M.

Tech Phase-I Report

Comparative Study on the Evolution of Microstructure

and Changes in Mechanical Properties of Al-alloy
during Post Heat Treatment of Plate-type Fuel

Submitted in partial fulfillment of the requirements for the degree of

Master of Technology

Submitted By

Divya Kohli
(10311008)

Supervisor

Prof. I. Samajdar Dr.G.J.Prasad

(IIT Bombay) (B.A.R.C.)

Department of Metallurgical Engineering and Materials

Science
Indian Institute of Technology, Bombay
Oct-2011
 ABSTRACT

Plate fuels with Al clad plates and U3Si2 as dispersoid in aluminum matrix

was studied with surrogate ceramic material (Y2O3) dispersed in Al matrix

to model the roll bonding and annealing behaviour of the actual fuel meat.

Roll Bonded (85% thickness reduction) plate fuel were recovered at 200 0C

for different times (15min, 30 min. and 60 min.). The recovery kinetics,

studied through a combination of X-ray line profile analysis and high

resolution electron diffraction, were best represented by logarithmic

relationship. In-grain misorientation in recovered bands was increasing.

Strain induced boundary migration (SIBM) or uniform movement of

boundaries into neighbouring orientations was leading to coarsening of

bands. Such uniform movement of boundary was incapable of reducing

internal defect density. Bond strength as a function of annealing time (15

min, 30 min., 1 hr) and temperature (2000C, 3000C, 4000C and 5000C)

nvestigated to find optimum post heat treatment cycle.

 CONTENTS

Page No.

Abstract (i)

1. Introduction

1.1 Background 1
1.2 Objective 2

2. Literature review

2.1 Fuel Selection 3

2.2 Solid state bonding 4
2.3 Roll bonding process 4
2.4 Parameters affecting bonding 5
2.5 Bonding mechanisms 6
2.6 Effect of post-heat treatment on bond strength 6
2.7 Recovery of Roll Bonded Plates 7
2.7.1 Recovery mechanisms 7
2.7.2 Measurement of recovery kinetics 9
2.7.3 Structural changes during recovery 10
2.7.4 Orientation dependent recovery 11
2.7.5 Strain induced grain boundary migration (SIBM) 11

3. Experimental Methods

3.1 Materials 16
3.2 Fabrication of the fuel plates 16
3.3 EBSD measurements 17
3.4 X-ray Diffraction 17
3.5 Hardness Measurement and Heat Treatment 21
3.6 Bond Strength 21
4. Result and Discussion

4.1 Direct Observation of Recovery Phenomena 23

4.1.1 EBSD measurements 23
4.1.2 Hardness 28
4.1.3 FWHM and Dislocation Density 29
4.1.4 Residual Stress 32
4.2 Bond Strength 34
4.2.1 Annealing time 34
4.2.2 Annealing temperature 35

5. Conclusion 37

6. Future Work 38

List of References
 LIST OF FIGURES

Figure Figure caption Page No.

No

2.1 Schematic of Roll bonding 5

2.2 Schematic of successive dislocation annihilation mechanisms 8

2.3 Schematics showing dislocation structure changes during 11

recovery-random dislocations tangles through cell structure to
subgrains

2.4 (a) SIBM of a boundary separating a grain of low stored 13

energy (E1) from one of higher energy (E2), (b) dragging of
the dislocation structure behind the migrating boundary, (c)
the migrating boundary is free from the dislocation structure,
(d) SIBM originating at a single large subgrain

3.1 Illustration of picture frame technique of preparing plate type 16

fuels.

3.2 X-ray diffractogram of Al used for Dislocation density calculations 18

3.3 (a)Schematic arrangement for residual stress measurement, (b) 20

Experimental set-up for residual stress measurement

3.4 Plot of dhkl (ψ, φ) vs. Sin2ψ for residual stress measurement 20

3.5 XRD plot showing a schematic of bi-axial residual stress 21

measurement

3.6 (a) Geometry of test specimen (b) Schematic of bond test, (c) 22
Experimental set-up of bond strength measurement

3.7 Typical plot of peel test 22

4.1(a) EBSD images, in inverse pole figure notation, of the deformed 24
and recovered (200C) plate fuel. Points of low (<0.1) CI are
marked in black

4.1(b) IQ map showing sub boundaries (red color) in the area shown 25
by the inset in Fig.4.1 (a)

4.2 (a) Subgrain diameter as a function of annealing time, (b), (c) 25

IQ map showing sub-boundaries (red color)

4.3 Low angle (2-150) boundary density as a function of annealing 26

time for sample recovered at 2000C

4.4 (a) Average deformed band thickness, as a function of 27

annealing time for samples recovered at 2000C. Error bars
represent standard deviations of the measured data – as
obtained from multiple manual measurements. (b,c) EBSD
images: describing significant changes in band thicknesses.

4.5 Average misorientation as a function of annealing time 27

4.6 Variation of micro-hardness with prior-deformation and 28

recovery time. Error bars represents standard deviations of the
measured data as obtained from multiple measurements.

4.7 Schematic diagram showing the operation of an in-plane shear 29

stress at the boundary between the Al and Al(Surrogate)
[Al(S)] layers thereby creating a tensile drag force on
Al(S)[28].

4.8 Dislocation density, from the respective peaks ((111) and 30

(200)), as a function of annealing time for samples annealed at
(a)2000C (b)3000C. Error bars represents the
measurement/analysis uncertainties.
4.9 Dislocation density, from the respective peaks ((111) and 31
(200)), as a function of annealing time for samples annealed at
(a)2000C (b)3000C. Error bars represents the
measurement/analysis uncertainties.

4.10 Normal residual stress from the respective peaks ((111) and 32
(200)), as a function of annealing time for samples annealed at
(a)2000C (b)3000C

4.11 Shear Residual Stress from the respective peaks ((111) and 33
(200)), as a function of annealing time for samples annealed at
(a)2000C (b)3000C.

