Yongzhou Wang

Fundamentals of Recrystallization in Titanium
Alloys
A dissertation submitted to the University of Manchester for the degree of Master of

Science by Research
in the Faculty of Engineering and Physical Sciences
2014
Yongzhou Wang
School of Materials
Fundamentals of Recrystallization in Titanium Alloys
CONTENTS
CONTENTS ...................................................................................................................1
DECLARATION ...........................................................................................................3
COPYRIGHT STATEMENT ........................................................................................3
ACKNOWLEDGEMENT .............................................................................................4
ABSTRACT ...................................................................................................................5
1. GENERAL INTRODUCTION ..................................................................................6
1.1. General Introduction............................................................................................6
1.2. Aims of this Investigation ...................................................................................7
2. LITTERATURE REVIEW ........................................................................................8
2.1. Basic Properties ...................................................................................................8
2.1.1. Crystal Structure ...........................................................................................8
2.1.2. Classification and Alloying Elements...........................................................9
2.2. Deformation in HCP materials ..........................................................................12
2.2.2. Slip Modes ..................................................................................................12
2.2.2. Deformation Twinning ...............................................................................15
2.2.3. Deformation Texture...................................................................................16
2.3. Recrystallization ................................................................................................19
2.3.1. Nucleation ...................................................................................................20
2.3.2. Factors Affecting the Rate of Recrystallization ..........................................26
2.3.3. Grain Growth after Recrystallization ..........................................................30
2.3.4. Recrystallization Texture ............................................................................31
3. EXPERIMENT ........................................................................................................35
3.1. Materials ............................................................................................................35
3.2. Rolling Process ..................................................................................................35
3.3. Pickling and Heat Treatment .............................................................................37
3.4. Sample Preparation............................................................................................37
3.5. Characterization Methods..................................................................................38
3.5.1. Vickers Hardness Testing ...........................................................................38
3.5.2. Optical Microscopy.....................................................................................39
3.5.3. Electron Backscattered Diffraction (EBSD) ...............................................40
4. RESULTS ................................................................................................................43
4.1. Hardness ............................................................................................................43
1

4.2. Optical Microscopy ...........................................................................................44
4.3. EBSD Mapping .................................................................................................51
4.4. Texture Evolution ..............................................................................................56
5. DISCUSSION ..........................................................................................................59
5.1. Deformation Microstructure ..............................................................................59
5.2. Static Recrystallization ......................................................................................64
6. CONCLUSIONS AND FUTUREWORK ...............................................................67
6.1. Conclusions .......................................................................................................67
6.2. Future Work.......................................................................................................67
REFERENCE ...............................................................................................................68
The final word count13827
DECLARATION
No portion of the work referred to in this thesis has been submitted in support of an
application for another degree or qualification of this or any other university or other
institute of learning.
COPYRIGHT STATEMENT
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dissertation) owns any copyright in it (the Copyright) and s/he has given The
University of Manchester the right to use such Copyright for any administrative,
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accordance with the regulations of the John Rylands University Library of
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(Reproductions), which may be described in this dissertation, may not be owned by
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School of Materials.
ACKNOWLEDGEMENT
I would like first extend my most sincere gratitude to my supervisor, Dr. Joao
Fonseca. His encouragement and the instructions were second to none.
I am also deeply grateful to Mr. Ken Gyves, Mr. Michael Faulkner and Mr. Feng Li
for their support during the experimental work.
ABSTRACT
Commercial pure (CP) titanium plates were rolled at various of temperatures at
25,150,300and 450with a reduction of 30%. After pickling and annealing
for 1 hour at different temperatures above and below that of recrystallization,
specimens were characterized using Vickers hardness testing, optical microscopy and
electron back-scattered diffraction (EBSD).
Optical microscopy characterization provided evidence of the microstructure
evolution in all the samples. Most of the grains were elongated or broke up after
rolling. Interestingly, material rolled at higher temperature gave much more
heterogeneous microstructure which led to faster recrystallization in subsequent
annealing.
EBSD technique showed the detailed grain orientation information and texture of the
samples. Warm
rolling produced greater orientation gradients and more
heterogeneous deformation microstructure than cold rolling and the texture was
strengthened by higher rolling temperature. Thus, the start of recrystallization is faster
after warm rolling due to higher nucleation rate; recrystallization was promoted in
spite of the decrease of stored energy consumed by dynamic recovery.
1. GENERAL INTRODUCTION
1.1. General Introduction
Titanium and its alloys have gained more and more attention recently because of their
excellent properties such as unique low density, good high temperature properties and
excellent resistance to corrosion [1]. However, a wider variety of applications are
hindered due to its relatively high price, for which reason sometimes titanium has to
be replaced by other materials such as magnesium, aluminium and steel. Though
more understanding of the disadvantages for titanium and its alloys is required,
continuous improvement of titanium smelting and processing technology could lead
to an increase in the application of titanium alloys in the near future.
A great number of applications for titanium are located in aircraft area like structure
materials in SR71 reconnaissance airplane as depicted in Fig.1.1 [2] and in aeroengines like Fig.1.2 [1]. Although among the usage of 10% weight of titanium in
Boeing 777 airplanessome classical titanium alloy fan blades have been gradually
replaced by polymer composite material, still we can see from Fig.1.2 that great
noticeable proportion of parts are composed of titanium. It worth to point out that
titanium has gained much closer connection to our daily life such as acting as golf
clubs or seat posts of a bicycle[3].
Fig. 1.1. SR71 aircraft[2].
Fig. 1.2.Titanium in GE-90 aero-engine[1].

1.2. Aims of this Investigation
The research of fundamentals on recrystallization of titanium alloys aims to
understand the microstructure evolution and macrostructure behavior of titanium
during recrystallization which unlike cubic materials, has rarely been investigated.
Details of deformation structure and nucleation and grain growth during
recrystallization will be studied.
2. LITTERATURE REVIEW
2.1. Basic Properties
The basic properties of titanium consist the crystal structure, classification, phase
transformation and the anisotropy of alpha Ti.
2.1.1. Crystal Structure
Pure titanium has a relatively high melting point of 1668. Below 882 titanium
has a hexagonal close-packed (HCP) structure ( phase) and it changes to a bodycentered structure ( phase) above its phase transformation temperature of 882.
Fig.2.1. Unit cell ofa phase andb phase [1].

The HCP structure unit cell of phase with the lattice parameters a=0.295nm,
c=0.468nm thus the c/a ratio is 1.587 as shown in Fig.2.1. The three most densely
packed planes are (0002) plane, one of the {
} planes and {
1} planes, in
other words, the basal plane, prismatic planes and pyramidal plane. The BCC unit cell
of phase is presented in Fig. 2.5 illustrating one of the six most densely packed {110}
8

lattice planes. The lattice parameter value of a = 0.328nm at room temperature while
at a level of 0.332nm at 900 is demonstrated as well.
2.1.2. Classification and Alloying Elements

The titanium family has three categories: , + and alloys, depending on the
position of isomorphous phase diagrams. The binary phase diagram in Fig.2.2 [4] is
divided into three parts which belong to , and + alloys with different shape
varying with the stabilizers elements. The definition of and stabilizers depends on
how alloying elements change the transformation temperature. For instance,
stabilizing increases the transus temperature. The stabilizing phase diagram is
shown opposite in Fig.2.2. By adding high content of strong stabilizers like V, Nb
and Ta, the elevated temperature phase can sometimes appear at even room
temperature [5]. Fig.2.3 [6] schematically demonstrates the phase diagram of
stabilizers concentration and temperature in detail. Ms line is the martensitic start line
which will be described later.
There are two special titanium alloys that merit special mention: CP titanium and Ti6Al-4V titanium alloy. CP titanium has the most typical hexagonal structure and the
lowest content of other element. Though CP titanium is more expensive than some
other metallic materials like stainless steel, products made from it can have lower life
cycle cost due to its excellent durability [7]. Besides, it has good corrosion resistant
ability and fabricability as well as ideal properties for research. Another important
titanium alloys, Ti-6Al-4V, belongs to the + group. It contains about 15% phase
at 800 and is the most widely used in the titanium industry. Ti-6Al-4V offers a
good balance of superior strength, lightweight, ductility, fatigue and corrosion
resistance which makes it a popular advance material in various areas like medical
devices, sports equipment and aerospace application [8].
Fig.2.2. Schematic representation of different alloying elements on titanium phase

diagrams[4].
Fig.2.3. Binary phase diagram of the a classification of titanium alloys [6].

