both by the shear and fracture of the various phases present.
Methods of SPD should meet the generation of a fine-grained structure with
prevailing high angle grain boundaries, since only in this case can a qualitative
change in properties of materials occur, and the production of a uniform structure
within the whole volume of a sample without mechanical damage or cracks.
Traditional methods of SPD such as rolling, drawing or extrusion usually cannot meet
these requirements. In recent years, various severe plastic deformation (SPD)
techniques have been practiced towards synthesizing bulk fine structured materials
attributed to the multifarious advantages of these techniques with fine and uniform
microstructure where the processed materials contain no or very minimum porosity
and impurity. Equal Channel Angular Pressing (ECAP) is an efficient technique for
grain refinement using severe plastic deformation[5]

There is considerable current interest in fabricating metals with ultrafine grain sizes.
This interest arises for two reasons. First, it is possible in principle to increase the
strength of a material at low temperatures through the standard Hall-Petch
relationship as mentioned in equation 2.1, because the strength varies with the
reciprocal of the square root of the grain size.

16
 2.1

where σ0 is termed the friction stress, ky is a constant of yielding and d is the diameter
of grain Second, the retention of an ultrafine grain size at high temperatures, in the
regime where diffusion-controlled processes become important, offers the potential
for achieving a super plastic forming capability at high strain rates because the rate of
flow in super plastic deformation is inversely proportional to the square of the grain
size.
. Several methods are now available for attaining metals with extremely small grain
sizes, usually within the nanometer range, including inert gas condensation, high
energy ball milling and sliding wear. However, these procedures have not been
developed sufficiently to date that they are capable of producing large bulk samples
which are free of any residual porosity. As a result of these limitations, attention has
been devoted to the alternative processes of Equal-Channel Angular Pressing (ECAP)
and High-Pressure Torsion (HPT) in which ultrafine grains are introduced into a
material through intense plastic straining. In practice, ECAP appears to have greater
utility than HPT because there is a potential for scaling-up the process for industrial
applications through procedures such as the development of multi-pass facilities
where high strains are attained in a single passage through the ECAP die. The
principle of ECAP is that a metal is deformed through a process of simple shear with
the shear taking place without any concomitant change in the cross-sectional area of
the sample.[6]

2.9 EQUAL CHANNEL ANGULAR PRESSING

2.9.1 Principle of ECAP

There are numerous well-established methods for subjecting metallic samples to an

imposed strain, including through the standard industrial metal-working processes of
rolling or extrusion, but all of these methods necessitate a change in the physical
dimensions of the sample. By contrast, ECAP differs from these conventional
procedures because the cross-sectional dimensions of the sample remain unchanged

17
during straining. Historically, ECAP was first developed in the Soviet Union almost
twenty years ago. The principle of ECAP is depicted schematically in the three-
dimensional illustration in Fig. 2.10. The ECAP die contains two channels, equal in
cross-section, intersecting at an angle near the center of the die[3]. The test sample is
machined to fit within these channels and it is pressed through the die using a
plunger. Thus, simple shear is imposed at the shearing plane between the two
adjacent segments labelled 1 and 2 in Fig. 2.11. Three planes may be defined within
the sample at the point of exit from the die, as indicated in Fig. 2.10 where plane x is
perpendicular to the longitudinal axis of the sample and planes y and z are parallel to
the side and top faces, respectively[3].

Fig. 2.12 illustrates a section through the die and defines two internal angles, ϕ and Ψ,
delineating the curvature associated with the two channels: there is an angle ϕ
between the channels and an angle Ψ at the outer arc of curvature where the two
channels intersect[6,14,15].

Figure 2.10 Schematic illustration of ECAP showing the three orthogonal planes
x, y, z

