Abstract:
Zircaloy-2 is used for fabricating core components in nuclear power reactors. The alloy in
the form of tubes i) 60 mm diameter with a wall thickness of 1 to 2 mm is used as Calandria
tubes in Pressurised Heavy Water Reactor (PWR). ii) Less than 30 mm diameter is used as a fuel
cladding in Boiling Water Reactor (BWR). These components are exposed to temperature of
400oC to the inner surface and outer surface temperature of 280 to 350oC.
Almost 90% of the zirconium produced is used in nuclear plants and it cannot be recycled
due to high cost factor. It is very essential to improve the mechanical and corrosion resistance
properties of the Zr alloys, for enhancing service life of the structural components, through new
thermo mechanical processing routes without altering its chemical composition. Ultrafine and
nanostructured bulk materials produced by SPD techniques exhibit enhanced mechanical and
functional properties as compared to bulk alloys as reported in the literature. The reduced grain
size enhances the yield strength as per Hall-Petch relation. Strengthening is also possible by other
structural features such as dislocations, subgrain boundaries, nanotwins and solute atoms. The
sum of all these structural features are responsible for strengthening mechanisms. .
The performance of structural components in nuclear power reactors depends on tensile,
creep and corrosion resistance properties. These properties are heavily influenced by
microstructure of the material fabricated through different thermo mechanical treatments. SPD
processing along with apt post heat treatment could produce multimodal microstructures in the
materials, which can provide simultaneous improvement in strength and ductility. Cryorolling is
one of the novel deformation processing techniques used widely to produce ultrafine and
nanostructures in the pure metals and alloys. In this technique, dynamic recovery is suppressed to
accumulate high density of dislocation in the materials during processing at liquid nitrogen
temperature. The literature on the influence of cryorolling and cross rolling on the mechanical
behaviour of zircaloy-2 is limited. Therefore, the present work has been focused on producing
ultrafine and nanocrystalline zircaloy-2, with improved mechanical properties, from its coarse
grained alloy using the various thermomechanical processing such as cryorolling, room
temperature rolling, room temperature cross rolling and cryo cross rolling.
The objectives of the present work was to investigate (i) Mechanical behaviour and
microstructural characteristics of ultrafine grained zircaloy-2 processed by cryorolling; (ii)
ii
Mechanical and microstructural evolution of ultrafine grained zircaloy-2 produced by room
temperature rolling; (iii) Texture and mechanical behavior of zircaloy-2 rolled at different
temperature; (iv) Development of ultrafine grained zircaloy-2 by room temperature cross rolling
and cryo cross rolling; (v) Microstructure and mechanical behavior of room temperature rolled
zircaloy-2 after water and mercury quenching; (vi) Experimental evaluation of mechanical
properties and fracture-fatigue simulation of cryo and room temperature rolled zircaloy-2; (vii)
Experimental and simulation study on the fracture toughness of zircaloy-2 processed by rolling
and cross rolling at different temperatures A chapter wise summary of the thesis is given below.
Chapter 1 highlights a brief introduction to the material used in the present investigation,
deformation mechanism of the material used, various SPD processes used to produce UFG
materials, applications of UFG materials in various fields and pros and cons associated with the
SPD techniques.
The literature relevant to the present research work on ultrafine grained zircaloy-2 is
critically reviewed in Chapter 2. A brief description of the properties and application of
zirconium alloys as well as the effect of alloying elements on mechanical and corrosion
behaviour are made. Deformation mechanism and mechanical properties of UFG Zr and its alloy
is reviewed. It forms a strong basis to formulate the key objectives pertaining to the development
of ultrafine grained zircaloy-2 with improved strength and ductility as compared to their
commercially available bulk counterpart.
All the related experimental techniques and procedures employed in the present work are
outlined in the Chapter 3. The methodology for characterizations and mechanical behaviour of
UFG materials are discussed. The simulation is performed by using FEM and XFEM software
package Abaqus.
In Chapter 4, Section 4.1 describes the following experimental investigations performed
on zircaloy-2. The mechanical properties and microstructural characteristics of ultrafine grained
zircaloy-2 processed by cryorolling (CR) were investigated. The solutionised zircaloy-2 was
rolled at liquid nitrogen temperature (77K) with different thickness reductions (25% to 85%).