Some important titanium alloys listed in Table 2.1 [2] can demonstrate the alloy
composition and their strength. The main interstitial elements are N, C, H, Fe, O and
main substitutional elements are Al, Zr, Sn, and Mo.
Clearly, the six kinds of important commercial pure titanium have the lowest strength
and the relatively lower level of impurities. It can be seen that with the content of
10

oxygen increase from 0.18% (grade 1 and grade 11) to 0.40% (grade 4), giving
significant increases in strength. The yield stress of grade 1 titanium to grade 4
titanium increases from 170MPa to 480 MPa. As a matter of fact, -titanium can be
significantly hardened by interstitial element of oxygen. Furthermore, it has been
noted by Williams, SommerTung that increase of oxygen content can also change
the titanium slip mode from wavy slip to planar slip [9].
As can be seen from Table 2.1, there is another important element which occurs in
and + titanium should be pointed out, that is aluminium. Al is a substitutional
element has the highest solubilities in both and phase. Different substitutional
elements with large atomic size like Al in a titanium matrix can create a lattice strain
area, hindering dislocations moving thus increase the strength of titanium. Besides,
aluminium in titanium can also form Ti3Al precipitates which can act as coherent
particle obstacles to lower the mobility of dislocations.
Table 2.1 Some titanium alloys [2].
In phase, since it is hard to separate the solution hardening effects of precipitates,

the effect of alloy element partitioning precipitates accompanying with alpha
11

titanium [1] becomes a very important solid strengthening effect, as supported by the
data of Pearson [10].
2.2. Deformation in HCP materials

Deformation in titanium is more complex than cubic materials. Conventional slip and
twinning modes in , + and alloys are different, let alone the additional slip
system in hexagonal phase.
2.2.2. Slip Modes

Both of the HCP and FCC structures are closely packed while deformation in
titanium is harder than cubic materials mainly due to its unique structure and
symmetry behavior.
The main slip planes in hexagonal titanium is the (0002) basal plane, the (
pyramidal plane and the (
direction is <
) prismatic plane as marked in Fig.1.1a. The main slip
> direction which is the most close-packed direction. According to
Von Mises criterion, it requires 5 independent slip systems for homogeneous

deformation for a polycrystalline material. But there are not enough independent slip
systems from basal <a> slip, prismatic <a> slip and pyramidal <a> slip which can be
seen in Table 2.2 from Yoo [11]. Considering the six {
planes and (0002) plane with the <
1} planes, three {
> slip directions there are 12 slip systems in
total. As a matter of fact, the actual independent slip systems can be reduced to 4
nominally due to the same shape change of type1 and type 2 comparing with type 3.
Hence another kind of slip, with non-basal Burgers vector will get activated.
12

Table 2.2. Slip systems in the hexagonal phase [11].
By only comparing the four kinds of slip types and considering the number of
independent slip systems in Table 2.2, we can draw a conclusion that the fourth type
is the easiest way to activate deformation. Not only because it has enough
independent slip systems, but also for the reason that the plane is the nearest to 45
with the highest Schmidt factor among the 4 types.
Fig.2.4. <c+a>/<a>Prism and <a>Basal/<a>Prism slip ratio as a function of

temperatures for single crystal Ti6.6Al [14].
However, all this is based on the assuming that the critical resolved shear stresses
(CRSS) are the same. Actually, there are large differences as is shown in Fig.2.4 [12].
The CRSS of <c+a> prism slip is the highest and has a dramatic difference of about 34 times than others when increase the temperature. The basal slip is slightly higher
13

than prismatic slip at all temperatures. Taking the significant difference of CRSS at
higher temperature into consideration, the presence of <c+a> type is less than what
has been considered. In fact, prismatic slip dominants the plastic deformation in
titanium and it might be responsible for the main rolling texture in the later stage of
deformation in titanium [13] .
In an ideal close-packed hexagonal material, the (0001) basal plane is the most
closely packed plane where slip always takes place with an ideal c/a ratio is 1.633.
Usually, basal slip exists with high c/a ratio. The c/a ratio in hexagonal titanium is
less than 1.633 which means distance between the two basal planes is reduced
comparing with the ideal hexagonal crystal. Therefore the relative atomic packing in
prismatic and pyramidal planes gets increased and slip by these two types is promoted
[15]. Moreover, slip modes in real titanium crystals has a strong dependence on
interstitial impurity concentration, especially dependent on oxygen and nitrogen on
the basis of Churchman [16]. Table 2.3 shows the relationship between slip systems
and concentration of oxygen and nitrogen. By increasing the concentration of oxygen
and nitrogen tenfold, basal <a> slip, prismatic<a> slip and pyramidal<a>slip all get
promoted especially obvious for pyramidal slip which does not even occur at the
lower impurities level of 0.01% at room temperature. Churchman also explains the
reason why less pure metal does not have the phenomenon that the CRSS for
prismatic slip is lower than that for basal slip which occurring in purer metal. This is
because the interstitial oxygen atoms influence the movement of dislocations along
{
} planes [16].
Table 2.3 Slip in titanium crystals [16].
14

2.2.2. Deformation Twinning
Generally, slip in hexagonal packed structure material is restricted for its low
symmetry and deficiency of independent slip systems. Therefore, twinning is
necessary to sustain deformation compatibility hence twinning and slip often occur
together [17][18][19]. It is noted by Kocks & Westlake [20], twinning is needed to
accommodate the external plastic strain state which makes deformation in
hexagonal materials different from cubic structure materials.
Basically, twinning is a kind of deformation mode which is different from slip. The
relative motion of one part of the crystal against another creates shear, resulting in the
twinning structure of two crystals sharing some identical crystal lattice points in a
symmetrical manner. It plays an important role in the plastic deformation of materials
at low temperatures and low strain. Since twinning shear achieved by twinning is
relatively small, in order to compensate for the deformation strain together with slip,
large amount of twinning is required in hexagonal structure materials.
Twinning is directional which is different from slip. There are two different kinds of
twinning which are tensile twinning and compression twinning depends on whether
the <c>axis is in tension or in compression as shown in Fig.2.5 from Partridge.
According to Olaf & Valeria [21], {
}< 011> is the most important twinning
system in HCP materials, but other twinning systems may be activated with a varying
c/a ratio.
Blicharski et al [22] found that twinning occurs in all grains at very early stage in cold
rolled titanium. The main twinning types observed in alpha titanium are {
{
1}tension twinning, and {
},
2} compression twinning[1]. In a hexagonal metal,
the critical c/a ratio is 1.732, above or below which twinning will form by tension or
compression with tension according to Reed & Abbaschian. In general, tension
twinning is more common in titanium since the c/a ratio of titanium is 1.587 and
{
}< 011> twins are the most common type though they have the smallest
magnitude of twinning shear hence they are the easiest to activate.
15
Fig.2.5. (a) Tensile twinning in HCP metal. (b) Compression twinning in HCP metal.
(from Professor Michael Preuss lecture).
It is worth mentioning that twinning on {
3} and {
4} which are high order
pyramidal planes only appears in single crystal titanium flakes with the direction
along c- axis observed by Liu & Steinberg [23]. Liu & Steinberg also pointed out that
oxygen and other impurities also have an effect on twinning mechanism of hexagonal
material. Again, like what happens in slip systems in titanium, {
than {
{
2} type is less
} twins first found by Rosi, Dube & Alexander [15], mainly because
} twins replace the former {
2} twins since the basal plane is sharply
inclined to c-axis.
2.2.3. Deformation Texture

After processing with deformation, crystallographic texture can be produced in
materials. These non-random crystallographic textures, also called preferred
orientation, come from the fact that deformation takes place on the most preferred
orientation during twinning and slip process [24]. Textures will cause anisotropy
instead of a random oriented structure. Anisotropic properties can be harmful,
however sometimes we need certain special ability from textures as well. Therefore it
is important to understand the origin and evolution theory for textures as well as the
influence factors.
Generally, uniaxial deformation like wire drawing and extrusion results in relatively
simple textures comparing with rolling where more than one deformation axis exists
16

[21]. Fig.2.6 from Hatherly Hutchinson [25] shows three different hexagonal
material pole figures of rolled magnesium, zinc and titanium.
Fig.2.6. Rolling textures of (0002) pole figures of cold rolled HCP metals:(a) c/a ideal:
magnesium; (b) c/a high: zinc; (c) c/a low: titanium [25].
Fig.2.7. ODF sections at constant Phi 1 (1) for the T40 titanium plate cold-rolled to
80% [29].
The texture difference of the three hexagonal metals comes from their c/a ratio and
particular slip systems according to Grewen [26]. For magnesium whose c/a ratio
close to 1.633 (ideal c/a value), the cold rolling texture is dominated by a strong
{0001}basal plane fiber texture (Fig.2.6a).This is because the effect of basal slip
systems which compels grain orientation rotates to {0001} promptly and consume
other twinning or slip possibilities easily. It is proved in behavior of magnesium sheet
by Agnew et al. [27] and Yang et.al. [28]. Textures in zinc whose c/a ratio higher than
1.633, the basal plane is tilted 20-30 degrees towards the rolling direction resulting in
the pole figure of Fig.2.6b. In the case of metals with lower c/a ratio like titanium and
17

zirconium, the basal plane is tilted 30-40with the rotation axis of <
> parallel
to rolling direction, as shown in Fig.2.6c.