18
 Figure 2.11 The principle of shearing between elements 1 and 2 in ECAP

Figure 2.12 A section through an ECAP die showing two internal angles ϕ and Ψ

19
2.9.2 Significance of the channel angle ϕ
A series of detailed experiments on pure aluminum, using dies having values of
ranging from 90◦ to 157.5◦, showed that an ultrafine microstructure of essentially
equiaxed grains, separated by grain boundaries having high angles of disorientation,
was attained most easily when imparting a very intense plastic strain with a value of ϕ
very close to 90◦. Evidence from finite element modeling suggests a potential
problem with dies having both ϕ = 90◦ and Ψ=0◦ because of the development of a
small “dead zone” which remains unfilled with material at the sharp outer corner
where the two channels intersect[6.14]
2.9.3 Effect of sample rotation between repetitive pressings
When sample is rotated between repetitive pressings, route B in which the
sample is rotated by 90◦ between each pressing and route C in which the sample is
rotated by 180◦ between each pressing. A further possibility may be introduced when
it is noted that route B may be undertaken either by rotating the sample by 90◦ in
alternate directions between each individual pressing, termed route BA, or by rotating
the sample by 90◦ in the same direction between each individual pressing, termed
route BC. The principles of these four different routes are illustrated schematically in
Fig. 2.13. In order to understand the shearing associated with these different
processing routes, it is convenient to consider the deformation of a cube passing
through an ECAP die with internal angles of ϕ =90◦ and Ψ=0◦.

Figure 2.13. Different routes of ECAP .

20
The mechanical properties of the alloy are influenced by the different textures present
after extrusion and subsequent processing by ECAP[9]. The development of low
temperature super plasticity and texture is examined in an AZ 31 Mg alloy after
extrusion and processing by ECAP.It is demonstrated that an elongation of 460% may
be attained at a temperature of 150°C, equivalent to 0.46 Tm where Tm is the
absolute melting temperature[8].This result demonstrates the potential for achieving
low temperature super plasticity[8].

Grain refinement of pure magnesium using severe plastic deformation was

investigated in order to enhance mechanical properties of the hard to deform
materials. ECAP of channel angle 90 deg and corner angle 0 deg was successful
without fracture of the magnesium work piece at 300°C.but not under 200 deg
C[9].The hardness of the ECAP processed Mg decreased with increasing ECAP
processing temperature[9].

2.9.4 Grain refinement Mechanism

Grain refinement occurs by the extension and compression of grain boundaries with

strain, combined with grains subdividing by new HAGBs forming discontinuously,

on a finer and finer length-scale as shown in fig 2.14 where (a) the formation of

arrays of equiaxed sub grains alternating with areas of elongated sub grains (b)

interaction of LAGBs with lattice dislocations resulting in progressive increase in

their disorientation (c) a nucleus in 3-D sub grain structure, and (d) rotation of (sub)

grains facilitates the transformation of LAGBs into HAGBs. Ultimately, a lower limit

is reached when the HAGB spacing approaches the sub grain size. Hence, the sub

grain size produced at a given temperature and strain rate ultimately determines the

finest grain size achievable.[5]

21
 Fig 2.14 Schematic representation of grain refinement
2.10APPLICATIONS AND ADVANTAGES OF ECAP
The major applications of ECAP include
i. Refinement of grain size by appropriate combination of extrusion and annealing.
ii. Production of filamentary microstructures from initial structures with an equiaxed
grain/ particle shape.
In comparison with traditional metalworking processes, ECAP presents several
advantages. The advantages are,
(i) Relatively low pressure and load can be used to produce extra-large, strictly
uniform and unidirectional deformations for massive products and industrial
applications
(ii) It provides the potential for various metals and alloys to achieve super plastic
characteristics at lower temperatures and high strain rates

22
(iii) It breaks up any reinforcement particle clusters, eliminates most of the defects
present in these particles, decreases their size and enhances their distribution
(iv) There is a potential for samples subjected to ECAP to associate with the
subsequent processes after ECAP without any reduction in the super plastic
properties.
(v) It is a relatively inexpensive processing method and can be used to process
conventional alloys, and can potentially be scaled up to produce large quantities of
material.

23
 CHAPTER III
EXPERIMENTAL
3.1 MODELLING AND FABRICATION OF ECAP DIE, PUNCH AND
FIXTURE SET UP
The intersecting angles of die used in this study are 120° and 90°.The 90°angle die was
available. The 120° angle die was modeled as per the existing 90° die design using Pro-E
software and manufactured. The die, punch and fixture set up are shown below.

Fig 3.1 Die fixture set up

24
 Fig 3.2 Final assembly of die, fixture and punch set up

The die and punch are made by die steel (H13) and the fixture is made by mild steel.
The channel of the die was made by milling operation. After machining the die and
punch, it was heat treated as per the ASTM standard for improving the hardness. The
heat treatment procedure is as described below.