4.12 Variation of bond strength with annealing time 35

4.13 Variation of bond strength with annealing temperature 36

 LIST OF ABBREVIATIONS

Al Aluminum
U3Si2 Uranium Silicide
Y2O3 Yttria (Yttrium Oxide)
LEU Low enriched uranium
HEU High enriched uranium
RERTR Reduced Enrichment for Research and Test Reactor
MWth Megawatt thermal
MWe Megawatt electrical
EBSD Electron Backscatter Diffraction
XRD X-ray Diffraction
ASTM American Standard of Testing Materials
RD-ND Rolling Direction-Normal Direction
SEM Scanning Electron Microscope
TSL Tex SEM Ltd
CI Confidence Index
SIBM Strain Induced Boundary Migration
LAGB Low angle Grain Boundary
HAGB High angle Grain Boundary
DD Dislocation density
 CHAPTER 1
Introduction

1.1 Background

Research in Plate type reactors has gained importance in the recent past owing to the low
temperature operation, even below 100°C which has made the use of pressurized water
redundant. Also modern mobile reactors like the one used in nuclear submarines are
based on plate fuel type reactors. The most important goal for the nuclear fuel designers
was to develop a fuel cycle which is based on low enriched uranium (LEU < 20% U235)
rather than high enriched uranium (HEU > 85% U235) under the Reduced Enrichment for
Research and Test Reactor (RERTR) program, which was launched in the late 1970‟s to
reduce the risk of nuclear proliferation[1].

The APSARA research and test reactor, which is located in BARC, India, is under up-
gradation and the project of developing LEU based fuel is a part of the program. At
present this reactor uses plate type fuel of HEU in the form of UAl3 dispersed in
aluminum matrix. With a view to develop an alternate LEU fuel, work has been initiated
in BARC to develop plate fuels with U3Si2 as dispersoid in aluminum matrix clad in Al-
alloy because of its stable irradiation behavior as compared to other several intermetallic
compounds of uranium and also has comparatively higher loading of Uranium. This new
fuel will enable to increase the reactor power from 1 MWth to 2 MWth[2]. The final
electrical output in MWe depends on the thermal efficiency of the reactor.

The thermal efficiency depends on the effectiveness of metallurgical bond between fuel
and the cladding. There are a variety of bonding methods used in the industry which
includes explosion cladding, forging, diffusion bonding, friction welding, laser cladding,
extrusion and roll bonding. However, the more commonly used cladding process is by
laser cladding, extrusion and roll bonding. The cost of laser cladding process limits its
use for fabrication of complex parts and cladding on unreachable areas. For bonding

1
techniques by extrusion and rolling, it has been find out that the roll bonding process
offers more advantages in terms of cost, productivity and flexibility of net-shape
forming with less occurrence of defects [3].

In view of the above and also since it allows the use of LEU fuel in place of HEU while
keeping the fuel design same , roll bonding technique is preferred for plate fuel
fabrication. Thus, roll bonding is the most effective way of plate fuel fabrication due to
the better clad-meat interaction or metallurgical bond formation leading to effective heat
withdrawal from the core.

1.2 Objective

The current project work involves the study of roll bonding in plate fuels with sandwich
geometry. The roll bonding characteristics of Al clad plates with U3Si2 as dispersoid in
aluminum matrix as the fuel meat is to be studied with surrogate material.

The project is planned to study the roll bonding characteristics with surrogate ceramic
material like Y2O3 dispersed in Al matrix to model the roll bonding and annealing
behaviour of the actual fuel meat.

The objectives of the current work are enlisted below:-

 To study the bond strength as a function of annealing time (15 min, 30 min., 1 hr,
2 hr, 4hr and 8hr), temperature (2000C, 3000C, 4000C and 5000C) and grain size
with Y2O3 dispersed in Al matrix type meat in between Al 6061 clad plates.
 To compare the bonding characteristics and finding an optimum post heat
treatment cycle.
 Direct observations to study the effect of annealing time (15 min, 30 min. and 60
min.) and temperature(2000C ,2500C, 3000C, 3500C) on recovery (strain induced
boundary migration, misorientation, residual stress and dislocation density) of roll
bonded plates.

2
 CHAPTER 2
Literature Review

2.1 Fuel Selection

Till mid 1970s most of the research and test reactors worldwide were using high
enriched uranium (HEU > 85% U235) in plate type dispersion fuel elements; generally
consisting of UAlX (mainly UAl3) or U3O8 dispersed in aluminum matrix and clad in an
Al-alloy [2]. In the late 1970s the Reduced Enrichment for Research and Test Reactor
(RERTR) program was initiated to address the concern related to proliferation and
diversion issues. After this the most important goal for the fuel designers was to develop
a fuel cycle which is based on low enriched uranium (LEU < 20% U 235) rather than high
enriched uranium (HEU > 85% U235)[2].

This can be achieved either by increasing the fuel loading or by using higher uranium
density compounds/alloys. The most common fabrication techniques which allow the
use of LEU fuel in place of HEU while keeping the fuel design same is roll bonding
technique for plate fuel fabrication[4]. Plate type fuel geometry (fabricated by roll
bonding method) does not allow the fuel particle volume to exceed 55 volume % [4].
Limitation on the increase of fuel particle volume percentage in the fuel meat implies the
only option to increase the heavy metal (i.e. uranium) density in the fuel itself. This can
be achieved by using high density uranium compounds or alloys as fuels. There are
several intermetallic compounds of uranium which were considered because of their
higher heavy metal density. The U3Si compound and intermetallic compound U6Me
where Me can be Fe, Ni, Mn or Ge gives higher uranium metal density. But their high
swelling rate (break away swelling) even under low burn up condition is the major
disadvantage[5]. The irradiation studies show their poor irradiation behavior for thin
plate type dispersion fuel geometry due to the breakaway swelling under relatively low
burn ups. On the other hand U3Si2 fuel particles in aluminum matrix clad in Al-alloy
shows stable irradiation behavior. Here the maximum uranium metal density in the fuel

3
meat one can achieve is in the range from 4.8 to 6.0 g/cm3[1]. So large number of
current research work focuses on the development of U3Si2 dispersion type fuel in plate
fuel type reactors by roll bonding technique.

2.2 Solid state bonding

The solid-phase welding technique can be used on a variety of materials, which may be
the same, possessing identical attributes, or may be different, possessing widely varying
mechanical and metallurgical properties. Roll Bonding is a type of solid-phase welding
process where bonding is established by joint plastic deformation of the metals to be
bonded. Bonding is obtained when surface expansion has cause contaminant free areas,
termed virgin metal surfaces, to be exposed and extruded the virgin material through the
cracks of the fractured covering layer so establishing contact and bonding between the
opposing virgin surfaces [6].