Fig.2.7 from Wagner et al. demonstrates that the main peak occurs around 1=0, =
45, 2=0which is around (
3)<
> . The secondary peak is centered at a
position around 1=0, = 32, 2=30which represents (
3)<
0> [30]. The
result is quite close to what Inoue & Inakazu observed that after medium cold rolling
process, the orientation of titanium sheet has a tendency to arrange along a fiber along
at 1=2=0and when subjected to higher reduction level, the orientation tends to
aggregate around =35-40. The reason for this is pointed by Tom et al., owing to
the combination of {
2} compression twinning and {
2} tension twinning.
Furthermore, the contributions of pyramidal <c+a> slip and basal slip is low with
prismatic slip {
0}<
0> dominating.
A more detailed deformation texture evolution of titanium with different rolling

reduction level can be seen in Fig.2.8. from Bozzolo [13]. The starting material is CP
titanium with fully recrystallized homogeneous microstructure which undergo a
moderate grain growth with ODF maximum around 1=0, = 35, 2=15-20noted
by Bozzolo et al.[31]. The strong texture with texture index of 6.5 weakens to 2.8-3.5
during cold rolling, {
0} maximum shift along the rolling direction and becomes
the dominant components whereas (0001) maxima spread out to 1=0, = 40, 2=0
after 80% rolling, at the same time, 1=0, = 90, 2=0 comes into being and
remains. When comes to 25% cold rolling, 1=0, = 0, 2=30 generated with
[0001] axis close to normal direction and vanish away from the texture index of 3.1 at
larger strain. The weaken of texture index and the texture randomness probably
comes from the twinning activity [32], as well as for the appearance of 1=0, =
90, 2=0and 1=0, = 0, 2=30texture components.
Generally, when CP titanium is subjected to reduction up to 40%, deformation is
accommodated by twinning and slips while when the reduction increase to 60%-90%,
slip overcomes twinning and become dominant in deformation. Meanwhile, twinning
makes the texture random while slip strengthens it [33].
18

EBSD analysis from Bozzolo [13] declares the phenomenon which tensile twins
appearing in compression twins was found in many of the grains thus many different
orientations were created during this process.
Starting material 25% cold rolled 50%cold rolled 80%cold rolled
Texture index:
6.5
3.1
2.8
3.5
Fig.2.8. Texture evolution during deformation with different strain. Texture index
values and ODF section at 1 = 0for as-received CP- Ti and after reduction of 25%,
50% and 80% [13].
2.3. Recrystallization
As a result of subgrain coalescence after recovery, a crystallite is formed, whose size
is larger than the critical size can grow to form high angle boundaries while others
annihilate. High angle boundaries can move easily in the deformed region reducing
19

the dislocation density. This is the primary recrystallization which in other words, is a
process that new equiaxed grains form from the deformed matrix where high angle
boundaries migrate driven by the stored energy [34]. Recrystallization homogenizes
the microstructure of materials. Before and after recrystallization, recovery and grain
growth also play an important role in microstructural changes and restoration of
physical properties[35].
2.3.1. Nucleation
Nucleation is the first step of recrystallization which not only related to some previous
situation such as the deformed state, annealing condition and recovery but also has a
contribution to the following grain growth. Hence to gain a deep understanding of
nucleation is crucial; however, it is difficult to measure nucleation experimentally
since the nucleation rate is not a constant.
There is a very important kinetic model of nucleation in the scientific study of phase
transformations which is the thermal fluctuation model. This classical nucleation
model was firstly created in physical chemistry by Volmer et al. and Becker and then
was noticed that it fitted well with solidification and solid state phase transformation
as well by Turnbull [36]. Calculations based on this classical theory by Christian [37]
supported it as well. If the free energy driving pressure is Gv per unit volume, the
per unit area interfacial energy of between the new and old structures and, for a
defect interface with an angle when a heterogeneous nucleation takes place, there is
an energy barrier, G*, to form a critically sized small clusters of crystalline
(embryos) which are just stable and capable of growing [34]. The energy barrier is
described as:
*
+ (
(1)
Where is a constant which depends on the shape of the small clusters of crystalline,
and the function f ( cos) varies from 0.1 to 0.5, depending on the defect geometry.
The new grains formation rate, Iv, defined as:
20

(2)
Where the density of critical new grain clusters, nv*, is described as:
(
(3)
Where Nv is the total number of clusters and it is clear seen that the formation of
critical clusters is a thermal activated process.
The kinetic parameter is the rate at which atoms can add to critical clusters to turn
them into growing nuclei which related to the rate of diffusion:
(
(4)
Where is a frequency factor, and Q is the activation energy for diffusion.

While nowadays it has been realized that nucleation of new grains in a deformed
structure probably might not be achieved by localized classical fluctuation mechanism,
because the driven energy for recrystallization is very small and the interfacial energy
for high-angle boundaries is large [24]. People start to consider new grains generated
from some pre-existing structures of a deformed material. In this way, nucleation is
strongly linked with the structure of the deformed state.
Two main models describe grain nucleation in the deformed substructure: Strain
induced grain boundary migration (SIBM) suggested by Beck and Sperry [38] and
coalescence of subgrains, as first proposed by Li [39].
The SIBM mechanism, as can be seen clearly in Fig.2.9a, has been observed in a wide
range of metals [40] [41]. SIBM usually takes place at the grain boundaries. It mainly
involves migration of a boundary adjacent to two subgrains or by bulging of one part
of a pre-existing single large grain boundary.
As we can see in the EBSD map of magnesium, among the gains there are several
special arcs indicated by arrows. They look like one grain grows into another adjacent
grain. The big bowing grain in Fig.2.9.b with light and dark colors changing indicates
21

the stored energy is different on either side of the grain boundary, hence there must be
a driving force which can compensate for the total system energy.
Fig.2.9. EBSD map showing SIBM in (a)Alloy M03 after annealing for 2 h showing
examples of grain boundary bulging (indicated by arrows) [40] (b) in aluminum [41].
The driving force for SIBM is usually considered to be the difference of dislocation
density on separate sides of the grain boundary which lead to a stored energy gradient.
When the metal is deformed, the stored energy produced by dislocations is given as:
ED= Edis= c2Gb2
(5)
Where is the density of a deformed material, c2 is a constant of 0.5 and G is the

shear modulus.
It should be pointed out that total dislocation density increases rapidly when the true
stain goes up to 0.5 and then continue to increase linearly with strain according to
Zehetbauer & Seumer [42].
Bailey and Hirsch firstly analysed the kinetics of the nucleation process as shown in
the schematic diagram of Fig.2.10. Large amount of dislocations generated by
deformation causes unstable states and the driving force associated with stored energy
forces one subgrain whose dislocation density is less than others to bulge out into its
neighbor with higher dislocation density. When a high angle grain boundary sweeps
over subgrains, dislocations were eliminated and thus a strain-free nuclei is created
[43].
22
Fig.2.10 Schematic diagrams of recrystallization by high angle boundary migration

through a partially-recovered microstructure [43]
Mathematic detailed modal is shown in figure 2.11a. Considering two grains in a
deformed structure with the stored energy difference of E 1 and E2 of grain 1 and grain
2 respectively (E2>E1) which lead to the energy difference of E = E2 - E1 then the
energy difference drives the boundary between them with a spherical shape of radius
R bulging out into grain 2. With the interface energy of
b per unit volume, the total
bulging area interfacial energy is defined as:

EB=4R2 b
(6)
With change of the volume energy E of a bulging region with a sphere volume of
4/3R3 , the energy difference is represent with
E= 4/3R3 E
(7)
If the bulge want to grow then the whole system Gibbs free energy should decrease,
which means:
G=EB-E=4R2b - 4/3R3 E0
23
(8)
Fig.2.11. (a) Grains with low stored energy (E1) and higher energy (E2), (b) bulging of
the migrating boundary, (c) the migrating boundary is free from the dislocation
structure, (d) SIBM originating at a single large subgrain [24].
then we have R >
,which means as long as the boundary bulge to
hemispherical where R = Rcrit = Lthe critical radius is given by:

Rcrit >
2b /
24
(9)
Fig.2.12 Schematic diagrams of schematic diagrams of subgrain rotation and

coalescence [43].
Another way for nucleation comes from subgrain coalescence. Fig.2.12 shows a
schematic diagram of subgrain coalescence by rotation. The rotating subgrain
between low angle boundaries has a small misorientation between the adjacent
subgrain and it attempts to rotate to coincidence in order to lower the surface energy
between them. Slip and climb by low angle boundary dislocations were involved in
order to obtain coincidence and larger misorientation [43].
Fig.2.13 The misorientation increases with the number of edge dislocations.