25
 Table 3.1Heat treatment procedure of die steel
Heating From room temp to 400°C

Holding Duration-30 minutes

Heating From 400°C to 600°C

Holding Duration-30 minutes

Heating From 600°C to 900°C

Holding Duration-30 minutes

Heating From 900°C to 1050°C

Holding Duration-60 minutes

Quenching Quenching medium-Lubricating oil(room temp)

3.2 FABRICATION OF AZ 91 MAGNESIUM ALLOY

The AZ91 magnesium alloy was prepared by melting together pure Mg, pure Al,
pure Zn and Al–Mn master alloy. Melting is carried out in a steel crucible in the
resistance furnace under proper flux cover to the required temperature The melt was
poured in to a preheated mould. Sulphur dusting was carried out during pouring to
avoid burning.
3.2.1 Cleaning of materials
In order to remove the oxides sticking on the wall sand bottom of the crucible from
the previous melting the crucible was filled with water and kept for one day for
oxides to get dissolved. Then it should be cleaned with MS wire brush. All the steel
tools used for melting and pouring purpose like skimmer, starrier etc and metal ingots
were cleaned by metal wire brush. Metal ingots are then, cleaned with acetone. All
the tools and metal ingots should be preheated before use. The properly cleaned
mould should be given a graphite coat and preheated to 250 deg C in a heating oven
as shown in fig 3.3(A) for 1h just before the casting[10]

26
3.2.2Melting

Resistance box furnace was used for melting as shown in fig 3.3(B). The
preheated flux was sprinkled in the bottom and side of the cleaned crucible and was
kept inside the furnace. After the crucible reached the red hot condition, the preheated
ingots were charged in to the crucible. Initially part of the total magnesium ingots
were charged. After melting of charged ingots completed, the remaining ingots were
then immersed in to the molten metal. This kind of charging practice of metal ingots
avoids the excessive oxidation during melting. Crucible was covered with furnace lids
to minimize the air contact with the molten metal. Flux should be sprinkled over the
metal throughout the melting. Before addition of alloying elements, the top layer of
oxides was completely removed and fresh layer of flux applied. After addition, the
melt should be gently stirred for dissolution of the added elements. Again the top
oxide layer was to be removed and fresh layer of flux was applied. The melt should
be held for 10 minutes to ensure the complete dissolution of elements in to the
melt[10].The melting set up was schematically represented in fig 3.4.

A B

Fig 3.3Photograph of (A) Oven (B) Furnace

27
Flux Melting Holding time 10 min Poured at 740°C
Fig 3.4 Melting set up

3.2.3 Refining

After the complete melting of the metals in the crucible, the refining of melt should
be carried out at a temp of 720°C. Initially the top layer (oxide layer) of the melt was
removed and the melt was rigorously stirred for 2-3 minutes. Flux should be applied
during stirring. This stirring helps to mix the added flux with the melt uniformly.
After thorough mixing, the top surface of the molten melt was removed and fresh
layer of flux was applied. Then the melt is held for 10-15 minutes without
distributing, which enable the added flux react with oxides inclusions presents in the
melt and become heavier and settled down in the bottom of the crucible[10,11].

3.2.4 Pouring and casting

After the refining and settled process was over, the molten metal was poured in to the
pre heated moulds. During pouring much care should be taken to avoid the breakage
of top flux protective layer. The pouring was carried out gently without any jerk in
the melt, since excessive jerk disturbs the settled oxide inclusions in the bottom. The
flux layer near the lip of the crucible was pulled back gently by using a skimmer for
smooth flow of molten metal. Sulphur powder dusting was carried out to remove the
oxygen around the melt jet. Three fourth of the melt in the crucible was poured in to
the preheated mould. The remaining metal was poured separately as a
scrap[10,11,12].

28
Plate Mold

Skimmers

Crucible

Sulphur Dust

Fig 3.5 Casting equipments

3.3 ECAP OF AZ 91

ECAP uses a die containing two channels, equal in cross-section, intersecting at an

angle. In this study 90°and 120° are used as the intersecting angle. The casted alloy
was cut in to the dimensions of 12mmx12mmx60mm. The strain imposed on the
sample during ECAP is dependent upon both the channel angle between the two
channels, (90°&120°), and the angle defining the outer arc of curvature where the two
channels intersect. (20°).After the sample got prepared it was placed in a heat
treatment furnace for preheating to a temperature of 300°C and soaked to a duration
of 1 hour. In the mean time the die punch set up was heated to the same temperature
by a heating coil arrangement[9].Kanthal wire was used for the heating purpose. The
die punch set up temperature was measured by means of a thermocouple. After both
the material reached the required temperature, the sample was taken from the heat
treatment furnace and applied molybdenum di sulphide as lubricating agent before
pressing.