2.3 Roll bonding process

The schematic illustration of roll bonding for the production of layered materials is
presented in Fig. 2.1. In this process, two or more sheets, plates or strips of metals or
alloys are stacked together and then passed through a pair of rolls until an appropriate
deformation is achieved to produce a solid state bonding between the original individual
metal pieces. Before roll bonding, the surfaces to be bonded must be properly cleaned
and prepared to remove any surface layers [7]. The removal of contamination layers
from the surfaces of the two metals is usually carried out by chemical and mechanical
treatments. Previous investigations have shown that the function of scratch brushing is
not only to clean, but also to form locally a brittle layer on the metal surfaces by work
hardening the surface layer [8,10].

During bonding, a high reduction in the thickness of the materials (capable of up to 50%
or more in a single rolling pass) is achieved under a high pressure at the roller [7]. The
high reduction generates a great amount of heat and creates virgin surfaces on the
materials being bonded. A bond (normally a mechanical bond) in the layered composite

4
is thus obtained through interfacial mechanical and atomic affinity between the two
metals. Roll welding can accompany heating of strips before rolling processes that cause
the reduction of required energy for bond formation [9,10]. In general, an annealing
treatment is performed after rolling in order to increase the bond strength because the
annealing treatment is expected to develop a strong metallurgical bond at the original
interface of the metals.

Fig. 2.1: Schematic of Roll bonding [7].

2.4 Parameters affecting bonding

Many research studies on the parameters governing bonding have been carried out to
understand the complex nature of the bonding mechanisms, and the conditions of the
process have been well defined empirically. It has been reported [7] that the roll bonding
of metals is affected by various factors, such as the amount of deformation, the type of
metal under consideration, the temperature of bonding, the amount of enforcement
pressure, the time of bonding, the metal purity, the lattice structure the surface
preparation conditions, the geometry of the deformation zone (shape factor), the stacking
sequence, the number of layers, the layer thickness and the type of post-heat treatment.

5
2.5 Bonding mechanisms

Over the past decades, many attempts have been made to explain the mechanism of
bonding [6,7,10,11]. Till now, four theories have been proposed to explain the
mechanism of roll bonding, i.e. the film theory, energy barrier theory, diffusion bonding
theory and recrystallization theory. According to film forming theory [6]:

(a) Fresh metal surface is exposed due to deformation

(b) At a sufficiently high value of deformation, contact bonding between the sheets
is obtained
(c) Work-hardened surface layer or oxide film is fractured
(d) Virgin metals is extruded through the cracks which plays very important roles in
the real contact between metals

Such a mechanism has been confirmed by optical and scanning electron microscopies.
Therefore the metal bonding mechanism involves three-stage process of (i) development
of physical contact, (ii) activation of the surfaces in contact and (iii) interaction within
the materials being bonded. The mechanical bond between the metals first develops
during rolling and then a strong metallurgical bond develops at the interface of the
metals during following the heat treatment[7].

2.6 Effect of post-heat treatment on bond strength

The post heat treatment of roll bonded plates involves annealing treatment which is
performed after rolling in order to increase the bond strength because the annealing
treatment is expected to develop a strong metallurgical bond at the original interface of
the metals [7]. Roll Bonding followed by heat treatments has been carried out for
aluminum, copper and steel in the temperature range of 50–9000C depending on the type
of metal [7,11,12]. In all cases, it has been shown that short-time heating at low
temperatures can produce an increase in bond strength before the onset of recovery and
recrystallization. The degree of improvement was marked for bonding achieved with a
small deformation, and it was suggested that thermally activated short-range atomic
movements were responsible for producing an improved bond. If the metallic regions are

6
only partially bonded, heat treatment will complete bonding. If the oxide film is soluble
in the metal, the treatment at a sufficiently high temperature will cause complete failure
of the interface. In addition, brittle phases will be formed and will grow at the contact
interface for some metals with increasing temperature; thus, an optimum time-dependent
annealing temperature will be determined in the metals, achieving suitable formability
and bond strength. Thus, the post heat treatment has a strong impact on bond strength of
plate fuels.

2.7 Recovery of Roll Bonded Plates

The post heat treatment of plate fuels involves annealing of roll bonded plates which
occurs by the processes of recovery and recrystallization. Since aluminum is having high
stacking fault energy, recovery often involves subgrain growth, which generally occurs
uniformly throughout the microstructure [13-16]. In contrast, recrystallization usually
occurs in a non-homogeneous manner through the nucleation and growth of new grains.
Further lowering of the energy of the material may subsequently occur by grain growth.

The recovery processes which occur during the early stages of the annealing of
deformed metals are probably not as well understood as the subsequent processes of
recrystallization and grain growth [14]. The roll bonded microstructure is characterized
by sub-micrometer lamellar structure and the lamellar boundary spacing decreases and
the misorientation across the lamellar boundaries increases with increasing rolling
strain[17]. On annealing, the main recovery process is then sub-grain growth, which
occurs by the migration of low angle grain boundaries [14]. Subgrain growth in regions
of the microstructure where there are large orientation gradients may also lead to the
initiation of recrystallization.

2.7.1 Recovery mechanisms

The various mechanisms of recovery include (in order of increasing difficulty):

(a) Annihilation of point defect (vacancies and interstitials) by diffusion to sinks

such as dislocations,

7
 (b) Mutual dislocation annihilation (closely spaced dislocations of opposite sign, or
dipoles, which require small amounts of dislocation climb and/or cross slip),
(c) Organization of free, random dislocations into dislocation walls or sub-
boundaries (polygonization) and
(d) Coalescence of sub-boundary walls during subgrain growth (Fig.2.2).

Fig. 2.2: Schematic of successive dislocation annihilation mechanisms [18].

There is no clear demarcation in recovery mechanisms as they often operate

simultaneously [18]. For example, it is impossible to distinguish the collapse of diffuse
dislocation cells into well-defined subgrain boundaries and subgrain growth. This is one
reason why recovery is difficult to treat analytically. Also, the mechanisms of the later
stage of recovery, e.g. the formation of welldefined subgrains, are often the first stages
of recrystallization nucleation which can lead to rapid recrystallization, stopping any
further recovery. Finally, these fundamental mechanisms are also very sensitive to a
wide variety of material parameters and processing conditions, such as deformation,
temperature, etc[18].

Solute atoms has a major role in reducing defect mobility and therefore recovery
kinetics. For example, deformed ultrahigh purity metals can recover at about 0.2Tm and
start recrystallizing at 0.3Tm. Solute atoms in commercial alloys push recovery and
recrystallization temperatures to 0.4 and 0.6Tm, respectively Second phase particles,
particularly as very fine distributions, will also inhibit recovery by pinning dislocations.