Specifically, the coalescence of subgrains by movements of the dislocations, which
leave one subgrain boundary entering the adjacent one, leads to larger subgrains,
which create a larger misorientation. As Fig.2.13 shows the orientation differences
can become more bigger when subgrains are coarse. The edge dislocation wall
becomes thicker which means the misorientation is proportional to the density of the
25

dislocation which can be defined as =b/h where h is the spacing of the dislocations.
When the misorientation is large enough (0.15 - 0.35 rad), the mobility of the
boundary increases strongly as the two equations indicate.
ED 3s /D
(10)
s =0(A-ln)
(11)
Where D is the diameter of a spherical grain and A=1+lnb/D.
2.3.2. Factors Affecting the Rate of Recrystallization

(1) Strain
Generally, as the strain level increased, the material recrystallizes faster (e.g.
Fig.2.14), more energy stored in defects such as dislocations and vacancies hence
more nuclei per unit volume can be formed during annealing. Furthermore, the large
number of nuclei will lead to a finer recrystallized grain size.
Fig.2.14. Recrystallization kinetics of aluminium as a function of strain annealed at

350C [45].
26

There is a minimum critical strain, below which recrystallization cannot initiate. In
pure metals such as aluminum and iron this minimum strain is 1-5% elongation, but it
is dependent on the actual annealing temperature, and for a given temperature tends to
be raised by alloying according to Honeycombe [44].
(2) The original grain size
Recrystallization proceeds more readily in fine-grained metals as shown in Fig.2.15.
[46] In general, the smaller the initial grain size is, the larger grain boundaries area
per unit volume exists. Since grain boundaries are the preferential nucleation sites,
recrystallization can be promoted in those finer grains. As for the opinion that there
more stored energy in finer grains, it is mainly suit for low strains as discussed by
Hatherly [47] since both deformation bands and shear bands which are preferential
nucleation sites in coarse grains, appear frequently with larger grain size.
Fig.2.15 The recrystallization kinetics at 225C of copper of different initial grain sizes
cold rolled 93% fraction recrystallized [46].
(3) Purity
27

Usually, the purer a metal, the lower the temperature at which recrystallization will
occur noted by Dimitrov et al. [48].Table 2.4 shows the effects of zone refining on the
recrystallization temperature of different metals after rolling.
Clearly, it can be seen that in ultrahigh purity aluminum the recrystallization
temperature decrease to a quite low value of -50. This phenomenon, also called the
solute drag, occurs in impure metals especially in metals with low very limited
solubility. Impurities can segregate near grain boundaries at which nuclei prefer to
form, and act as obstacles to debase the mobility of boundaries which slow down the
grain growth speed and hence influence the recrystallization.
Table 2.4 The effect of purity on the temperature of recrystallization [48].
But the condition for recrystallization of two-phase alloys is quite complex. Larger
particles may either act as a pre-existed nucleation sites for recrystallization or cause a
significant pinning effect by impeding the mobility of dislocations. However, small
particles with lower volume fraction generate less deformation around them when
grains undergo a shape change. Besides, a small particle requires less energy for a
dislocation to pass by.
(4) The Annealing Temperature and Annealing Rates
It is clearly seen from Fig.2.16 that the higher the annealing temperature isthe faster
the recrystallization rate will be. Since both nucleation and grain growth are thermally
activated processes, as can be seen the equations below:
28
Q
N C1 exp N
KT
(12)
Q
G C2 exp G
KT
(13)
In other words, recrystallization is a diffusion controlled process. For this reason, a

higher annealing temperature enhances recrystallization.
Fig.2.16. Recrystallization kinetics of of Fe-3.5%Si deformed to 60% as a function of

annealing time [49].
When the heating rate has been increased, generally, the recrystallization temperature
will be lower due to lack of time for the recovery process which consumes the stored
energy and hence promotes the recrystallization. Besides, phase transformation should
be considered as well as noted by Wert et al. [50]. If the annealing rate is too slow, a
supersaturated solid solution will become precipitates and hinder the following
recrystallization. However, when the material is conducted a rapid heating rate,
recrystallization may be completed before those precipitates occur.
29
Fig.2.17. Recrystallization kinetics at 600C of CP-Ti rolled to a 60% reduction at

various temperatures between 25C and 600C.
However, the recrystallization kinetics of HCP material might be different. Fig.2.17
demonstrates the recrystallization kinetic of CP-Ti rolled at different temperatures.
Clearly, we can find that warm rolling promotes recrystallization. The microstructural
inhomogeneity effect overcomes the effect of decrease of stored energy during warm
rolling [51].
2.3.3. Grain Growth after Recrystallization

As stated by Humphreys & Hatherly [24], when the primary recrystallization is
completed, the structure is still not stable, and further heating or heat preservation
may lead to grain growth. The driving force is to lower the stored energy in materials
in the form of grain boundaries.
There are two types of grain growth: normal grain growth and abnormal grain growth
also named secondary recrystallization. Normal grain growth is a continuous process
and the microstructure coarsens uniformly in comparison with abnormal grain growth.
The grain size distribution strongly depends on time. During abnormal grain growth,
certain grains in the matrix grow faster and consume the smaller grains which
resulting in a bimodal grain size distribution.
30

Normally, boundary migration plays an essential role in grain growth, and the pinning
effects of solutes and second-phase particles may be more sensitive to boundary
migration. Consider a two-dimensional microstructure. When boundaries are mobile,
a localized spontaneous equilibrium of grains will be set up. As shown in Fig.2.18
[52], The boundaries boundary energies are
12 , 12 , and 23 for grain 1, 2 and 3
respectively , to reach an equilibrium state the condition is required:
12
= 13 = 23
sin 3 sin 2 sin 1
Which means when
(14)
1 =2 =3 =120 the stable grain morphology in a two-
dimensional microstructure is equilateral hexagons . In order to make sure the

interfacial tension stays stable and to form the 120structure, the small grains will
shrink and the big grains will bulge out, which means big grains consume small grains
to grow. Fig.2.18b is what the real grains look like.
Fig.2.18 (a) The forces state at the boundary triple point. (b) BCC packing of
truncated octahedral [52].
2.3.4. Recrystallization Texture

There are two classic theories to explain recrystallization texture: orientated
nucleation theory and orientated growth theory. Burgers and Louwerse [53] first
31

found there is a preferred nucleation sequence between lightly deformed aluminum
fragments and the bulk part with heavy deformation. Supporters of orientated
nucleation theory believe that since the grains both in deformed matrix and during the
recrystallization process have a preferred orientation, when these grains grow up, they
should as well show an orientation preference which forms the recrystallization
texture.
Another theory, the orientated growth theory, focuses on another different part of
recrystallization. Evidences found by Barrett shows that recrystallized grains have a
relationship with the deformed matrix by a 45<111> rotation which fit well to the
oriented growth. Supporters of orientated growth theory hold their opinions that
subgrains with specific orientations have been formed during recovery, hence for
grain boundary of these preexist nuclei have higher mobility than those have not.
Thus recrystallization texture appears after the prior nuclei grow up with similar
orientation. Although there is some difference between the two theories, recent
evidence has proved that both orientated nucleation theory and orientated growth
theory should be considered together.
Recrystallization texture in hexagonal packed materials has been rarely studied
comparing to BCC and FCC materials. Among the factors influence the
recrystallization texture, the effect of deformation texture and recrystallization
behaviour of HCP materials should be highly considered. Generally, as noted by
Philippe [54], some recrystallization texture in hexagonal materials can be treated as a
redistribution of intensity from rolling textures.
Inoue & Inakazu [55], Singh & Schwarzer [32] have found that there is a preferential
orientation of {
3}[
0] with 1=0, = 32, 2=30in highly deformed titanium
and zirconium. Fig.2.19 [56]demonstrate the texture evolution of Zr702 partially

recrystallized state and the fully recrystallized state comparing with the deformed
state. The ODF peak around 1=0, = 30, 2=0, i.e. close to (
5)[
0], of the
deformed state is almost retained during as well as after primary recrystallization.

