Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

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Journal of Science: Advanced Materials and Devices

journal homepage: www.elsevier.com/locate/jsamd

Review Article

Recrystallization mechanisms and microstructure development in

emerging metallic materials: A review
Kenneth Kanayo Alaneme*, Eloho Anita Okotete
Department of Metallurgical and Materials Engineering, Federal University of Technology, Akure, PMB 704, Nigeria

a r t i c l e i n f o a b s t r a c t

Article history: This review is devoted to the understanding of the recrystallization mechanisms and its role in the
Received 27 October 2018 control of the microstructure in emerging metallic materials. Recrystallization is a very pervasive
Received in revised form transformation phenomenon that is considered to be very important in efficient microstructure designs.
19 December 2018
Currently, there is hardly any work which has attempted to present a concise and systematic review of
Accepted 20 December 2018
Available online 28 December 2018
the recrystallization in emerging materials with a view to reconcile its manifestations with trends
established from recrystallization studies in traditional alloys. This review aims to address this by first
reviewing the fundamental and nascent recrystallization mechanism concepts and then analyzing their
Keywords:
Recrystallization mechanisms
forms in emerging metallic materials, such as high strength steels, Ti- and Mg-based alloys, as well as
Microstructure high-entropy and shape-memory alloys. The reviews on these systems show that the classic recrystal-
Deformation processing lization concepts are still relevant for explaining the recrystallization behavior and by extension to the
Stored energy microstructure development in the materials. However, in some instances, structural factors exclusive to
Emerging metallic materials these materials influenced the driving force and recrystallization behavior yielding outcomes sufficiently
distinct from that observed in traditional alloys. Basically, deformation processing and material factors
such as stress accumulation, inhomogeneous strain distribution, stored energy, available slip systems,
phase composition, microstructural variability, initial grain size, texture, stacking fault and lattice
distortion energies, strain path, deformation temperature, and solute clustering and diffusion rates were
at play in determining the recrystallization mechanisms and kinetics in these emerging metallic
materials.
© 2019 The Authors. Publishing services by Elsevier B.V. on behalf of Vietnam National University, Hanoi.
This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

1. Introduction microstructures in metals is the recrystallization. Its prominence is

due largely to its capacity to control the structure and properties,
In the design of metallic materials, materials scientists and en- specifically structure-sensitive properties of materials [2]. This has
gineers are always conscious of the functionality which is a great made it of great scientific interest over the years, since it can be
determinant of technical efficiency and performance of materials in utilized to control several physical, mechanical and technological
service, and a vital factor influencing materials service life. Tradi- properties of materials [3]. Processes involving the development of
tionally, developing high performance metallic materials was pur- conventional alloys, super plastic alloys, thermo-electric materials
sued by appropriate alloying and heat-treatment, which help in the (semiconductor alloys), thermomechanical processing, powder
development and control of microstructures to meet the target metallurgy, metallic thin films and several other materials pro-
properties [1]. In this regard, several transformation phenomena cessing operations rely on the application of the recrystallization
are explored in structure and property control in metallic materials mechanisms [4]. Although predominantly applicable for the design
depending on the composition and the nature of the phase of metallic microstructures tailored to possess properties for spe-
constitution of the metallic system. One of the most influential cific applications, it has also been employed in polymers [5] and
transformation phenomena vastly applied in the development of ceramics [6].
Recrystallization refers to groups of processes which can man-
ifest stress relaxation to varied extents in a deformed metal by
* Corresponding author.
releasing the stored energy generated from the deformation pro-
E-mail address: [email protected] (K.K. Alaneme). cess when heat-treated at an appropriate temperature [2,7].
Peer review under responsibility of Vietnam National University, Hanoi.

https://doi.org/10.1016/j.jsamd.2018.12.007
2468-2179/© 2019 The Authors. Publishing services by Elsevier B.V. on behalf of Vietnam National University, Hanoi. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/).
20 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