29
 Fig 3.6 EACP samples Fig 3.7 Schematic representation of Route Bc
Among the four various routes in the present study told about route Bc.ie where the
sample is rotated in the same sense by 90˚ between each pass[13].The sample was
pressed up to 3passes in 2 different die angles 90° and 120°.The photographs of two
different dies are shown in fig 3.8.

A B
Fig 3.8 Photographs of dies used for ECAP(A)120°die (B)90° die

30
 A

B C

Figure 3.9 Photographs of(A) ECAP punch, Die, Sample (B) Fixing sample in
ECAP die (C) ECAP pressing machine with the die and punch setup

3.4 HEAT TREATMENT OF SAMPLES

After completing the ECAP,the pressed samples were placed in a mild steel tray in
such a way that no piece touches others and kept inside the furnace. It was solution
heat treated for 48 h at a temperature of 410°Cfollowed by water quenching at room
temperature..A sand bed prepared using carbon char coal and dry sand dry sand with
a volume ratio 20:80 was placed in the furnace. This mixture was replaced in every

31
one hour for the better heat treatment. These samples were then aged at 200°C for
1h[10,11]

3.5 CHARACTERISATION
3.5.1 X ray diffraction
The various micro structural constituents of castings were identified using XRD. The
samples were cut from the castings and machined as small chips.XRD spectrums
were obtained using Phillips PW 1710 Powder Diffractometer

3.5.2 Microstructure analysis procedure of AZ 91

Initially the samples should be polished using different grades of emery papers of
progressively fine grades of 80, 100,220,400,600,800,1000 grits. After completing the
paper polishing, the samples are polished in a rotating disc of proprietary cloth
(Selvyte cloth) charged with a diamond paste of 6,3,and 0.25 μm particle size in
sequence as shown in fig 3.10 . Filtered kerosene is used as lubricant during cloth
polishing. Samples are gently pressed against rotation wheel[10].
3.5.2.1Chemical etching
Different kinds of etchants are tried to get a clear microstructure. After various trials,
picric acid based etchant is found to be an efficient one, which clearly revealed the
micro constituents of magnesium alloys. The etching time is found to be optimum
with 2-3 seconds[10].

Fig 3.10 Polishing machine

32
Micro structural specimens(after polishing and etching) were observed under a Leitz-
Metalloplan optical microscope. Photographs were taken at different location with
various magnification.

Fig 3.11 Optical microscope

Quantitative analysis of the microstructure is to be carried out using a Leica 2001

image analyzer in conjunction with the optical microscope as shown in the above
figure. Size of the various intermetallics and grain size of various pressings was
observed by microscope. The fields of observations were selected randomly at
different locations of the sample.

3.5.3 Micro hardness

Hardness is a measure of resistance to indentation. It is the easiest property which is

evaluated for studying the mechanical properties of engineering materials. The
Vickers hardness measurement was carried out using the fully automated CLEMAX
micro hardness tester as shown in 3.12 of square base diamond pyramid indenter and

33
the angle between the opposite face was 136°.A 50 g constant load was maintained
throughout the experiments with 10 s.The micro hardness value was taken at 5
different locations and the average was taken in to account.

Fig 3.12 Micro hardness testing machine

3.5.4 Tensile properties

The tension test is one of the most commonly used tests for evaluating mechanical
properties of the materials. The sub- standard tensile samples were cut from the as-
cast and the pressed samples to the specified dimensions as shown below. The tensile
specimens were fabricated according to the sub standards followed by the review
paper[13].The tensile test sample dimensions are shown in fig 3.13. Room
temperature tensile tests were performed using an INSTRON 8810 Universal Testing
Machine as shown in fig 3.15 at a constant cross head speed of 2mm/min.