Interestingly, the maximum intensity decreases. It is also the same with the situation
of Ti40 titanium cold rolled to 80%, followed by annealing showed by Fig.2.20 and
the deformed state represented by Fig.2.8 since the difference is fairly limited.
32

In particular, both the orientation density with high value phi values and low phi
values decrease while more orientations turned up around positions with 1=0, =
45, 2=0(near (
3)<
0>) and 1=0, = 32, 2=30( near (
3)<
0>)
[30]. Recovery contained dislocations rearrangement and subgrain coarsening may be

responsible for such phenomenon. Besides, hexagonal metals have higher stacking
fault energy than cubic metals according to Wagner et al. [29]. It is well established
that stacking fault energy will promote the recovery process which means materials
with higher stacking fault energy have higher extent of recovery hence continuous
recovery occurs [24].
Fig.2.19. ODF sections and pole figures for Zr702 [57].
33
Fig.2.20. ODF sections (1=0) for the T40 titanium plates cold-rolled to 80% with
subsequent annealing at 500 C: (a) 40 min; (b) 80 min; (c) 160 min; (d) 210 min; and
(e) 360 min [29].
Recently, Bozzolo and Wagner have conducted a series of experiments to study the
texture evolution in hexagonal materials. According to Bozzolo et al. [58], the major
recrystallization texture change did not result from the primary recrystallization stage
but mainly comes from grain growth. Furthermore, in 80% cold rolled titanium alloys,
there were 80% of the grains subjected to recrystallization in the first stage of
annealing and the remaining 20% grains recrystallized later without any orientation
change. Dewobroto et al. [59] studied the texture development in Zirconium and
proved that the global texture change is slight from deformation texture mainly due to
the selected growth of sub-grain or recovered cell growth. The nuclei with 1=0, =
30, 2=30 texture component undergo less orientation pinning and become
dominant after grain growth. It is worth mentioning that twinning plays an important
role on influencing the major texture component of titanium in the first stage of
recrystallization [60].
34
3. EXPERIMENT
3.1. Materials
A block of the as-received commercial pure grade 2 titanium with the size of
150mm*100mm*30mm used in the current project was manufactured by Smiths
Metal Centres Ltd.. It is forged and annealed with the proof stress 0.2% of 317MPa
and the tensile strength of 437MPa. The chemical composition is demonstrated in
Table 3.1.
Table 3.1 Elemental compositions in wt. % of CP-Ti.
3.2. Rolling Process

The as-received titanium block cut and machined to 4 pieces of titanium plate with
the size of about 154*30*10mm from the workshop of Materials Science Centre,
University of Manchester. The rolling process was carried out in the Mechanical
Working Laboratory via a mill produced by Marshall Richards Barcro. Before and
between each pass, the three titanium plates were put in a furnace whose type is
LHT6/60 produced by Carbolite Ltd. at temperatures of 150, 300 and 450 for
3 minutes respectively. When the temperature and microstructure of the whole plate
was homogeneous, the three specimens were rolled by the rolls immediately. The last
one was rolled at room temperature. All the samples were rolled to a reduction of 30%
by three or four passes. When the final pass was completed, the thickness dropped
35

from 10mm to about 7mm. Table 3.2 establishes the rolling schedule. Fig.3.1
illustrates the stress state of the specimen. The stress along the rolling direction was
tensile stress while along the normal direction was compression.
One might consider that there might be recrystallization took place when the rolling
temperature increased to 450C. As a matter of fact, according to Chun & Hwang,
there is no recrystallization occurred during warm rolling at 450 for CP-Ti plate
with even 60% reduction [51].
Table 3.2 Rolling schedule of the four CP titanium plates
Compression
Tension
Tension
Compression
Fig.3.1 Stress state of the rolling CP-Ti plate.
36
3.3. Pickling and Heat Treatment

After the rolling process, the four CP-titanium plates were cut to small cubes in a size
of 10mm along RD, 7mm along ND and 6mm along TD which means the
characterization direction is TD (RD-ND plane). This is because in the RD-ND plane
both the extension and compression of grains becomes quite clear.
Pickling was carried out prior to any treatment or sample preparation in order to
remove the deformation layer which may influence subsequent recrystallization
behavior. The pickling acid is a mix of 28ml HNO 3, 3.5HF and 70ml H2O (400g/L
HNO3, 40g/L HF) [61].
After pickling at 50 in the acid for 2 hours, the
deformation layer as well as the oxide layer of the sample was wiped off and the
surface of the sample looked shining.
The subsequent annealing was carried out with argon atmosphere in a LTF-1200
tube furnace produced by Lenton. Oxygen and nitrogen contamination were prevented
during heat treatment at temperatures of 400, 450, 500, 550, 600, 650,
700 and 750 for 1 hour respectively. Samples in a ceramic sample holder were
put right in the centre of the furnace to achieve the best temperature condition and
were pulled out rapidly after one hour and following by air cooling.
3.4. Sample Preparation

The heat treated samples were mounted in the resin using a combination of 7 minutes
heating and 3 minutes water cooling. Subsequent grinding was performed using
water-lubricated silicon carbide papers of 800ppm with rotating disc at speed of 200
rpm for about 30 seconds. After carefully cleaning the sample to remove any silicon
carbide particles, mechanical polishing was used to achieve a better surface. During
the polishing process each with 5minutes from coarse abrasive diamond polishing
disc with 15m particles on the cloth to finer one with 6m and 1m, applying
sufficient polishing lubricant liquid when needed. Finally, colloidal silica polishing
(i.e OPS) with a combination of colloidal silica emulsion and hydrogen peroxide was
conducted for two hours with slightly etching in KROLLS solution in between and
37

after. The OPS process repeated three times and last one thinned with water to get to
pH7. The POL filter in the optical microscope brings out the twins nicely when the
top layer is removed.
3.5. Characterization Methods

Procedures to characterize the properties of samples are summarized in Fig.3.2. The
techniques involved will be described in the following sections.
Characterization
n
Hardness
EBSD
Optical Microscopy
Test
Orientation
Pole
Rx
Map
Figure
Analysis
Fig.3.2. Characterization Methods (Rx means recrystallization).
3.5.1. Vickers Hardness Testing

In order to collect the recovery and recrystallization information of the samples after
annealing, hardness was measured by a pyramid hardness testing machine produced
by Vickers Armstrongs (Engeineers) Ltd. The load used in the current test is 5kg.
38
Fig.3.3 Vickers hardness test (schematically) [62].

Comparing to other hardness tests, the Vickers hardness test is accurate and easier
since the hardness calculations are based on the size of the indenter, and the Vickers
indenter can be used for almost all materials without regard to hardness. The essential
principle, like other measurements of hardness, is to measure the resistivity to plastic
deformation by the diamond indenter with a standard load. The unit of hardness is
known as the Vickers Pyramid Number (HV). Fig.3.3 shows the schematic diagram of
Vickers hardness testing. According to the size of rhombus left by the indenter, the
Vickers hardness can be calculated by [63]:
(15)
Where d is the average length of (d1+d2)/2 in millimeters and F is the kilogram force.
3.5.2. Optical Microscopy

Microstructure evolution of the samples after rolling and annealing was characterized
by optical microscopy of AxioCam MRc 5 produced by Zeiss. The differential
interference contrast (DIC) microscopy technique was applied.
Differential interference contrast microscopy can transform the phase shift of light
which induced by the specimen refractive index, into detectable amplitude differences
[64]. The images from differential interference contrast microscopy will appear bright
39

against a dark background whereas unlike phase contrast, there is no diffraction halo.
A plane polarized light serves as the light source. After the light get through the prism
refraction, two beams of orthogonally polarized mutually coherent parts are divided.
After they travel through the samples in adjacent area and create an optical path
difference, they will be recombined by another prism. Tiny difference on the
thickness of the sample will be converted into the difference between light and shade.
Contrast of the sample surface morphology is increased, hence an appearance of a
three-dimensional physical relief is produced and the images are comparable to that of
the embossment on the marble. The setup of differential interference contrast
microscope is showed in Fig. 3.4.
Fig.3.4 DIC optical microscopy (schematically) [64].
3.5.3. Electron Backscattered Diffraction (EBSD)

The electron backscattered diffraction technique is applied to study the orientation
map, bulk textures and recrystallized fraction of the samples using a FEI Sirion field
emission gun scanning electron microscope (FEG-SEM) with EBSD acquisition
software of Aztec. The working distance is about 16mm and the accelerating voltage
is 20Kv. The step size for detailed orientation map scan is 0.5m and 10m to obtain
40

the texture. The critical misorientation angle, , is defined by 10. HKL Channel 5
software is used to measure the orientation data, grain boundary information and the
recrystallization behavior.
The EBSD technique, also called orientation imaging mapping (OIM) technique,
based on the scanning electron microscope (SEM), provides a way to examine the
crystallographic orientation as well as the grain boundary misorientation and local
crystalline perfection of materials [21]. When the electron beam hit the sample which
tilted 70from the horizontal, some of the incident electrons (backscattered electrons)
will be reflected by the sample and will create a diffraction pattern on the phosphor
screen. This specific pattern stores the information of orientation of the grains and
will be collected by a sensitive CCD camera. The schematic diagram of a typical
EBSD installation in an SEM is provided in Fig3.5 [24].
Fig.3.5 Electron backscattered diffraction technique. (schematically) [24].