Understanding of the mechanisms of recrystallization evolved over reasons for the type(s) of recrystallization behaviour observed in
time from its first mention in scientific communications recorded several metallic material systems.
in 1885 [7], to the epochal works of Cahn [8,9], Cottrell [10], and a
host of other eminent scholars whose contributions are detailed in 2. Stored energy e driving force for recrystallization
several classic reviews on the subject [2,3,11]. Perhaps some of the
most exciting breakthroughs in recrystallization studies were the The driving force for recrystallization is the amount of stored
understanding of recrystallization nucleation mechanisms [11], and energy within the metallic material. This energy arises from the
the unravelling of recrystallization mechanisms when influenced lattice strains and the crystalline imperfections generated in the
by intervening metallurgical reactions such as solid solution de- material during deformation processing. The bulk of the energy
compositions, precipitation, crystallographic phase changes, and generated during the deformation of a metallic material is dissi-
coalescence of phases [12]. pated as heat with only a small fraction of the energy stored in the
Recrystallization nucleation mechanisms were subject of material. Martin et al. [28] reported that the greater proportion of
contention for several years. It is now appreciated that the recrys- the stored energy is contributed by the crystal imperfections (dis-
tallization nucleation mechanism differs from that characteristic of locations and point defects) with dislocations being the major
conventional phase transformations where classical nucleation contributor. A deformation process such as cold working, is known
theories are applicable [13]. The nuclei which give rise to new to increase the dislocation density in a metal to an estimated
recrystallized grains are believed to be already present in the 1016m
2 from approximately 1010
12m
2, which is observed in the
deformed state where the deformation structures with high local unworked state. It can then be understood why they contribute to
orientation gradients constitute the pre-deformed nuclei [14]. the stored energy as each dislocation being a crystal defect gener-
Recrystallization mechanisms tend to compete with other ates lattice disturbances in form of strains within its vicinity. The
phase reactions for the stored energy from the defect structure of increased lattice strain is associated with the increase in strain
metallic systems, accumulated during deformation processing. energy in the metal [29].
This stored energy serves as driving force for the recrystallization/ Several factors, both processing and material variables, have
structural transformation to occur [15,16]. The competition been reported to influence the amount of the stored energy in
among the contending phase reactions can either suppress, occur deformed metals. The type and severity of the deformation
concurrently with, or accelerate the recrystallization process [16]. including the deformation temperature, composition and metal-
The unpredictability of the transformation process, generally lurgical nature of the metallic system are some of the factors which
creates a confused scenario, difficult for an effective and optimal will be discussed.
microstructure design. Detailed scientific explanations on how to Generally, the less the complexity of the mode of deformation,
explore effectively recrystallization occurring with intervening the lower the stored energy. Martin et al. [28] adduced that this is
phase reactions to develop high strength recrystallized textures in because simpler deformation processes, involve less stress gradi-
metallic materials, have been provided by Hornbogen [17e19] and ents with little or no friction and redundant work. This has also
Kamma [12,20]. been corroborated by several works which compared stored energy
Presently, metallic materials processing and development of deformation between different metal working processes [32,33].
approaches have evolved over time with novel plastic working Zhang et al. [34] studied the effect of strain path on deformation
and forming processes such as severe plastic deformation and recrystallization in high purity tantalum. They reported the
applied in microstructure design and control. Also, advanced formation of different textures during unidirectional rolling and
metallic materials (such as Ti based alloys, Mg and alloys, high clock rolling deformation processes. Workhardening rates which
entropy alloys, shape memory alloys, biomedical alloys and reflect the pace at which the dislocation density in a deformed
weight saving high strength steels) characterised with unusual material increases is strongly dependent on the temperature. The
phase compositions and constitutions have opened new fron- rate of workhardening usually increases with the decreasing tem-
tiers for industrial, structural, biomedical and technological ap- perature, since the process of energy release occurring during or
plications of metallic materials [21e24]. A great success in the immediately after the deformation are suppressed to a greater
use of these emerging metallic materials is strongly dependent extent [35]. For instance, He et al. [36] observed from their study on
on the ability to harness the rare property variety they can avail cryo-rolling and the recrystallization of the hexagonal Zr-4 alloy
e a factor depending on the microstructure control and opti- that the intensity of the heterogeneous deformation in cryo-rolling
mization. Recrystallization processes have been observed to be performed at
7  C is more severe than that in room temperature
important in the development of microstructures in deformation rolling. Lu et al. [25] reported that the dynamic recovery is normally
processed metallic materials [25]. suppressed during cyro-rolling which in the case studied, was
Several insightful reviews which are classics on recrystalliza- carried out below 0  C, resulting in a higher deformation energy
tion are available in literature: Doherty et al. [11] covered majorly storage (Fig. 1). Materials variables such as melting point, alloying,
the fundamentals of recovery and recrystallization processes grain size and orientation, and the presence of second phase par-
while Rios et al. [2] focussed more on understanding the ticles, have also been reported to influence the amount of stored
recrystallization nucleation and growth mechanisms. Recent re- energy in deformed metallic materials [28]. The effects of these
views by Sakai et al. [3], and Huang and Loge [26] are more variables are summarized in Table 1.
devoted to theories and models in dynamic recrystallization
processes. Few review articles exist which have discussed both 3. Recrystallization mechanisms
fundamental and nascent recrystallization concepts - such as
recrystallization in non-deformed metals subjected to electric If deformation processing is performed at temperatures that are
current stressing [27], and recrystallization mechanisms in low (less than 0.1) relative to the absolute melting temperatures of
emerging metallic materials, the primary concern of the present a metallic system, there will be a high likelihood for defect accu-
review. This review covers recrystallization mechanisms in mulation to occur resulting in an increase in the stored energy [44].
selected deformation processing and emerging metallic mate- The deformed state due to defect accumulation and work hard-
rials. This is preceded by a concise look at some of the funda- ening is thermodynamically unstable. It is also usually accompa-
mental concepts of recrystallization, which help in explaining the nied with changes in mechanical properties and other material
 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33 21