34
Fig 3.13 Tensile sample dimensions Fig 3.14 Photograph of tensile samples

Fig 3.15 Tensile testing machine

35
3.5.5 Fractured surface study

Scanning Electron Microscope (SEM) consists of an energetically well defined,

highly focused beam of electrons scanned across a sample. The microscope uses a
LaB6 source and is pumped using turbo and iron pumps to maintain the highest
possible vacuum. In a typical SEM, electrons are thermionically emitted from a
tungsten or lanthanum hexaboride (LaB6) cathode and accelerated towards the anode;
alternatively electrons can be emitted by field emission (FE). Tungsten is used
because it has the highest melting point and lowest vapor pressure of all metals,
thereby allowing it to be heated for electron emission. The electron beam has energy
ranging from few hundred 15eV to 30 KeV, is focused by one or two condenser
lenses into a beam with a very fine focal spot sized 1nm to 5nm. The beam passes
through pairs of scanning coils in the objective lens, which deflect the beam in a
raster fashion over the sample surface. The electrons are in elastically scattered by
the sample atoms. The primary electron beam effectively spreads and fills a tear drop
shaped volume, known as interaction volume, extending from less than 100nm to
around 5µm into the surface. Interactions in this regions lead to a subsequent
emission of electrons which are then detected to produce an image. X-rays which are
also produced by the interactions of electrons with the sample may also be detected in
a SEM equipped for energy dispersive X-ray spectrometer or wavelength dispersive
X-ray spectrometer. Secondary electron imaging works on the principle that this
electron beam generates a splash of electrons with kinetic energies much lower than
the primary incident electrons, called secondary electrons. Because of their low
energies and low penetration depth, the detection of secondary electrons as a function
of primary beam position makes it possible to attain high magnifications and high
resolutions for imaging the areas of interest.

The SEM has compensating advantages, including the ability to image a

comparatively large area of the specimen; the ability to image bulk materials; and the
variety of analytical modes available for measuring the composition and nature of the
specimen. Depending on the instrument the resolution can fall somewhere between
less than 1nm and 20 nm.

36
To study the micro mechanism of fracture during tensile test, samples were cleaned in
ethanol and the fractured surfaces were examined in a JEOL, JSM 35C Scanning
Electron Microscope operating at an accelerating voltage of 15-30KeV as shown in
fig 3.16..In the present study the 3rd pass sample in both 120° and 90° that gave
maximum UTS has been taken for SEM analysis.

Fig 3.16 Scanning electron microscope

37
 CHAPTER IV

RESULTS AND DISCUSSIONS

4.1 X-RAY DIFFRACTION

The XRD results shows peaks for only two phases α-Mg and β- Mg17Al12. The results
were obtained as graphs having Bragg’s angle (of 20° to 80°) at abscissa and intensity
in Angstrom units at ordinate. Major peak for β phase at 2θ value of 36.5 can be seen
very clearly. Other intermetallics might have formed but not observed in the XRD
results which may be due to the volume fraction of these intermetallic phases may be
well below to the detectable limit in XRD.

Fig 4.1 XRD results of AZ 91

4.2 MICROSTRUCTURE ANALYSIS OF AZ91 ALLOY

The microstructure of the as cast sample at different locations was taken is shown in
the fig.4.2. By analyzing the microstructure we can see three different phases. These
three different phases are primary α-Mg, massive precipitates which is known as β-
Mg17Al12 intermetallic and a dark area surrounding the massive sized particles which
is eutectic α-Mg. Both the massive β- Mg17Al12 intermetallic and dark phase together
is known as eutectic.

38
 A0-As cast A1-120° 1st pass

A2-120° 2nd pass A3-120° 3rd pass

Fig 4.2 Microstructure of AZ 91 alloy and 120°ECAPed sample
By analyzing the microstructure of the120° pressed sample it can be seen that gradual
breakage of phases during each pressing. Among the three microstructure of the
pressed sample, maximum breakage was seen after 3rd pass.

The microstructure of the 90° pressed sample also gives the same type of grain
refinement. Due to larger strain induced, the micro structure of the 90° pressed
sample shows maximum grain refinement than 120° pressed sample. The three
microstructures of the 90° pressed sample reveals that a gradual breakage of phases
occurred from 1st pass to 3rd pass. For getting a clear picture of grains, the pressed
sample was heat treated.