8
2.7.2 Measurement of recovery kinetics

The process of recovery involves several concurrent/consecutive mechanisms,

formulations of all the factors affecting recovery and the heterogeneity of recovery are
difficult and a comprehensive formulation does not exist. Two empirical relationships
are, however, often used to express the overall kinetics of recovery which are given
below:

Type 1: 𝑑𝑋 −𝑘1 X= k1’-k1lnt ………………. …(2.1)

=
𝑑𝑡 𝑡

Type 2: 𝑑𝑋 X(1-m) -X0(1-m) = (m-1)k2t ……… ……….(2.2)

= −𝑘2 𝑋 𝑚
𝑑𝑡

where X is the fraction recovered (or change in recovery-dependent parameters –

mechanical properties, resistivity or enthalpy), t is the annealing time and k1, k2 and m
are the constants (k1 and k2 often scale with the activation energy of self-diffusion). Both
relationships have been reported during recovery of single and polycrystalline metallic
materials, but type 2 tends to be applicable for the special cases of single crystals with
uniform substructures (and single mechanisms). Type 1 empirical kinetics is more
typical of the complexities of deformed industrial alloys, where several recovery
mechanisms can operate.

A more physically based kinetics analysis developed by Nes [16], considers that the
activation energy for the process increases during recovery as the internal stress, or the
driving force, decreases. The easier, low energy, processes operate first and the higher
activation energy mechanisms later, up to the value expected of atomic diffusion. If the
activation energy for the process is written QF (X ) and that for diffusion Qd then

𝑑𝑋 𝑄𝑑 −𝑄𝐹 (𝑋)
= −𝑐𝑒𝑥𝑝 − … … … … … … … . . (2.3)
𝑑𝑡 𝑘𝑇

If QF(X ) is a linear function, this gives a logarithmic time dependency for recovery of
the form

9
 𝑘𝑇
𝑋 = 1− ln 1 + 𝐵𝑡 … … … … … … … … (2.4)
𝐴

where A and B are constants. This is similar to the type 1 kinetics.

2.7.3 Structural changes during recovery

Firstly there is rapid loss of point defects, apart from it, the main structural changes
taking place during recovery can be categorized as:

(a) Rearrangement of dislocations into cellular structures (for high-SFE materials

and most hot-deformed metals, this occurs simultaneously with deformation).
(b) Elimination of free dislocations within the cells.
(c) Collapse of the complicated dislocation cell walls into neat subgrain boundaries
–mostly by annihilation of excess or redundant dislocations and rearrangement of
the others into low-energy configurations (Fig. 2.3).
(d) Subgrain growth: During continued annealing, an increase in subgrain size is
theoretically expected since it leads to a reduction of internal energy. The
experimentally observed kinetic relationships are usually written

𝑑 𝑛 − 𝑑0𝑛 = 𝑘3 𝑡 ………………………..(2.5)

where d and d0 are the final and initial subgrain size, n, and k3 are constants. While k3 is
strongly temperature-dependent (through the activation energy), values of n between 2
and 7 have been reported.

It has been found [19] that where sub-boundary mobility is the highest i.e. in high-
purity metals and at high temperatures, n value is found to be lower. The n exponent
may vary due to changes in the subgrain misorientation [19]. Both average
misorientation and the misorientation spread are reported to drop slightly and then
remain stagnant during recovery, though there is also evidence of misorientation
increase with recovery. A possible explanation is the role of orientation gradients, which
tend to increase the average misorientation.

10
Fig.2.3: Schematics showing dislocation structure changes during recovery-random
dislocations tangles through cell structure to subgrains [19].

2.7.4 Orientation dependent recovery

Another important aspect of recovery, with direct implication to recrystallization, is the

issue of orientation dependence. This is also the least understood. Differences in stored
energies, or in dislocation substructure, are often related to differences in Taylor factor
[18] and also to differences in the so-called „textural softening‟ [18]. Both are, however,
related more to deformation than to recovery. The classical example is „recovery‟ in
rolled Cube {001}<100> oriented grains of fcc metals. In this situation, the Burgers
vectors of the active edge dislocations are perpendicular to each other, a particular case
which avoids strong dislocation interactions and so facilitates rapid Cube recovery [18] .

2.7.5 Strain induced grain boundary migration (SIBM)

The migration of low angle grain boundaries (LAGB) and high angle grain boundaries
(HAGB) plays a central role in the annealing of cold worked metals [19,20]. Low angle

11
boundary migration occurs during recovery and during the nucleation of
recrystallization, and high angle boundary migration occurs both during and after
primary recrystallization. Boundaries migrate by means of atomistic processes which
occur in the vicinity of the boundary [20]. The boundaries move in response to a driving
pressure (P) which generally arises from stored dislocations or from the energy of the
boundaries in the material, and in most cases it is expected that the velocity of the
moving boundary (v) will be given by an equation of the form

V= MP ……………………(2.6)

where M, the boundary mobility, is usually assumed to vary with temperature according
to

M = M0 exp[-Q/RT] ……………………(2.7)

where M0 is a constant, T the absolute temperature, Q the activation energy for boundary
migration and R is the gas constant. There may be situations in which M is dependent on
P, in which case equation 2.6 will not be valid, and examples of this might be associated
with changes of migration mechanism or boundary structure, and in some cases, low
angle boundaries are predicted to exhibit such behaviour [20].

The process for creating a new recrystallised grain by the bulging out of an existing
grain boundary within the deformed structure is described as strain induced boundary
migration, often now as SIBM. It involves the bulging of part of a pre-existing grain
boundary, leaving a region behind the migrating boundary with a lower dislocation
content as shown schematically in Fig. 2.4. A characteristic feature of this mechanism is
that the new grains have similar orientations to the old grains from which they have
grown.

12
Fig. 2.4: (a) SIBM of a boundary separating a grain of low stored energy (E 1) from one
of higher energy (E2), (b) dragging of the dislocation structure behind the migrating
boundary, (c) the migrating boundary is free from the dislocation structure, (d) SIBM
originating at a single large subgrain[19].