Fig. 1. EBDS orientation maps room temperature rolled (a, c) and cryorolled CueAg alloys (b,d) annealed at 300  C (a, b)and 400  C (c, d) (Culed from Lu et al. [25] with permission
from Elsevier). It shows that cryorolled CueAg alloys have local areas of recrystallized grain at low annealing temperatures compared to room temperature rolled CueAg alloys
because of higher stored energy during deformation.

Table 1
Influence of material variables on stored energy.

Variable Effect on stored energy

Melting Point Stored energy decreases with decreasing melting point (exceptions exist!) [28]
Foreign Atoms Elastic stress field interactions between atoms and dislocations allows larger amount of energy to be stored [37,38]
Grain size and Orientation At same strain, fine grains result in greater accumulation of dislocations resulting in higher stored energy in comparison to coarse grains
[25,30,39]. Different grain orientations have varying slip accommodation and hence have different values of stored energy [31]
Vacancy Concentration High vacancy concentrations induced from high strains increase the stored energy [40]
Second phase particles Influence dependent on volume fraction and applied strain [2].
Coherent precipitates which are deformable with the matrix results in increased yield strength due to coherency strains, and several
short range interactions [41,42]. For non-deformable second phase particles, much higher dislocation density (reflecting higher stored
energy is achieved) in comparison with single phase metals [28].
Crystallographic texture Generally orientations, planes or directions which favor easy slip will result in lower stored energy because of lesser dislocation
accumulation [31]. Dislocations pile up easily along grain orientations, planes and directions where slip is constrained hence more
stored energy will be amassed [29].
Stacking fault energies Stacking fault energies influence dislocation mobility and morphology e in high stacking fault energy metals (such as Al) there is ease of
dislocation movement by glide, climb and cross slip during plastic deformation, thus less dislocations are accumulated resulting in low
stored energy [43]. Low stacking fault energy metals (such as Mg) restrict the mobility of dislocations and as a result accumulate high
dislocation densities which increases stored energy [43].

properties, such as electrical conductivity and corrosion resistance The recrystallization mechanism with the capacity to eliminate
[45]. For such an unstable system, there is a natural tendency to almost all the deformation induced dislocations in worked metallic
revert to the unworked or annealed state so as to minimize its materials is referred to as the primary recrystallization. Simply
overall energy. Reverting to the unworked state will require acti- stated, it is the process of formation and growth in a deformed
vating the stored energy release which can eliminate the defects matrix of new grains which are distortion free and appreciably
locked in the material. These processes usually require heating, and more perfect than the proper matrix and are separated from the
depending on the activation energy, results in different levels of latter by large angle boundaries [14]. This process is propelled by
stress relaxation, namely: recovery and recrystallization. the excess volume energy accumulated during the prior plastic
Recovery is the term used to refer to multi-stage processes deformation, and is mostly localized in the stress fields which
which result in the redistribution and annihilation of point defects surround the dislocations formed by deformation [50]. The acti-
and the redistribution and annihilation of dislocations either vation energy for the recrystallization is generally higher than that
without the formation of new boundaries or with the formation required for the polygonization and point defect annihilation. The
and migration of low angle boundaries [26,46]. Recovery processes activation energy, however, changes all through the recrystalliza-
are basically divided into two types - the processes involving the tion process as the stored energy is used up [50].
redistribution and the elimination of point defects (point defects A critical amount of deformation is reported to be prerequisite
annihilation) [47,48], and the processes resulting in the rear- for the primary recrystallization to occur during heating [51]. Above
rangement and the partial annihilation of dense dislocation net- the critical deformation, the recrystallization nuclei are postulated
works formed by the glide and interaction of dislocations during to appear during heating and are formed first of all in portions of
cold working - a phenomenon referred to as polygonization [49]. the crystal lattice that have been most severely misoriented and
Both processes generally result in the release of some of the stored distorted by the cold work. Haasen [50] pointed out that recrys-
energy arising from deformation. tallization commences in the areas of high dislocation density, and
22 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