39
 A0-As cast B1-90° 1st pass

B2-90° 2nd pass B3-90° 3rd pass

Fig 4.3 Microstructure of AZ 91 alloy and 90°ECAPed sample

4.3 MICROSTRUCTURE OF HEAT TREATED SAMPLE

The normal sequence of heat treatment is solution heat treatment at 410°C for 48hrs
and aging temperature of 200°C. With as cast microstructure the grain boundaries of
Mg-Al alloys are not revealed property. The normal procedure to visualize the alloy is
to solution treatment. During solution treatment, dissolution of eutectic Mg17Al12 is
slow mainly due to its massive size. With 24 h of solution treatment, complete
dissolution of this takes place; however, 48 h of solution treatment is normally
required to obtain completely homogenous mixture of Al in Mg matrix. During
solution treatment at 410°C for 48 h the Mg17Al12 intermetallic gets dissolved . Aging
treatment enhances delineation of grain boundaries,

40
 A0-As cast A1-120°1stpass

A2-120° 2nd pass A3-120° 3rd pass

Fig 4.4 Microstructure of heat treated AZ 91 alloy and 120°ECAPed sample

By studying the microstructure we can see new grains are formed. During each
repetitive pressing grains are more refined. Among the above microstructures the 3rd
pass sample shows maximum grain refinement. The first pass divides the large grains
into arrays of sub grains that are well delineated and where all of the grain boundaries
have low angles of disorientation. A second pass through the die, following a rotation
by 90° between passes, leads to the microstructure where the sub grain structure has
broken into an array of ultrafine grain. The disorientations across the grain boundaries
have increased with increasing strain. After 3rd pass there is no longer any evidence
for the initial formation of the sub grain bands. Instead, the microstructure consists of
an essentially equiaxed array of grains, so that some of the grain boundaries now have
high angles of disorientation.

41
The average grain size is measured by using linear intercept method. In this method,
one or more lines are superimposed over the structure at a known magnification. The
true line length is divided by the number of grains intercepted by the line. This gives
the average length of the line within the intercepted grains. This average intercept
length will be less than the average grain diameter. By measuring the grain size
obtained, 120° die shows a decrease of average grain size from 130µm to 40µm and
the 90° die shows a decrease of 130µm to 25µm. Average grain size values after
ECAP are described in table 4.1

A0-As cast B1-90°1stpass

B2-90°2nd pass B3-90°3rd pass

Fig 4.5 Microstructure of heat treated AZ 91 alloy and 90°ECAPed sample

42
 Table 4.1 Variation of grain size in ECAPed sample
SAMPLE GRAIN SIZE(µm)
120 90
AS CAST 130 130
1st PASS 100 70
2nd PASS 80 50
3rd PASS 40 25

From the table it is clear that the average grain size reduction of 90µm is achieved in
120°die and a grain size reduction of 105µm is achieved in 90°die.
4.3 MICRO HARDNESS
The hardness is measured from at least five locations of the same condition and the
average value is reported This increase in hardness after ECAP is attributed to the
work hardening caused by the formation of sub grain bands and the increase of
dislocation density occurring with the shear deformation in the initial grain interior.
The hardness decreases with increasing the ECAP temperature, because the work
hardening is limited more at higher temperatures by the occurrence of the dynamics
recovery, a thermally activated softening mechanism.
Table 4.2Variation of micro hardness value with respect to no. of passes
SAMPLE
MICRO HARDNESS (H V)
120 90
AS CAST 90 90

1st PASS 157 170

2nd PASS 164 193

3rd PASS 170 213

43
The hardness value shows that there is a gradual increase of value from the as cast
sample.Compared to both 90° and 120°die, 90° die shows maximum micro hardness
value because maximum grain refinement was occurred in 90° die. It is observed that
in the 120°die an increase in hardness value of 80 HV from as cast to 3rd press sample
where as in 90°die an increase of 123 HV is obtained.

4.4 TENSILE PROPERTIES

The reduction of the grain size and the increase of the dislocation density results in
the increase of the tensile strength. The following fig shows Ultimate tensile
strength(UTS) values of ECAPed samples both for 120 deg and 90 deg.The 1 st,2nd
and 3rd pressings are represented by A1,A2,A3 and B1,B2,B3 respectively. Here
again the UTS obtained is high for 90° die.