The driving force for SIBM is usually presumed to arise from a difference in dislocation
content on opposite sides of the grain boundary. This could result directly from the
deformation process, because it is known that the dislocation storage rate may be
dependent on grain orientation and may also be different in the boundary regions. The
kinetics of the process were first analysed by Bailey and Hirsch [21]. In figure 2.4a, if
the deformed grains have stored energies of P1 and P2 and P1<P2, then the driving force
is provided by the energy difference ∆P=P2-P1. If the bulging boundary is a spherical
cap of radius R, with a specific boundary energy γ b, For the bulge to grow

2𝛾 𝑏
𝑅> …………………….(2.8)
∆𝑃

13
This reaches a critical value when the boundary bulge becomes hemispherical, when
R=Rcrit =L, and

2𝛾 𝑏
𝑅𝑐𝑟𝑖𝑡 > ………………….(2.9)
∆𝑃

On its concave side, the bulging boundary is joined to the lower grain by an array of
dislocations or low angle boundaries, and it is not at all clear whether at the critical stage
(equation 2.9), the boundary can still be considered as separating regions of high stored
energy (P1 and P2) as shown in figure 2.4b, or whether it separates P2 and perfect crystal
(fig. 2.4c), in which case ∆P in equation 2.9 is now given by P2. Bate and
Hutchinson[21] have shown that if SIBM proceeds as shown in figure 2.4b, as the bulge
develops, the dislocation or boundary length attached to the bulging boundary remains
constant, whilst the boundary area is increased, and therefore the retarding pressure due
to the substructure acting on the concave side of the boundary is reduced. They define
the (constant) pressure on the convex side of the bulge as P, and that on the opposite side
as P.f, a fraction f of P. The critical length for bulging is then found to be

2𝛾 𝑏
𝑅𝑐𝑟𝑖𝑡 > 𝑃 ………………(2.10)
1−𝑓

compared to the Bailey and Hirsch value of equation 2.10, which can be written as

2𝛾
𝑏
𝑅𝑐𝑟𝑖𝑡 > 𝑃(1−𝑓) ..……………(2.11)

The implication of this analysis is that the critical bulge size is significantly reduced if
the stored energy is large and ∆P is small (f→1). As f increases, the difference between
Rcrit as given by equations 2.10 and 2.11 decreases.

From the above review of literature, it is realized that despite the importance of recovery
and grain boundary migration during annealing the details of the process are not well
understood [14,18,19,20]. There are multiple reasons: recovery involves multiple micro-
mechanisms and unlike the standard microstructural features, is intrinsically difficult to
quantify. The quantification of recovery typically involves changes in properties and/or
microstructural features. While the former has limited sensitivity, the microstructual
features affected by recovery often demand sophisticated measurements. Furthermore,

14
orientation sensitivity of recovery, though a topic of enormous significance may bias any
recovery measurements and boundary migration involves atomistic processes occurring
rapidly, at high temperatures, and under conditions which are far from equilibrium. It is
therefore very difficult to study boundary migration experimentally or to deal with it
theoretically. These, formulated the motivation behind the present study.

15
 CHAPTER 3
Experimental Methods

3.1 Materials

Commercial aluminum (6061) age hardenable type alloy is used for cover plates and
picture frame due its low neutron absorption co-efficient, high formability, medium
strength, weldability and corrosion resistance. Y2 O3 is used as a surrogate material to
model U3Si2 behavior.

3.2 Fabrication of the fuel plates

The fabrication of fuel plates is carried out by using picture-frame technique, Fig.3.1.
This method is used to produce the preplate (sandwich). The sandwich plate consists of a
core plate made from a mixture of yittrium oxide (Y2O3) and aluminum powder, which
is surrounded by a frame and two cover plates, made from 6061 aluminum alloy (the
cladding). The three-layer assembly is welded and rolled in several passes at about
5000C. During hot rolling passes, roll bonding takes place between all the sandwich
components. Then, the final plate thickness is obtained by a cold rolling pass. The
different reductions given were 35%, 60%, 72% in hot rolling condition while the fourth
sample was finally cold rolled to 85% reduction.

Fig 3.1: Illustration of picture frame technique of preparing plate type fuels.

16
3.3 EBSD measurements

All the samples were sectioned to obtain mid width RD-ND sections of the rolled plates.
All the specimens used for characterization were first polished mechanically using
emery papers of grit size 1000 to 4000, followed by diamond polishing using 1 μm and
0.5 μm diamond paste. The diamond polished samples were electropolished using
methanol and perchloric acid (80:20) at a voltage of 13 V for 17 seconds. The
temperature of the electrolyte was kept around -20ºC during polishing.

The electropolished RD-ND sections were mapped by EBSD (electron backscattered

diffraction). TSLTM EBSD packages on FEITM Quanta-200HV SEM (scanning electron
microscope) were used for the EBSD measurements. Beam and Video conditions were
kept identical between the scans. Inverse pole figure (IPF) maps were used to
qualitatively show microstructural changes at different annealing time and temperature.
Microindents were used to study the same area before and after annealing. Measurement
points above 0.1 CI (confidence index: an index of accuracy in automated indexing)
were used for subsequent analysis. Data points above 0.1 CI represent at least 95%
accuracy. The scans were taken with 0.1μm step size.

3.4 X-ray Diffraction

XRD measurements were taken in a Panalytical X‟Pert PRO MRD system. Peak profiles
of (111) and (100) poles were taken using a step size of 0.01 and a time period of 60s at
each step (Fig.3.2). Monocap attachment with a beam diameter 100µm was used to
obtain diffraction profile from specific areas traversing across the thickness of the
specimen. The analysis of the peak profiles, involved multiple aspects: ranging from
relatively simple peak broadening (full width at half maximum - FWHM) to more
involved dislocation density measurements.

17
 Fig. 3.2: X-ray diffractogram of Al used for Dislocation density calculations

The dislocation density () was determined according to the methodology described by
Groma [22]. According to Wilson and Groma [22], the second and fourth order
restricted moments of the X-ray line profiles has the form:

1 L   ln  q / q0 
M2 q  q 2 2 2  ………………………….. (3.1)
 F
2
4 K F 2 2

M4 q   3 
2 2
1
 2 q  ln 2 (q / q1 ) …………………………. (3.2)
q 2
3 F 4 2
4 q
2 2

4
where q   Sin  Sin0  , F is the average column length or the area weighted

particle size measured in the direction of the diffraction vector g, K is the Scherrer
constant, L is the so called taper parameter,  is the average value of dislocation

density, q0 and q1 are the fitting parameter not interpreted physically, 2 is the

average of the square of the dislocation density,  is a geometrical constant describing

the strength of the dislocation contrast and θ0 is the exact Bragg angle. The dislocation
M 4 q
densities are calculated by fitting eq. (3.2) to the linear part of [22]. This method
q2

18
provides internal checking, since that value of dislocation density is chosen for which
second order and fourth order moment gives almost same particle size. Momentum
method is effectively used in the past to find dislocation density in deformed materials.