at sites where the deformation is inhomogeneous. The mechanism stressing on the microstructure of non deformed brass is presented
of the primary recrystallization has led to the sub-classification of in Fig. 2.
the process. It is often referred to as static recrystallization when During the hot plastic deformation of metals and alloys, two
the process is propelled by annealing after prior cold working. The competing processes occur in parallel, strain hardening and soft-
term ‘discontinuous’ static recrystallization is used when recrys- ening ones. The strain hardening effect is due to the increase in the
tallization proceeds by a two stage process of nucleation and dislocation density under the action of external forces and to the
growth of new grains within the deformed microstructure [26]. interaction of dislocations which form dislocation pile-ups of
However, it should be noted that the origin of a recrystallized grain various degrees of stability and mobility [59]. The softening process
is reported to always preexist in regions that are highly misoriented consists in a decrease of the dislocation density and in the redis-
in relation to the material surrounding it. This high degree of tribution of dislocations into energetically more stable configura-
misorientation also gives the region from which the new grain tions. The dislocation redistribution is due to the vacancy climb, the
originates the needed growth mobility [52]. New recrystallized formation of recrystallization nuclei and their growth by the
grains are also formed by a process known as continuous static migration of large-angle boundaries under appropriate conditions
recrystallization. This involves gradual localized migration of sub- (temperature, amount and rate of deformation) [60]. When these
grains formed during severe deformation when subjected to processes occur during the high temperature deformation of ma-
annealing [53]. terials the structures formed are taken to be formed via the dy-
Some factors such as temperature, extent and complexity of namic recrystallization.
deformation, grain size, melting point and purity of metallic ma- The mechanism of dynamic recrystallization has been shown to
terials, presence of foreign atoms and second phase particles, be dependent on factors, such as the temperature, the amount and
stacking fault energies and crystallographic texture which affect rate of deformation, the stacking fault energy, the initial structural
stored energy of deformation are well known to influence the state, and the phase composition of a material [61]. Since the dy-
primary recrystallization process [28]. The influence of stacking namic recrystallization requires strain hardening and softening to
fault energies, melting point and purity levels of metallic materials occur in parallel, the final structure is strongly dependent on the
are summarised in Tables 2 and 3. aforementioned factors, albeit in a complicated manner. Dynamic
Recently, it has been reported that an electric current also in- recrystallization (DRX) is classified, on the basis of the mechanism
fluences the recrystallization kinetics [57]. The exposure of a cold- of formation of new grains, into discontinuous dynamic recrystal-
worked metal deformed at large deformation strains to an alter- lization (DDRX) and continuous dynamic recrystallization (CDRX).
nating electric current during annealing is reported to accelerate DDRX is a fast pace DRX process which proceeds by the nucleation
the recrystallization process [58]. This is because of greater sensi- of new grains at the expense of old deformed grains during high
tivity of sub grain/grain structures to the electron wind effect which temperature plastic deformation. DDRX mostly occurs in low
helps accelerate the grain boundary motion. This is coupled with stacking fault energy metals (Mg, Zn) where the dynamic recovery
the increased vacancy density facilitated by the applied current is suppressed [62]. DDRX is usually preceded by the serration and
which aids the motion of sub grains [57]. Liang and Lin [27] also bulging of pre-existing grain boundary and the recrystallization is
showed that recrystallization can be induced in non deformed confirmed by the appearance of a necklace structure [63]. CDRX
metals exposed to direct current stressing. They discovered that occurs by the migration of subgrains with low angle boundaries
direct electric current stressing produces a high dislocation density formed within the deformed structure into grains with high angle
in Cu36Zn brass, based on observations from EBSD and TEM anal- boundaries during straining at high temperature [64]. CDRX is
ysis. The recrystallization was triggered in situ by the Joules heat often preceded by the dynamic recovery and mostly occurs in high
generated during the electric current pulse treatment. The direct stacking fault energy metals.
current stressing followed by rapid quenching was reported to Dynamic recovery is a phenomenon associated with the defor-
result in substantial improvement in grain size refinement and mation processes undertaken at temperatures at which wholesale
micro-hardness. The extent of recrystallization was observed to sweeping of dislocations may not be energetically favoured [65].
depend on the period of current stressing which affected the Under such conditions the pace of defect generation (dislocation
amount of Joules heat supplied to the material. The longer the increase) is greater than that of the dislocation annihilation. That is,
current stressing period, the greater the likelihood of achieving only partial elimination of dislocations occurs under such condi-
complete recrystallization. Electromigration of atoms from their tions. In some metallic systems deformed at room temperature,
lattice positions and thermal expansion during joule heating were dynamic recovery has been reported [28]. The deformation induced
noted as the driving force for the recrystallization. This phenome- store energy in such material at room temperature is observed to be
non (recrystallization in non-deformed brass) has not been lower than that when processing is carried out under cryogenic
corroborated by other authors, or reported for other metallic ma- conditions such as cryo-rolling [30,66]. This is because the dislo-
terials, so it would be fascinating to see the response of other cation mobility is hindered during cryogenic deformations, hence
metallic materials to such direct electric current stressing. The suppressing the dynamic recovery. This leads to a high accumula-
micrographs confirming the influence of direct electric current tion of dislocations and an increase in potential nucleation sites for
new grains during annealing [66,67]. Fig. 3 illustrates the idealised
evolution of microstructure in hot deformed metals for cases where
Table 2 dynamic recovery and dynamic recrystallization are the activated
Influence of stacking fault energies on stored energy and recrystallization mode recrystallization mechanisms.
[43,54,55]. Grain growth also referred to as normal grain growth or
Stacking Fault Stored Energy Recrystallization mode continuous grain growth normally sets in after the primary
Energy recrystallization, as the growing recrystallization nuclei begin to
High Low Dynamic recovery, impinge on one another. It is characterized by the growth of some
(Al, b-Ti, ferritic steels) Continuous dynamic new grains at the expense of other newly formed grains resulting in
recrystallization a microstructure with a narrow range of grain size and shape
Low/Medium High Discontinuous dynamic [48,68]. The principal thermodynamic driving force of the grain
(Cu, Mg, Zn) recrystallization
growth is the tendency to diminish the overall grain-boundary
 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33 23