Usually, an inverse pole figure orientation (IPF) map is used to represent the
crystallographic orientation by different colors.
Another important information in addition to the local grain orientation can be
obtained from EBSD, is the textures representing by pole figures. A pole figure is a
stereographic projection displaying the distribution of certain orientation of grains as
well as the pole densities. As can be seen in Fig.3.6, the (0001) pole normal to (0001)
plane in the northern half sphere is projected to the reference equatorial plane by
joining the pole to the south pole. In addition, the angle can characterize the
azimuth of the pole and the angel representing the rotation of the pole around the
41

polar axis. Poles distribution as well as the angels of and should be read in
conjunction with the reference direction. Contour lines with values of 1 to N times R
(the value related to a sample of completely random orientation) can represent the
intensity distribution. The pole figure technique is perfectly appropriate to study the
highly deformed materials whose cells or subgrains number is too large for the
acquisition of individual TEM patterns [24].
Projection
Fig.3.6Orientation of the basal plane (0002) in a hexagonal crystal [65].

The recrystallization fraction can be calculated from EBSD data by Channel 5
software. At first, the internal average misorientation angle between grains should be
measured by Channel 5. If this angle is higher than the minimum angle to define a
subgrain c, which is 1here, then the grain is deformed. When a grain is consisted of
subgrains whose internal misorientation is lower than c while the misorientation
between each subgrain exceeds c, then the grain is substructured. The remaining
grains are considered as recrystallized grains.
The representing colors of deformed, substructured and recrystallized grains are red,
yellow and blue respectively.
42
4. RESULTS
4.1. Hardness
The Vickers hardness of the as-received CP titanium is 177.8. After rolling at various
of temperatures, work hardening took place and made the material harder. Hardness
increased to 208.8 for samples rolled at room temperature as shown in Fig4.1. The
same increase happened in the material rolled at 150 and 300 even though the
work hardening effect was not as obvious as samples rolled at lower temperature, it
did contribute to the rise of hardness. As for the last one, however, it was softer than
the as-received. It seems that the work hardening effect has been weakened by
another softening method at elevated temperature. All in all, the hardness of CP-Ti
increased after rolling to a reduction of 30% (true strain of 0.357), except the one
rolled at 450.
220
Rolled at 25
Vickers-Hardness
210
Rolled at 150
200
Rolled at 300
As-received
Rolled at 450
190
180
170
160
150
0
100
200
300
400
500
Temperature()
Fig.4.1 Vickers hardness for CP-Ti rolled at different temperatures.

The hardness of samples annealed at 400, 450, 500, 550, 600, 650, 700
and 750 for one hour has been demonstrated in Fig.4.2. It can be seen that heat
treating at 400 for one hour did not give much hardness difference of all the
samples rolled at different temperatures. As a matter of fact, they looked the same just
after rolling. However, hardness started to decrease for samples annealing at 450
with a slight amount of drop which meant recovery took place. Besides, the hardness
43

difference between each rolling temperature decreased as well. The same thing
happened when annealing temperature increased to 550 and after which the
hardness were all lower than the value of as-received CP-Ti. It is worth mentioning
that even though they were all becoming softer, it seems cold rolling samples were
undergone the fastest decrease of hardness which makes the hardness difference
increasingly smaller with annealing.
Interestingly, the hardness of all the samples rolled at room temperature, 150,
300, 450 shows a big drop after heat treatment at 600 for an hour comparing
550 . When heating temperature went to 650 , hardness difference was the
smallest. However, the difference increased a little when annealing at 700 and
750C although the rate of hardness decrease became very gentle at the later stage.
210
Rolled at 25
As-received
200
Rolled at 150
Vickers-Hardness
190
180
Rolled at 300
170
Rolled at 450
160
150
140
130
120
400
450
500
550 600 650

Temperature()
700
750
800
Fig.4.2. The Vickers hardness of samples annealed at 400-750 for 1 hour.
4.2. Optical Microscopy

The following differential interference contrast microscopy images in Fig.4.3 revealed
a noticeable microstructure transformation of deformation and microstructure
evolution of annealing behavior.
44
Fig.4.3. Optical images of samples rolled at of the CP-Ti samples rolled at (a) 25C,
(b) 150C, (c) 300C, (d) 450C.
There were many small but thin twins generated from cold rolling as showed in
Fig.4.3a, while less in specimens rolled at higher temperature and almost disappeared
at 300 and 450. Some hard grains which had resistance to polishing were still
existed and were highlighted in DIC images. They might have some special
orientations which were stable and did not vanish after rolling at room temperature
and 150 . These grains were usually elongated. Generally, the deformation
microstructure was more homogeneous for rolling at room temperature with twins and
deformed grains were evenly distributed. At higher rolling temperatures like 300
and 450, deformation became heterogeneous. Parts of the grains were undergone
much more deformation and formed linear structure and this kind of microstructure
even got distorted badly somewhere while some other grains did not seem to be
stretched much and formed wide zones with similar contrast. This variability in
behaviour was more pronounced in the sample rolled at 450 comparing to 300.
45

Some grains were not elongated at all as showed in Fig.4.3d. Grains with more
deformation of the latter two appeared to be more grain break-up and their
microstructure was discontinuous.
It did not seem much difference in the microstructure of the sample annealed at 400,
nor did in 450, 500 and 550 in the optic microscopy as shown in Fig.4.4.
46
47
Fig.4.4. Optical images of samples rolled at different temperatures and subjected to

annealing at 400-550.
When samples were subjected to heat treatment at 600 for an hour after rolling,
noticeable recrystallization occurred, which matches the Vickers hardness curve. In
the DIC picture of cold rolled sample showed in Fig.4.5, recrystallization was evenly
distributed. However, some grains were not recrystallized at all. Most of them were
large deformed grains as well as some of the undeformed ones. In addition, most of
the twins were consumed by new grains whereas some still retained. The
recrystallized grains in the material rolled at 150 were less than cold rolled one
while in map of material rolled at 300 there were large amount of new grains
generated. There are dense nuclei containing zones around large undeformed grains.
The same can be seen in the 450 rolled sample, only more severe: the regions
where big grains stayed un-recrystallized and the recrystallized zones were quite
distinct from each other.
48

When annealing temperature rose up to 650, recrystallization was nearly completed.
The grain size of cold rolled material was smaller than others. Still, a small number of
grains in material rolled at 450 have not recrystallized yet.
Recrystallization was completed when annealing temperature increase to 700 for
one hour. Grain size of samples rolled at room temperature was the smallest still. It
seemed that grain growth has taken place since some grains were larger than others,
especially in samples rolled at 450.
49
Fig.4.5 Optical images of samples rolled at different temperatures and subjected to

annealing at 600-700.
50

Fig.4.6 demonstrated the grain growth process after materials subjected to heat
treatment at 750. The microstructure was nearly the same, which agrees with the
truth that hardness difference was tiny at this moment. As a matter of fact, grains of
the sample rolled at the highest temperature were slightly bigger than others.
Fig.4.6. Optical images of samples rolled at different temperatures and subjected to

annealing at 750.
4.3. EBSD Mapping

Inverse pole figure map and the pole figure of the as-received CP titanium are shown
in Fig.4.7. In the as-received forged and annealed CP-Ti, as shown in Fig.4.7a, the
forged material had some stored energy already and the microstructure was composed
of slightly misoriented grains as well as some clusters of smaller grains. The average
grain size is about 50m. Among these grains, <0002>//ND orientation (i.e. red grains)
formed the majority of orientations. Comparing with the large scale area IPF map of
51