Fig. 3.3 shows the schematic of residual stress measurement by standard Sin2ψ (±40º
with 5 steps) method [23] was used for determining residual stress values of different
poles. Interplanar spacing, for a (hkl) pole, can be expressed as:

dhkl ()= d0[1+s1(σ11+σ22)+1/2s2σ sin2] ……………..(3.3)

Where ψ is the inclination angle and φ is the rotation angle of the goniometer. d0 is the
inter planar spacing of the stress free material. S1 and S2 are the X-ray elastic constants
(XECs), σ11and σ22 are the stresses expressed in sample reference and σφ is the residual
stress of the material. The above relation is derived from continuum approach to
elasticity. By using X‟pert stress analysis software and with appropriate material
constant inputs, the residual stress values can be estimated from the slope of dhkl (ψ, φ)
vs. Sin2 ψ (Fig.3.4). The (111) and (002) poles were the two highest intensity poles in the
2theta scan. The residual stresses in different directions have been studied by bi-axial
residual stress analysis. Thus the residual stresses for Phi=00,450,900 have been plotted
(Fig.3.5).

19
 (a) (b)

Fig. 3.3: (a)Schematic arrangement for residual stress measurement, (b) Experimental
set-up for residual stress measurement

Fig. 3.4: Plot of dhkl (ψ, φ) vs. Sin2ψ for residual stress measurement.

20
 Fig. 3.5: XRD plot showing a schematic of bi-axial residual stress measurement.

3.5 Hardness Measurement and Heat Treatment

A Leco-LM 300AT micro-hardness tester was used at 50gm load to measure micro-
hardness through the thickness of the specimen and at least 10 measurements were made
in each sample.

The heat treatment were carried out in muffle furnace at a constant rate of 10 0C and
with cooling rate 0.650C/min. Furnace cooling was done to avoid residual stress
generation due to thermal effect.

3.5 Bond Strength

Bond Strength of roll bonded plates were measured using ASTM D1876-01 standard
[24]. The specimen dimensions were scaled at ¼ (Fig.3.6). The peel tests were
performed on Instron capacity 5kN tensile testing machine with a crosshead speed of 5
mm/min. The bent, unbonded ends of the test specimen were clamped in the test grips of
the tension testing machine and an autographic recording of load versus head movement
was recorded (Fig. 3.7). The peel resistance over at least 31mm length of the bond line

21
after the initial peak was calculated. The bond strength was calculated using the
relationship:
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐿𝑜𝑎𝑑
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑏𝑜𝑛𝑑 𝑠𝑡𝑟𝑒𝑛𝑔𝑡𝑕 = 𝑊𝑖𝑑𝑡 𝑕 𝑜𝑓 𝑆𝑎𝑚𝑝𝑙𝑒 …………..(3.4)

(a) (c)

(b)

Fig.3.6: (a) Geometry of test specimen (b) Schematic of bond test, (c) Experimental set-
up of bond strength. Inset shows the debonded sample.

Fig.3.7: Typical plot of peel test

22
 CHAPTER 4
Results and Discussion

4.1 Direct Observation of Recovery Phenomena

Recovery and grain boundary migration during annealing has often been considered as
an important, yet neglected, part of annealing related phenomena in metallic materials
[14,18,19,20]. To an admirer of recrystallization, the importance is apparent. They sets
the basis for subsequent recrystallization. The importance of recovery is universally
acknowledged but involved experimental studies on recovery are at best „limited‟. There
are multiple reasons: clear demarcation between plastic deformation and recovery,
difficulties in exact quantification of associated microstructural changes, involvement of
multiple mechanisms, orientation dependent recovery, atomistic processes occurring
rapidly at high temperatures in boundary migration in non-equilibrium conditions. It is
therefore very difficult to study recovery and boundary migration experimentally or to
deal with it theoretically.

4.1.1 EBSD measurements

Fig. 4.1(a) shows the effect of annealing time at 2000C of the same area before and after
recovery. The image before annealing shows fibrous or lamellar microstructure. First
generation or non-crystallographic micro-bands which define [26] the nature of strain
localizations is also clearly visible. The IQ Map (Fig. 4.1 (b)) shows that with increase
in holding time the sub-boundaries are developing. The broken sub-boundaries can be
seen to re-organize to have a clear and sharp sub-boundary. Further increase in holding
time leads to migration of boundaries resulting in growth of subgrains. Fig.4.2 shows
the increase in subgrain size with recovery. A plot of low angle boundary density with
annealing time (Fig. 4.3) shows an increase in boundary density which further confirms
the development of subgrain boundaries. After 30 min. annealing the decrease in
boundary density can be due to growth of subgrains.

23
 0 min. 15 min.

30 min. 60 min.

Fig..4.1: (a): EBSD images, in inverse pole figure notation, of the deformed and
recovered (200C) plate fuel. Points of low (<0.1) CI are marked in black.

24
Fig. 4.1 (b) : IQ map showing sub boundaries (red color) in the area shown by the inset
in Fig.4.1 (a)

Fig. 4.2: (a) Subgrain diameter as a function of annealing time, (b), (c) IQ map showing
sub-boundaries (red color)

25
 5.2

Average Boundary Line length/

5.1
5
4.9

Area ()
4.8
4.7
4.6
4.5
4.4
4.3
0 10 20 30 40 50 60 70

Annealing Time (min.)

Fig.4.3: Low angle (2-150) boundary density as a function of annealing time for sample
recovered at 2000C

From Fig.4.4 it is observed that with increase in annealing time the band thickness
increases. This is not a classical SIBM where a new recrystallized grain bulges out of the
existing grain boundary within a deformed structure [19], but appears to be more of a
uniform boundary movement. The latter is expected [21] to be ineffective in reducing
internal defect density and that is apparent from the high resolution EBSD scans. As
shown in figure 8a, for deformed 111 bands there was a visible (and significant)
coarsening beyond 15 min. recovery treatment. This is an interesting observation, which
appears confusing in the first glance, is the „direction‟ of coarsening of uniform SIBM.
Such a phenomena is expected as an orientation with lower stored energy migrate into
neighboring orientation with higher stored energy. The present study, however, revealed
that higher stored energy 111 bands were growing into neighbouring non-111
orientations during extended recovery.