Table 3
Influence of melting point and purity levels on average grain size of annealed and HPT processed metals at 300K and 100K (adapted from Edalati et al. [56]).

Metals Zn Mg Al Cu Nb

Purity (%) 99.99 99.9 99.999 99.99 99 99.99999 99.99 99.9

Crystal Structure HCP HCP FCC FCC BCC
Tm (K) 693 922 933 1357 2740
gSFE (mJ/m2) 140 125 166 45 150
Grain size, ds (mm) Anneal 390 1600 >4000 1000 160 310 150 50
HPT 300 K 20 1.0 3.5 1.3 0.38 0.30 0.29 0.24
HPT 100 K 20 2.7 3.8 2.2 0.16 0.080 0.073 0.041
Self -Anneal 1.5 20

Fig. 2. (a) The EBSD image of the annealed as-prepared specimen shows dislocation of free grains. The EBSD image in the middle of the specimen (b) 4 h, 10 cycles (Curled from
(Liang and Lin [27], with permission from Elsevier) (Larger grains exhibit prominent colour contrast, The non-uniform color is ascribed to the high dislocation density induced by
current stressing).

‘surface’ energy [69]. Thus as the grains grow in size and their Some abnormal grain growth, that is the exaggerated growth of
numbers decrease, the grain boundary area diminishes and the some grains at the expense of others, is often observed after pri-
total surface energy is lowered accordingly [69]. mary recrystallization [47]. A typical microstructure of a metal that
24 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

Fig. 3. Evolution of microstructure during hot deformation of a material showing (a) dynamic recovery (b) dynamic recrystallization (Curled from Verlinden et al. [48] with
permission from Elsevier).