.
Fig 4.6 Comparison of UTS with respect to number of passes (120°)

44
 Fig 4.7 Comparison of UTS with respect to number of passes[90°]

Grain refinement by ECAP can lead to a unique combination of strength and ductility
in metallic materials. Such superior mechanical properties are highly desirable in the
development of advanced structural materials for the next generation. However, the
achievement of these properties is associated with the tailoring of specific
microstructures which, in turn, are determined by the precise processing regimes and
the nature of any further treatments.
The UTS of the as cast sample was measured as 177MPa.The value of the UTS in the
120° pressed samples corresponding to 1st, 2nd and 3rd pass are185,198 and 210 MPa
respectively. Similarly the value of the UTS in the 90° pressed samples corresponding
to 1st, 2nd and 3rd pass are 190,210 and 236 MPa. For the pressed sample there is a
gradual increase in the Ultimate tensile strength.It shows that the UTS is increasing
after each pass.After 3rd pass the total UTS increase of 19% was observed in 120° die
angle and an increase of 33% was observed in 90° die.This is because more grain
refinement is occurred in 90° die.
Concerning the origin of strengthening phenomenon, it has been suggested that it is
associated with an increase in the fraction of high-angle grain boundaries with

45
increasing straining and with a consequent change in the dominant deformation
mechanisms due to the increasing tendency for the occurrence of grain boundary
sliding and grain rotation.

4.5 FRACTOGRAPHY

120°3rd pass 90°3rd pass

Fig 4.8 Tensile fractography
The tensile fractured SEM fractgraph has been taken. Fig. 4.8shows the SEM
fractographs of the tensile fractured surface of 3rd pass ECAP processed AZ91 alloy
at 120° and 90°. Various dimples and cracks which occurred during fracture can be
identified from the above figures. Dimples represent the ductile fracture which is the
property of soft metal matrix. Disk shape continuous and discontinuous precipitates
with rod-like shape formed during ECAP and they play an important role during
deformation. Fracture is mostly initiated along them and the fine dispersion of
precipitates could improve ductility.
The discontinuous Mg17Al12 phase initially has a long rod like shape which are
broken during ECAP and their dispersion is relatively homogenous. The presence of
large amount of dimples in 90°die 3rd pass sample shows that the material is more
ductile compared to 120° die 3rd pass sample.

46
 CHAPTER 5
CONCLUSION
In this work, ECAP of cast AZ 91 alloy both 120°die and 90° die has been
carried out. Their effects on microstructure, heat treatment, micro hardness,
tensile properties and fractography are studied. This chapter summarizes all
the major observations and conclusions drawn from this study

 XRD results shows the presence of Mg17Al12 phase. Other intermetallics

might have formed but not observed in the XRD results which may be due to
the volume fraction of these intermetallic phases may be well below to the
detectable limit in XRD.
 α Mg, β- Mg17Al12 and eutectic α-Mg are seen by studying the microstructure
as cast AZ91. During solidification the first formed phase is called α phase
and this is primary and the second formed phase is called β phase and this is
secondary.
 Successful grain refinement occurred by using ECAP at 2 various die angle
120 and 90. . Maximum grain refinement was occurred in 3rd pass of the
sample. Compared to 90° and 120°die maximum grain refinement was
occurred in 90° die, because the strain induced is more in the case of 90° die
than 120° die.
 The grains has been seen clearly in the microstructure after the heat treatment
because the dissolution of Mg17 Al12 in to αMg. Average grain size reduction of
90µm was obtained in 120° die and a reduction of 105µm was obtained in 90°
die.
 Ultimate tensile strength and micro hardness gets improved compared to as
cast sample and it also increases by increasing the number of passes. The UTS
of as cast sample was obtained as 177MPa.After 3rd pass the UTS was
increased from 177MPa to 215MPa in 120° die and from 177MPa to 236MPa
in 90° die. The micro hardness value of as cast sample was obtained as
90HV.After 3rd pass the value increased from 90HV to 170 HV in 120° die

47
 and from 90HV to 213 HV in 90°.The maximum UTS and micro hardness
value was obtained in 90° die because of maximum grain refinement.
 Fractured surface study reveals that the material is having more dimples
represents the ductile fracture which is the property of soft metal matrix. More
dimples are present in 90°pressed sample than 120° pressed sample. It
represents 90°pressed sample is more ductile than 120° pressed sample.

48
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LIST OF PUBLICATION

 “Microstructure and Mechanical properties of Equal channel angular

processed AZ91 Magnesium alloy”, P Joffin Jose, K.K Ajith
th
Kumar,M.Bhramakumar,R Ajith,U.T.S.Pillai, presented in 12 National
Conference on Technological Trends(NCTT), College of Engineering,
Trivandrum

51