The dislocation density ‹ρ› in the cryorolled zircaloy-2 increases with increasing true strain due
to the suppression of dynamic recovery. The CR 85% alloy showed hardness and yield strength
values of 282 HV and 891 MPa, respectively. The annealed CR 85% alloy showed higher
ductility (9.5% and 11.2%) in rolling and transverse direction, respectively, as compared to CR
85% alloy.
iii
In section 4.2, the effect of deformation strain at room temperature on the
microstructural and mechanical properties of zircaloy-2 is discussed. The deformed alloy reveals
the misorientation of incidental grain boundaries (IDBs) due to large plastic strain induced in the
sample. The hardness of the alloy after 85% room temperature rolling (RTR) is found to be 269
HV, while the tensile strength is 679MPa and 697 MPa, in the rolling and transverse direction,
respectively. The deformed alloy subjected to annealing at 400o C for 30 minutes sample shows
increase in ductility (6% and 7.2% in rolling and transverse direction respectively) due to the
annihilation of dislocations as evident from the TEM study.
In section 4.3, the microstructural characteristics, texture, and mechanical properties of
the zircaloy-2 processed by CR and RTR are described. Texture results show the activation of
basal slip at higher strains in room temperature rolled zircaloy-2. In cryorolled zircaloy-2, only
activation of prism slip is observed. Grain refinement, sub-structures, and texture in the deformed
alloy contribute for the improvement in mechanical properties.
Effect of change in strain path by cross rolling at 300 K up to a true strain of 1.89 and at
77K upto 0.69 true strain has been studied and reported in section 4.4. The texture and
mechanical properties of cross rolled zircaloy-2 at 77K and 300 K temperature are discussed. The
fragmentation of near basal grains due to change in strain path is evident from the EBSD
micrographs. 1012 extension twins are observed initially up to 25% reduction, with the further
reduction in thickness, near basal grains are oriented towards the normal direction. These basal
grains are fragmentated due to changes in strain path upon room temperature cross-rolling as
observed from KAM and EBSD images. TEM results of the room temperature cross rolled
sample confirm the formation of ultrafine and nanograins in the alloy due to orientation of
incidental dislocation boundaries (IDB) in the direction of macroscopic plastic flow and postannealing
treatment of the deformed alloy. A tensile strength of 991 MPa with 7.5% ductility is
observed in the 85% room temperature cross rolled alloy. Annealing at 673K for 30 minutes
recrystallizes the deformed microstructure and forms ultrafine grains. Evolution of deformed
microstructure occurs by the activation of prismatic slip, 1122 contraction and 1012
extension twin at 77K. Probability of basal slip <a> at 77K is also observed by Taylor and
Schmid factor analysis. The deformation at 300K occurs by prismatic, basal <a> and Pyramidal
<c+a> slip predicted by texture images. Stored energy and dislocation density in the deformed
alloy is calculated with the help of KAM.
iv
In section 4.5, the effect of water and mercury quenching on the microstructural and
mechanical behavior of room temperature rolled zircaloy-2 is discussed. Solution treatment of
zircaloy-2 at 1073K, followed by quenching in mercury and water has been made prior to rolling.
Different reduction from 25% to 85% of the quenched alloy was given for characterizing their
microstructures and mechanical properties. Rolling reduction accumulates high dislocation
density inside the materials, thereby enhancing the mechanical strength. Initial deformation has
occurred by the activation of extension twinning as can be seen from EBSD microstructure. By
optimizing the annealing temperature (400o C for 30 minutes), ultrafine grains are produced in
85% room temperature rolled zircaloy-2. The mechanical properties of ultrafine grained zircaloy-
2 is found to be better than the coarse grained zircaloy-2.
Chapter 5 describes the results of compact tension test, FEM and XFEM simulation
performed for zircaloy-2. Section 5.1 describes Finite element method used to study the 2-D
quasi static crack analysis. J-integral and internal energy of the processed alloys are evaluated
and compared with each other. Fatigue simulations are performed by using ANSYS software to
find the S-N curve of mercury quenched, CR and RTR zircaloy-2.
In section 5.2, the fracture toughness of zircaloy-2 processed under rolling conditions is
discussed. The rolled sample shows better crack arresting capabilities due to larger back stress
produced during loading. Xtended finite element simulation is performed by using Abaqus
software package to evaluate the fracture toughness of the alloy. CT results obtained after
XFEM simulation show a good match for undeformed samples (MQ), while for severely
deformed samples, the values obtained are less because dislocations are not modeled in the
simulation.
The conclusions of the present investigation and scope of the future work are reported in