has undergone an abnormal grain growth show the growth of just a between 5 and 50% before annealing treatment at temperatures
few grains to very large diameters. This grain growth variant is between 673 (400) and 998K (725  C). It was observed from the
known as discontinuous grain growth, or secondary recrystalliza- study that softening of the test material readily occurred at
tion [43]. It occurs due to anisotropic properties of emerging grain annealing temperatures above 855 K (612  C) and the full recrys-
boundaries after recrystallization. The grain boundary anisotropy is tallization was observed in the material subjected to 973 K (700  C)
initially characterized by the inequigranularity, which is facilitated annealing temperature after 100 s. These observations were
by factors such as disparity in grains concentration of defects attributed to the presence of microtwins in the deformed structure
(volume energy), size, crystal orientation, dispersion of pre- which hindered recrystallization at lower annealing temperatures.
cipitates, second phases and impurities, structural and topological On the other hand, the fully recrystallized structure at high
characteristics [43]. annealing temperatures was characterized with the absence of
The recrystallization mechanisms discussed are drawn largely microtwins but this does not mean that the microtwins served as
from observations in traditional metals and alloys. How the preferential sites for the nucleation of new grains. The recrystalli-
recrystallization behavior is influenced by novel deformation pro- zation process was, however, associated with sweeping of bound-
cessing and in emerging materials, has not come under much aries of growing grains in which the deformation substructure
scrutiny. The recrystallization behavior and how it is harnessed in discontinuously disappears as the process proceeds. The texture of
the microstructure design in emerging metallic materials, are the the material appeared unchanged after the recrystallization and
concerns discussed in the succeeding section. this was attributed to the nucleation and growth of the recrystal-
lized structure without any preferred orientation as a result of the
4. Recrystallization mechanisms in emerging metallic energetically homogenous deformed structure.
systems Saha et al. [75] developed a fully recrystallized nanostructured
high Mn austenitic steel through conventional rolling and annealing.
4.1. Recrystallization mechanisms in high strength steels The research was aimed at producing ultrafine grained materials
which have a good balance of strength and ductility. The test ma-
High strength steels (HSS) are steels whose composition and terial was a Fe-31 wt. %Mn-3wt. %Al-3wt. %Si TWIP austenitic steel
structure have been metallurgically modified to provide a superior which has a high strength and a large ductility. A hot rolled plate of
combination of mechanical properties like strength, toughness, this steel was subjected to multiple passes of cold rolling under
ductility and formability [70,71]. These steels are modified using lubrication to about 92% reduction in thickness, and subsequently
the microalloying technology and thermomechanical treatments subjected to annealing treatments at 650  C for several period of
and are mostly developed for the use in automotive, petrochemical time. The presence of elongated regions, black points and low angle
and petroleum industries [72,73]. Examples of HSS are high Mn boundaries in the microstructure of test specimens annealed for
alloy steels, twining induced plasticity steels, transformation 0.18 ks at 650  C was indicative of the partial recrystallization at this
induced plasticity steels, complex phase steels and martensitic treatment time. It was, however, observed that as the annealing time
steels. The microalloying technology and thermomechanical was increased to 0.3 ks and 1.8 ks very fine and equiaxed grains were
treatments utilized in the development of these new generation observed in the microstructures depicting full recrystallization of the
HSS trigger metallurgical reactions (recrystallization processes in- test specimens. It was also established that the mean grain sizes
clusive) which influence the microstructures developed and ulti- (average 400 nm) observed in the fully recrystallized steel structure
mately the engineering properties. studied surpassed grain sizes previously reported for other metallic
Bracke et al. [74] investigated the recrystallization behavior of systems which were fully recrystallized. These observations were
the low SFE FeeMneC based alloys processed with twinning attributed to the low stacking fault energy of the high Mn steel under
induced plasticity (TWIP). FeeMneC alloys have exceptional me- study which greatly inhibits a dynamic recovery of dislocations
chanical properties like high ultimate tensile strength during rolling deformations at ambient temperatures resulting in a
(600e1000 MPa) and elongations (15e25%), which has informed its nanosized lamellar structure with a high dislocation density. Shear
use in automotive applications where high strength is required. The banding further subdivides the lamellar structure into finer length
test material (a fully austenitic FeeMneC steel) was hot rolled and scale which introduces more misorientation, and such deformation
quenched in water prior to the deformation process. Subsequently structures enhance the formation of recrystallized grains during
the material was subjected to cold rolling with total reductions annealing.
 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33 25