Role of recovery in misorientation developments is controversial. Though it is generally

believed that misorientation decreases with recovery [19], information on the contrary
also exists [13]. The latter has been attributed to the presence of orientation gradients
[13]. Results from the present study, indicate a clear statistical trend of overall

26
misorientation increase – see figure 4.5. A plot of misorientation gradient between a
reference subgrain and the 1st, 2nd...nth neighbor will indicate confirm the presence of
orientation gradient and hence increase in misorientation with recovery.

Fig.4.4: (a) Average deformed band thickness, as a function of annealing time for
samples recovered at 2000C. Error bars represent standard deviations of the measured
data – as obtained from multiple manual measurements. (b,c) EBSD images: describing
significant changes in band thicknesses.

6.6
Average Misorientation (0)

6.4
6.2
6
5.8
5.6
5.4
5.2
5
0 1 2 3 4

ln (Annealing Time)

Fig.4.5: Average misorientation as a function of annealing time

27
4.1.2 Hardness

The hardness through the thickness of the specimen was measured and profile was
plotted to study the effect of annealing time and heterogeneity in mechanical property in
the normal direction across the interface at annealing temperature of 200 0C. Fig.4.6
shows that effect of annealing time on hardness of the plate fuel. It is observed that
hardness is higher for near interface region than near surface.

Fig.4.6: Variation of micro-hardness with prior-deformation and recovery time. Error

bars represents standard deviations of the measured data as obtained from multiple
measurements.

According to S.H Lee et.al [27] rolling a layered composite (consisting of hard and soft
layers) creates strain incompatibility at the layer interfaces during deformation. This is
because the rolling mill induces the same magnitude of load to both the layers separated
by a bonded interface, across which the material in the softer layer flows to a larger
strain than the harder layer. Thus, the soft layer pulls the harder layer, resulting in an in-
plane shear force at the interface (schematically shown in Fig.4.7) [28]. In the light of
the above argument, hardness is expected to be high at the interface than at surface due

28
to large redundant shear strain induced by high friction between roll surface and
specimen during rolling.

Fig 4.7: Schematic diagram showing the operation of an in-plane shear stress at the
boundary between the Al and Al(Surrogate) [Al(S)] layers thereby creating a tensile
drag force on Al(S)[28].

4.1.3 FWHM and Dislocation Density

Full width half maxima (FWHM) and dislocation density gives indication about the stain
present in the material. Dislocations are the primary carriers of the plastic flow in
metallic materials [29]. Their collective behavior under the application of external
stresses dictates the materials mechanical properties and determines several of the
material phenomenon such as strain hardening, strain rate sensitivity etc. Typically
dislocation structure of any given material evolves during its fabrication (which can
involve a combination of deformation and heat treatments) and can continue to evolve
during the service too [29]. The knowledge of dislocation structure evolution can help
predict the rate of recovery.

Fig.4.8 and 4.9 shows the effect of annealing time and temperature on recovery kinetics.
It can best represented by a logarithmic relationship:

y = m (lnt) +c ..........................................(4.1)

where y represents quantities: FWHM of the respective X-Ray peaks and dislocation
density, m is the slope, t is the annealing time and c is a constant.

The difference in overall kinetics is evident in Table 4.1. The near interface region
shows faster kinetics than near edge region in all four cases. This is in agreement with
higher hardness at the near meat region. Due to wire brushing of the surface of cover
29
plates before rolling leads to work hardening thus leading to accumulation of more
dislocations in the near meat region. This results in more stored energy for recovery and
hence higher recovery kinetics.

It is also observed that 111 plane shows faster kinetics than 100 plane. This is because
111 has higher stored energy than 100 plane which undergoes comparatively lesser
plastic deformation than 111 plane.

0.6 0.7
0.5 0.6
0.5
0.4

FWHM (0)
FWHM(0)

0.4
0.3
0.3 NI
0.2
NI 0.2
0.1 NE
NE 0.1
0 0
0 2 4 6 0 2 4 6
ln (Annealing Time) ln (Annealing Time)

111 100
(a) 2000C
0.7 0.6
0.6 0.5
0.5
0.4
FWHM(0)

FWHM(0)

0.4
0.3
0.3
0.2 NI
0.2 NI
0.1 0.1 NE
NE
0 0
0 2 4 0 1 2 3 4
ln (Annealing Time) ln (Annealing Time)

111 100
(b)3000C
Fig. 4.8: Dislocation density, from the respective peaks ((111) and (200)), as a function
of annealing time for samples annealed at (a)2000C (b)3000C. Error bars represents the
measurement/analysis uncertainties.

30
 18 14

Dislocation Density (m-2) (1015)

Dislocation Density (m-2) (1015)
NI NI
16 12
14 NE
10 NE
12
8
10
8 6

6 4
4 2
2 0
0 0 2 4 6
0 2 4 6
ln (Annealing Time)
ln (Annealing Time)

111 100
0
(a) 200 C

18 14
Dislocation Density (m-2) (1015
Dislocation Density (m-2) (1015)

16 NI NI
12
14 NE
NE 10
12
10 8
8 6
6
4
4
2 2
0 0
0 2 4 0 1 2 3 4
ln(Annealing Time) ln (Annealing Time)

111 100

(b)3000C
Fig. 4.9: Dislocation density, from the respective peaks ((111) and (200)), as a function
of annealing time for samples annealed at (a)2000C (b)3000C. Error bars represents the
measurement/analysis uncertainties.

31
Table 4.1: Slope of Dislocation density versus ln (annealing time) indicating rate of
recovery.
2000C 3000C

111 100 111 100

Near Interface 3.43 2.57 3.12 2.18

Near Edge 1.43 1.12 2.07 1.56

4.1.4 Residual Stress

Residual stresses remain within a part after it has been deformed and all external forces
have been removed and are detrimental for service life of a product [23] . These elastic
stresses can be removed by giving a heat treatment to the material. Fig.4.10 and 4.11
shows the effect of recovery on shear residual stress in rolling direction and normal
residual stress in transverse direction at 2000C and 3000C respectively. It is observed
that residual stresses decreases with increase in annealing time and temperature
indicating the decrease in strain present in material.