Fig.4.1b, for a chosen scan area of 500m*370m, grains with <0002>//ND
orientation in majority is a random event though there were also many the red grains.
Moreover, it can be clearly seen in Fig.4.7b that grains with similar orientation
formed clusters resulting in a relatively strong texture as shown in Fig.4.7c. As
discussed before, a typical texture for HCP metals with c/a ratio lower than 1.633 is
the basal poles tilted about 30away from ND towards TD [30]. The pole figure of
as-received CP-Ti exhibited a typical texture which is good for conducting the
subsequent experiment.
Fig.4.7 EBSD (inverse-pole-figure) maps for the ND direction of the as-received CPTi scanning with a step size of: (a) 0.5 m (b) 10 m; (c) Pole figure of as-received
CP-Ti
From the EBSD map in Fig.4.8 we can see that more visually that some grains were
stretched towards the rolling direction and compressed along the normal direction.
Both the undeformed and elongated grains were near <
0>// ND orientation (i.e.
Orientation of green grains). Most of the twins seemed to occur in red grains,
52

however, a small number of green twins and blue twins (i.e. with <
0>//ND
orientation) can be recognized as well. Most of the twins were aligned towards 45to
the rolling direction and they made the grains more discontinuous. There were a mass
of grain boundaries and dislocation tangles. Deformation microstructure became a
little different in the material rolled at 150C. The fraction of grains without
remarkable deformation increased and their orientation varied. These stable grains
were hard to deform by either slip or twinning. In spite of some twins have started to
nucleate inside them, it was difficult for twins to expand. The number of twins might
decrease, but it the red (tensile) twins looked wider and coalesce, forming twinned
zones. Interestingly, there were some green grains and blue grains inside red twins. It
was hard to know whether they transformed from red grains or are remnants from the
original orientation. When came to the microstructure of the sample rolled at 300C,
the deformation method was totally different. Twins were hardly seen and
deformation was dominated by slip. The orientation imaging map was dominated by
red grains and they gathered together to form huge undeformed zones with similar
orientation near <0002>//ND. Other green and blue grains were barely visible.
Moreover, grains with severe distortion and squeezing around those regions without
noticeable deformation broke into small pieces, resulting in a heterogeneous
microstructure. Grain break-up existed in sample rolled at 450C as well. Lots of new
grain boundaries were created, leading to dark messy zones around the undeformed
region.
Fig.4.9 demonstrates two inverse-pole-figure maps for the ND direction of the CP-Ti
samples annealed at 550C. There was not much difference of the microstructure
between the cold rolled and then annealed at 550C (i.e.Fig.4.9a) and the one without
annealing (Fig.4.8a). But the microstructure of material rolled at 150C with
subsequent annealing at 550C showed some differences. There were a lot of nuclei
generated with different orientation from the matrix of the dark region which seems
more strained.
53
Fig.4.8 EBSD (inverse-pole-figure) maps for the ND direction of the CP-Ti samples
rolled at (a)room temperature,(b) 150C,(c)300C,(d)450C
(a) rolled at room temperature and annealed at 550C,(b) rolled at 450C and
annealed at 550C
Fig.4.10 illustrates the recrystallization behaviour of materials annealed at 600C for
one hour. In the IPF map for sample rolled at room temperature (i.e.Fig4.10a),
recrystallized grains distributed evenly with random orientation. Parts of the twins
54

were consumed by the recrystallized grains whereas some remained still. It is worth
mentioning that some grains were bigger than others. But it was hard to say these
grains were in the process of grain growth or they existed since as-received. The
recrystallization in sample rolled at 150C (i.e.Fig.4.10b) was much slower.
Nevertheless, some grains grew faster than others. Recrystallization processed not as
homogeneous as in cold rolled sample since some grains without any deformation and
a large twinned region have not recrystallized yet. Material rolled at 300C
(i.e.Fig.4.10c) and 450C (i.e.Fig.4.10d) gave a much more heterogeneous but faster
recrystallization. The un-recrystallized grains were the underformed grain clusters
with most of the orientation near <0002>//ND and this orientation seemed to form
most of the bigger recrystallized grains.
In general, cold rolling gives an even recrystallized microstructure while
recrystallization in samples rolled at 300C and 450C is more heterogeneous and
faster. Material rolled at 150C provides a transition stage between cold rolling and
hot rolling.
55

(a) rolled at room temperature and annealed at 600C ,(b) rolled at 150C and
annealed at 600C,(c) rolled at 350C and annealed at 600C,(d) rolled at 450C and
annealed at 600C.
(a) rolled at room temperature and annealed at 700C, (b) rolled at 450C and
annealed at 700C
Fig. 4.11 shows the progress of grain growth for cold rolling sample (i.e.Fig4.11a)
and warm rolling sample (i.e.Fig.4.11b). All the grains were recrystallized and have a
size larger than grains in samples annealed at 600C for an hour. Among those big
grains, several seem to have an advantage to grow and consumed the small ones
adjacent to them. Although the there was still a preferred orientation of basal pole
parallel to ND, the recrystallized and grown grains exhibited relatively random
orientations comparing to the status of rolled material.
4.4. Texture Evolution

The stereographic projected pole figures of CP-Ti rolled at different temperatures
were shown in Fig.4.12. Cold rolled sample exhibited a moderate basal texture in
which the basal poles preferred to concentrate at ND with a slightly detached
dispersion towards TD as shown in Fig.4.12a. After 30% reduction at 150C, a basaltransverse texture generated which was similar with the as-received texture, only with
56

some residual intensity dispersed on TD direction (i.e. Fig.4.12b). For samples rolled
at 300C and 450C (Fig.4.12c,d), the intensities were concentrated around the ND
for (0002) pole figure while less centred around ND for (
0) pole figure. Generally,
texture intensity was converged from the TD towards the ND after warm rolling.
Furthermore, intensity got strengthened when the rolling temperature increased.
Considering the prism poles, texture became more complicated after rolling. The
texture intensity peak around
30from ND to RD-TD plane got weakened when
materials subjected to rolling. However, in prism pole figure of sample rolled at

450C, the intensity peak split to 60from ND to RD-TD plane.
Fig.4.12 (0002) and (10-10) pole figures of the CP-Ti samples rolled at (a) room
temperature, (b) 150C,(c) 300C,(d) 450C
57
Fig.4.13 (0002) and (
) pole figures of the CP-Ti samples (a) rolled at room
temperature and annealed at 600C ,(b) rolled at 150C and annealed at 600C,(c)
rolled at 350C and annealed at 600C,(d) rolled at 450C and annealed at 600C,(e)
rolled at room temperature and annealed at 700C,(f) rolled at 450C and annealed at
700C.
After recrystallization proceeded, the peak position of the pole figure intensity did not
change much, however, the intensity of both the basal pole and the prism pole
decreased comparing with their deformation texture. Furthermore, there is a slight
decrease of intensity after recrystallization and the texture distributes more random
for both basal pole and prism pole as shown in Fig.4.13.e,f. All in all, the results were
similar with what Bozzolo et al.[31][29] noted that the rolling texture as well as the
recrystallization texture is very close with the major orientation around {0, 35, 0}
while the grain growth texture is around {0, 30, 30} in Euler space.
58
5. DISCUSSION
5.1. Deformation Microstructure
By measuring the IPF maps in Fig.4.8 of materials after deformation, the deformation
behavior can be divided into two series. Cold rolling and sample rolled at 150C
created many twins and deformation were more homogeneous whereas higher rolling
temperatures brought out more heterogeneous microstructure. Besides, DIC images in
Fig.4.3 illustrate different grain colours for the two series clearly which represents
different reflective properties of oxides layer in front of grains indicating different
orientations.
Fig.5.1.Boundary frequency plots map of specimens rolled at: (a) 25C, (b)150C,
(c)300C, (d)450C.
59

The hardness of the materials exhibited a monotonous decrease when rolling
temperature increased and latter two rolling temperatures there was almost no work
hardening. Boundary activity maps in Fig.5.1 also demonstrate different deformation
modes between lower rolling temperature and higher rolling temperature. The peak
around misorientation angle of 65 and 85 of the first two rolling temperatures
indicated the compressive ({
2}<
>) and tensile ({
}< 011>) twins
respectively, while in the latter two, twinning activities were fairly limited. Instead,
basal slip and prismatic slip got activated by higher temperature which is the reason
why the texture of CP-Ti plates rolled at 300C and 450C as shown in Fig.4.11c, d
exhibited a tendency of concentration in ND. At the lower temperatures, since the
stress along ND was compression, compressive (
2}<
>) twinning got
activated, resulting in a 65splitting from ND to TD texture as given in Fig.4.11a,b.

Fig.5.2 and Fig5.3 compared the orientations between ND reference direction and RD
as well as the deformation modes. Compression twinning in specimens rolled at room
temperature and 150C were generated more likely dependent on the orientation from
grains with (0002)//ND while tension twinning activated without a noticeable
dependence on special matrix of orientation [33].
By comparing the IPF maps based on ND and RD, we found that the green grains as a
reference to ND were almost <
>// ND and <
0>//RD without any
<0002>//RD grains and the blue grains were composed of <

<
0>// ND and
>//RD without any grains of <0002>//RD. The elongated grains were green
grains which exhibited a soft but stable orientation while those blue grains showed
unstable properties since they broke up and disappear during deformation. This
phenomenon was more obvious when specimens deformed at higher temperature of
300C and 450C. Almost all the blue and green grains have either disappeared
became too small to be visible.
The red grains based on reference direction of ND can be divided into two groups on
the basis of their behaviour during rolling. One is the <0002>//ND and <
0>//RD
grains. These grains were the red grains with reference direction of ND and green
grains in IPF map with the reference direction of RD. Regarding the twined red grains,
the rest of them stayed unbroken by and large. Another group is the <0002>//ND and
60