The dynamic recrystallization mechanism of the Fe-8 wt.% Al low accumulation during the deformation and this corresponds to a
density steel under hot rolling conditions was investigated by Castan critical strain value.
et al. [76]. These steels are reported to have tendencies to exhibit Layus et al. [35] studied the recrystallization based formation of
surface defects referred to as roping (surface corrugations parallel to the uniform fine grained austenite structure in high strength steels
rolling direction) which originates from the inhomogeneous orien- for artic applications. This study was necessitated by the need to
tation distribution of individual grains. The purpose of the research develop low cost high strength steels with excellent low temper-
was to understand the conditions of recrystallization during hot ature properties for artic marine construction. The test material
rolling which can control the microstructure and curb the occurrence was a cold resistant high strength F620 steel micro-alloyed with Nb
of roping in this steel. The steel for the test was rolled in three suc- and V to improve the aforementioned properties of the steel. Dy-
cessive passes which accumulated to a total deformation of 1. The namic recrystallization was observed to be hindered in the steels
dynamic recrystallization behavior of the steel was studied by per- studied (Nb and V micro-alloyed steels) and this was a function of
forming the hot torsion test in a direction involving a negative shear the micro-alloying constituents which restricted the threshold
and under argon atmosphere to reduce the oxidation phenomena. strains for the deformation during processing at temperatures be-
The test was performed within a temperature range of 900e1100  C tween 950 and 1150  C. The effect of the micro-alloying constitu-
and a strain rate range of 0.1e10 S
1. The deformed test samples were ents on the dynamic recrystallization behavior of F620 high
quenched immediately in argon to preserve the microstructure and strength steel was observed to be sensitive to higher deformation
avoid post dynamic-recrystallization. It was observed from the study temperatures and DRX ceased in both steels at 950  C. The obser-
that the test material undergoes continuous dynamic recrystalliza- vations imply that a uniform fine grained austenite structure
tion (CDRX) at lower temperature (1000  C) and lower strain rates cannot be formed during high temperature processing of the
(0.1 S-1). This was evident in the presence of subgrains formed close modified F620 steels since the strain accommodation is hindered in
to the initial grain boundaries which gradually replaced the initial the steels. Consequently, the stress relaxation method was used to
large grain structure with finer recrystallized grains. The observa- investigate the static recrystallization behavior of the steels using
tions were linked to the simultaneous action of strain hardening and the Gleeble 3800 simulator. The test specimens were subjected to
dynamic recovery which results in the redistribution of the dislo- five sequential strains with unregulated pauses and regulated
cation and the formation of subgrain boundaries, which divide initial pauses in the first and second treatment steps, respectively, and the
grain boundaries to subgrains. On the contrary, small and equiaxed pause duration was selected to give room for the complete primary
freshly recrystallized grains free of substructure were observed in the static recrystallization. Uniform fine grained recrystallized
steel subjected to higher processing temperatures (1000  C) and austenite was observed in specimens subjected to treatment with
higher strain rates (5 S
1 - 10 S
1). This is indicative of the activation regulated pauses. Thus, it is necessary to gradually increase the
of the discontinuous dynamic recrystallization (DDRX) which is not pause duration during the successive deformation within the pro-
commonly associated with high stacking fault energy materials like cess temperature for both steels to ensure complete static
ferritic alloys but can be a function of specific deformation condi- recrystallization.
tions. At these processing conditions the rate of strain hardening is The studies reviewed show that the recrystallization in high
very high and renders the dynamic recovery less effectively leading strength steels is basically influenced by factors, such as the amount
to accumulated dislocation densities and stored elastic energy which of stored energy, the defect structure, the amount of strains, the
is the driving force for the formation of new recrystallized grains. The annealing temperature and time. Some defects, such as microtwins
nuclei usually appears near the original grain boundaries and is when present in the deformed structure can hinder the recrystalli-
formed either by the accelerated rotation of a particular subgrain, zation at low temperatures while shear bands in the deformed
coalescence of adjacent subgrains or local migration boundary into structure contribute to more misorientation in the deformed struc-
the interior of neighboring grain. It was also noted that the grains ture, thus, facilitating the recrystallization. Also, low stacking fault
recrystallized by DDRX had no preferred orientation (low texture energies observed in some of these steels inhibit the dynamic re-
intensity) which would reduce the tendency of roping in these steels. covery of dislocations, thereby contributing to high dislocation
The dynamic recrystallization behavior of a high strength low densities. However, some deformation modes can readily activate
alloy steel during hot deformation was investigated by Wu et al. the DDRX in high stacking fault energy materials, even when con-
[77]. The aim of the study was to assess the role of strain, strain rate ventional thought supports the contrary. That is, the deformation
and temperature on the compressive deformation characteristics of modes where the rate of strain hardening is very high can suppress
the steel with a view to understanding optimum processing con- the dynamic recovery resulting in an accumulation of dislocations
ditions. Hot compression test was used in the study and performed with the corresponding increase in the stored energy which facili-
within a temperature range of 950e1150  C under strain rates of 0.1, tates the recrystallization of new grains. The increase in the defor-
1 and 5 S
1 up to a true strain of 0.9 using a Gleeble-500 thermo- mation temperature and the decrease in the strain rate of high
simulation machine. The test specimens were heated to 1200  C at strength steels favors the dynamic recrystallization as both condi-
a rate of 10  C/s and held for 3 min, then cooled to the deformation tions help the softening process by increasing the mobility of grain
temperature within the range 950e1150  C at a rate of 5  C/s and boundaries and providing longer time for the dislocation annihila-
held for 30 s. After the hot deformation, the test specimens were tion to occur. Lastly, the presence of some micro-alloying elements,
quenched immediately in tap water. It was observed from the study such as V and Nb in high strength steels can hinder the formation of
that the dynamic recrystallization (DRX) occurs easily with the the dynamic recrystallization, as they restrain the strain accumula-
increase in the deformation temperature and the decrease in the tion, a critical amount of which is required for the dynamic recrys-
strain rate. This is because these processing conditions support the tallization to occur.
softening process by increasing the mobility of grain boundaries
and providing longer time for the dislocation annihilation and the 4.2. Recrystallization mechanisms in Ti based alloys
occurrence of DRX. The study further established that work hard-
ening dominated the initial stages of straining during the high Ti and Ti based alloys are currently of growing engineering in-
temperature deformation. However, as the deformation tempera- terest attributed to their light weight and good engineering prop-
ture is increased the softening rate equalled and surpassed work erties (such as good fatigue strength, good anticorrosion and
hardening. DRX was summed up to occur at a critical level of stress biocompatibility, relatively low modulus and high specific strength
26 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