600 500
500 NE 400
Normal Residual Stress (MPa)
Normal Residual Stress (MPa)

400 NI 300
300 200
200 100
100 0
0 -100 0 2 4 6
-100 0 2 4 6 -200
-200 -300
-300 -400
-400 -500
ln (Annealing Time) ln(Annealing time)

111 100

(a) 2000C

32
 600 500
400

Normal Residual Stress (MPa)

400

Residual Stress (MPa)

300
200 200
100
0
0
-200 0 1 2 3 4
-100 0 2 4
-400 -200
-300
-600 -400
ln(Annealing Time) ln (Annealing Time)

111 100

(b)3000C
Fig. 4.10: Normal residual stress from the respective peaks ((111) and (200)), as a
function of annealing time for samples annealed at (a)2000C (b)3000C.

50 350
Shear Residual Stress(MPa)

Shear Residual Stress(MPa)

300
0 250
0 2 4 200
-50 150
100
50
-100 0
-50 0 1 2 3 4
-150 -100
ln(Annealing Time) -150
ln(Annealing Time)

111 100

(a) 2000C

33
 100 250
80 200

Shear Residual Stress

Shear Residual Stress

60
150
40
100
20
50
0
-20 0 1 2 3 4 0

-40 -50 0 1 2 3 4

-60 -100
ln(Annealing Time) ln(Annealing tIme)

111 100

(b)3000C
Fig. 4.11: Shear Residual Stress from the respective peaks ((111) and (200)), as a
function of annealing time for samples annealed at (a)2000C (b)3000C.

4.2 Bond Strength

Three phenomena may influence the bond strength during the annealing treatment. First,
annealing reduces hardness at the interface and therefore, increases the bond toughness.
In the peel test, a crack propagates through the bonded area and separates two bounded
sheets. Improvement of the bond toughness raises the required force for the crack
propagation and so, increases the bond strength. Second, annealing is used to remove or
reduce residual stresses between the solid-state bonded dissimilar materials. Third, since
Y2O3 is inert under the condition thus no intermetallic phase forms at the interface of
cladding and meat, enhancement of the bond strength after annealing may be related to
the diffusion phenomenon at the interface.

4.2.1 Annealing time

4.12 shows the effects of annealing time on average peel strength at constant annealing
temperatures (T = 200 and 5000C). Increasing the annealing time increases average peel
strength, and thereby also bond strength, because the increased annealing time
diminishes the work-hardening effect. In other words, the sample annealed for 60 min
34
has the highest formability and bond strength because the work-hardening effect of this
sample has been completely eliminated by a great increase in annealing time. Moreover
reduction in residual stress at interface also leads to improvement in bond strength. But,
it is observed that at higher temperature (5000C) with longer time (60 min.) results in
reduction of bond strength. This is discussed in subsequent section.
Average Bond Strength (N/mm)
2.5

1.5

200
1
500

0.5

0
0 20 40 60 80
Annealing Time (min.)

Fig. 4.12: Variation of bond strength with annealing time

4.2.2 Annealing temperature

Fig. 4.13 demonstrates the variations in average peel strength, versus annealing
temperature at a constant annealing time (t = 30 min). It is shown that increasing the
annealing temperature at first increases the average peel strength and, thereby, the bond
strength but further increase of temperature is detrimental to the bond strength. The
initial increase in bond strength is due to the greater diminishing of the work-hardening
effect as the annealing temperature is increased. Furthermore, the energy of the atoms at
the interface is an important factor for metallurgical bond formation. Based on the
theory of energy barrier, a metallic bond occurs between two metals when the energy of
the atoms at the interface exceeds a certain limit, i.e., the activation energy for bond
formation [11]. It is necessary to overcome the activation energy of bond formation to

35
initiate the bonding process in the roll bonding process. This energy may be provided by
the annealing treatment. When annealing time or temperature is increased, more atoms
obtain the activation energy necessary for bond formation. Thus, increasing the
annealing time or temperature improves the bond strength.

3.5
Average Bond Strength (N/mm) Holding Time: 30 min.
3

2.5

1.5

0.5

0
200 250 300 350 400 450 500
Temperature (oC)

Fig. 4.13: Variation of bond strength with annealing temperature.

But further increase in annealing temperature may lead to dissolution of second phase
particles leading to excessive grain growth which result in shift of diffusion phenomena
from grain boundary diffusion to volume diffusion. It is known [25] that grain boundary
diffusion makes a significant contribution to the total flux when

Dbδ > Dld ……………………..(4.2)

The effective width of a gain boundary is ~0.5 nm. Grain sizes on the other hand can
vary from ~ 1 to 1000 µm and the effectiveness of the grain boundaries will vary
accordingly. The relative magnitudes of Dbδ and Dld are most sensitive to temperature.
Measurement of grain size variation with annealing time and temperature can help to
answer the above decrease in bond strength.

36
 SUMMARY

 The current project work involved the study of roll bonding of plate fuels with
sandwich geometry. The roll bonding characteristics of Al clad plates with U 3Si2
as dispersoid in aluminum matrix as the fuel was studied with ceramic surrogate
material Y2O3.
 Direct observation on static recovery at 2000C of roll bonded plate fuel with 85%
prior reduction in thickness, studied by a combination of X-ray line profile
analysis and high resolution electron diffraction, were best represented by
logarithmic relationship.
 Increase in misorientation was observed with recovery which could be due to
strain localization.
 Roll bonded plate showed clear signatures of coarsening of bands. This was
considered as a case of uniform boundary movement or SIBM (strain induced
boundary migration) which was incapable of reducing internal defect density.
However, its exact mechanism remains to be charted.
 Dislocation density and hardness measurement showed higher recovery at near
interface region than near surface because of higher stored energy in near meat
region.
 Dislocation density measurement showed higher rate of recovery of 111 grains
than 100 grains.
 Reduction in hardness, residual stresses and diffusion at interface lead to
improvement in bond strength with increase in annealing time and temperature.

37
 FUTURE WORK

 Direct observation of recovery at higher temperatures (250 0C, 3000C, 3500C) to

characterize the exact mechanism of uniform boundary migration in SIBM.

 Bond strength measurement for longer annealing time (2 hr, 4hr and 8hr),
temperature and simultaneous measurement of grain size to quantify the
temperature at which volume diffusion overcomes the grain boundary diffusio n
so as to find optimum post heat treatment cycle.

38
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