<
>//RD grains which were the red grains with reference direction of ND and
blue grains in IPF map with the reference direction of RD. These grains were
fragmented and broke up into small sections, especially distinct at 300C and 450C,
besides at this two temperature most of those huge grain clusters left were the stable
green grains for RD direction. In general, grains in the <
more stable than those in the <
0> fibre are significantly
> fibre, in agreement with the work by
Honniball.P.D et.al.(2014). As the deformation temperature increases, the difference

of CRSS for the slip systems increases (i.e Fig.2.4) and the Schimd factors changes
when the CRSS on the highest stressed planes is not identical. Then the unbalanced
shear stress leads to rotation of orientation. The rotation of <
0> orientation
reduces the Schmid factor of the active slip systems while <
> orientation
increases it and lead to rotation until the stable <
0> orientation along RD.
Fig.5.2 IPF maps along ND illustrating the twinning activity of samples rolled at
(a)25C,(b) 150C,(c)300C,(d)450C. Black boundaries: tensile twinning boundaries;
white boundaries: compression twinning boundaries
61
Fig.5.3.IPF maps along RD illustrating the twinning activity of samples rolled at

(a)25C,(b) 150C,(c)300C,(d)450C.
Fig.5.4 compares the misorientation and orientation spreads of CP-Ti specimens

rolled at room temperature and 300C. Two elongated grains exhibited the same
orientation by basal poles lain at 30from ND to TD and prism poles lain near RD,
which also supported the theory of stable grains that they did not break up. It seems
that warm rolling produced greater orientation spreads as well as more dislocation
tangles, leading to large misorientation and heterogeneous microstructure.
62
Fig.5.4.Misorientation profile and orientation spreads of two grains in CP-Ti

specimens rolled at room temperature and 300C.
When CP-Ti subjected to warm rolling, the huge unbroken grains clusters in
Fig.4.8c,d underwent less strain whereas those green and blue grains were deeply
deformed by high deformation temperature-activated slip systems and break up,
resulting in microstructure with much more inhomogeneity. The higher orientation
gradients as well as some deformation induced HAGBs might provide more
nucleation sites in the deformed matrix for subsequent recrystallization [66][67][68] .
The texture intensity of the samples in Fig.4.13 increased with the rolling temperature.
This phenomenon probably came from the effect of the remaining huge red grains
with strong intensity.
63
5.2. Static Recrystallization

The nucleation process of samples rolled at room temperature and 450C and
annealed at 550C for an hour is demonstrated in Fig.5.5. Clearly, cold rolling gives
an even nucleation while hot rolling brings an inhomogeneous and faster nucleation
than cold rolling. The nuclei in blue colour are activated in clusters where more strain
and stored energy exist. There are almost no recrystallized grains in the red deformed
matrix of both cold and hot rolled materials.
Fig.5.5 Nucleation analysis for samples (a) rolled at room temperature and annealed
at 550C ,(b) rolled at 150C and annealed at 550C. The representing colors of
deformed, substructured and recrystallized grains are red, yellow and blue
respectively.
The partially recrystallized maps in Fig.5.6 demonstrated the difference of
recrystallization behaviour in a more apparent way as well as the recrystallization
kinetic bar graph in Table 5.1. The number of remained deformed grains decreased as
the rolling temperature increased. Meanwhile, recrystallized grains were in the
majority, especially in samples rolled at 300C. Interestingly, the size of the new
grains was slightly smaller in hot rolled samples which might mean the growth rate
was faster in cold rolled material. This is because the grain growth in warm-rolled
samples is retarded by the remaining huge red grains even though they exhibited a
faster nucleation rate. Considering the higher nucleation rate in places with high strain
where deformation-induced HAGBs favour to develop as nucleation sites of the
warm-rolled samples, it can be concluded that the overall process of recrystallization
64

was more influenced by the nucleation rate than by grain growth rate [51]. Another
important factor enhancing the nucleation could be orientation gradient within grains.
Table 5.1 Recrystallization kinetics of CP-Ti annealed at 600C for 1 hour.
80.00%
70.00%
Fraction
60.00%
50.00%
40.00%
30.00%
Recrystallized
20.00%
Substructured
10.00%
Deformed
0.00%
25
150
300
Rolling Temperature ()
65
450

Fig.5.6 Recrystallization analysis for samples (a) rolled at room temperature and
annealed at 600C ,(b) rolled at 150C and annealed at 600C,(c) rolled at 350C and
annealed at 600C,(d) rolled at 450C and annealed at 600C.
As discussed in the literature review, HAGBs can be developed during subgrain

growth, and orientation gradient is needed in the deformed matrix to produce HAGBs
during recovery [51]. Hence, nucleation of warm rolled sample is enhanced due to the
higher orientation spreads (as discussed by Fig.5.4) provided by the increased
activities of diversified slip systems at elevated temperature.
Overall, in spite of the consumption of stored energy by dynamic recovery,
recrystallization was promoted by higher rolling temperature for not only the more
nucleation sites and faster nucleation rate, but also for the greater orientation spreads
and gradient provided by warm rolling.
As to the effect of different rolling temperature on grain growth process, there seems
to be no big difference. Grains with the orientation with around 30 have an
advantage to nucleate and undergo less pinning effect to grow up [31], resulting in the
grain growth texture centred around {0, 30, 30}.
66
6. CONCLUSIONS AND FUTUREWORK

6.1. Conclusions
On the basis of the results achieved by the investigation on deformation and
recrystallization of CP-Ti alloy, several conclusions can be drawn:
Firstly, it is found that work-hardening played an important role on specimens rolled
at room temperature, 150 and even on relatively high temperature of 300 ,
however, dynamic recovery was deeply enhanced when the rolling temperature
increased to 450, which resulted in a soften effect.
Secondly, the microstructure heterogeneity increases with rolling temperature. This
has a direct consequence on recrystallization: there are more nucleation sites and the
start of recrystallization is faster in the hot rolled material, whereas in the cold rolled
material there are less but more evenly distributed new grains.
Finally, although the textures are not very different near the end of and after
recrystallization, the recrystallized texture is stronger for the warm rolled material.
6.2. Future Work

Future work should be carried out in the future in order to address some outstanding
questions:
Simulations should be undertaken to study the effect of activities of twinning and all
kinds of slip during deformation. It is a good way to measure the results in theoretical
manner.
Another future work is to carry out the compression tests along the rolling direction or
the transverse direction to study the deformation behavior of those grains which are
the hard grains with their c- axis along ND.
67
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Fundamentals of Recrystallization in Titanium

A dissertation submitted to the University of Manchester for the degree of Master of

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

The final word count13827

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

rolling produced greater orientation gradients and more

Fundamentals of Recrystallization in Titanium Alloys

Fig. 1.1. SR71 aircraft[2].

Fig. 1.2.Titanium in GE-90 aero-engine[1].

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

Fig.2.1. Unit cell ofa phase andb phase [1].

Fundamentals of Recrystallization in Titanium Alloys

2.1.2. Classification and Alloying Elements

Fundamentals of Recrystallization in Titanium Alloys

Fig.2.2. Schematic representation of different alloying elements on titanium phase

Fig.2.3. Binary phase diagram of the a classification of titanium alloys [6].

Fundamentals of Recrystallization in Titanium Alloys

In phase, since it is hard to separate the solution hardening effects of precipitates,

Fundamentals of Recrystallization in Titanium Alloys

2.2. Deformation in HCP materials

2.2.2. Slip Modes

) prismatic plane as marked in Fig.1.1a. The main slip

> direction which is the most close-packed direction. According to

Von Mises criterion, it requires 5 independent slip systems for homogeneous

> slip directions there are 12 slip systems in

Fundamentals of Recrystallization in Titanium Alloys

Fig.2.4. <c+a>/<a>Prism and <a>Basal/<a>Prism slip ratio as a function of

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

}< 011> is the most important twinning

1}tension twinning, and {

2} compression twinning[1]. In a hexagonal metal,

magnitude of twinning shear hence they are the easiest to activate.

Fundamentals of Recrystallization in Titanium Alloys

4} which are high order

} twins replace the former {

2} twins since the basal plane is sharply

2.2.3. Deformation Texture

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

to rolling direction, as shown in Fig.2.6c.

> . The secondary peak is centered at a

position around 1=0, = 32, 2=30which represents (

0> [30]. The

2} compression twinning and {

A more detailed deformation texture evolution of titanium with different rolling

0} maximum shift along the rolling direction and becomes

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

Fundamentals of Recrystallization in Titanium Alloys

Where is a frequency factor, and Q is the activation energy for diffusion.

Fundamentals of Recrystallization in Titanium Alloys

Where is the density of a deformed material, c2 is a constant of 0.5 and G is the

Fundamentals of Recrystallization in Titanium Alloys

Fig.2.10 Schematic diagrams of recrystallization by high angle boundary migration

b per unit volume, the total

bulging area interfacial energy is defined as:

Fundamentals of Recrystallization in Titanium Alloys

then we have R >

,which means as long as the boundary bulge to