to weight ratio) [78,79]. Thus, these alloys are attractive for mate- fault energy of the g phase in the alloy is lower than that of the a2
rials selection in biomedical, aerospace and automotive applica- phase, hence, the dynamic recrystallization is favored in the g
tions [80]. TieAl based alloys are among the most amenable Ti phase and the dynamic recovery favored in the a2 phase. The re-
based alloys for use in high temperature applications because of the sults show that even at high deformation temperature, the TNB
excellent combination of low density, high strength, good creep alloy would still contain remnant lamellar since the a2 laths do not
and oxidation resistance they possess [22,81]. Lately, TieAl based break into recrystallized grains after the deformation. It was
alloys are being alloyed with Nb to stabilize the beta phase and therefore proposed that reducing the deformation resistance by a
refine the microstructure, giving rise to a new TieAleNb (TNB) multistep processing where the deformation proceeds from high to
alloy. The TieAleNb (TNB) alloys are now being considered as the low temperatures can help produce a fine and homogeneous
substitute for the nickel based superalloys in high temperature microstructure. High deformation temperatures would form rela-
applications [82]. However, the poor plasticity at ambient tem- tively fine microstructure, while grain boundary sliding promotes
perature which is associated with the specific crystal structure of Ti the homogeneity of microstructure; and further refinement could
and its alloys remains a major setback to the use of the TNB alloys be achieved by processing at lower deformation temperatures.
[22,83]. Grain refinements via thermomechanical treatment have Experimental study and numeric simulation of the dynamic
been explored to reduce the deformation resistance of TNB alloys. recrystallization behavior of TieAl based alloy was investigated by
In view of this, several studies have been embarked on to under- Wan et al. [83]. This was achieved by subjecting a Ti - 47Al e2Nb e
stand the dynamic recrystallization behavior of TNB and other 2Cr alloy produced via powder metallurgy to thermomechanical
TieAl based alloys. simulations. The compression test samples were deformed by the
Li et al. [84] investigated the effect of hot forging on the hot compression carried out in a Gleeble 1500D simulator at tem-
microstructure and the mechanical behavior of a high Nb content peratures of 1223e1473 K (949.85e119.85  C) at a strain rate of
containing TieAl based alloy. This study was centered on using pack 0.001 S-1 to 0.1 S-1. The samples were subjected to 55% reductions
forging for processing of the Ti e 45Al e 7Nb e 0.3W alloy. Pre- (3 ¼ 0.8), and immediately quenched in water to preserve the
alloyed powders of predetermined compositions were prepared deformed microstructure. The initial microstructure was composed
using plasma rotating electrode processing. The pre-alloyed pow- of equiaxed strain free grains with large volume of high angle
ders were compacted into cylindrical billets and then quasi- boundaries. The alloys deformed at 1323K (1049.85  C)/0.05 S-1
isothermal forging was carried out on the billets at a temperature were characterized with a mixture of coarse un-recrystallized
of 1280  C and at the strain rate of 0.1 S-1 with a total strain of 80%. It grains and fine dynamic recrystallized grains at a strain of 0.3.
was observed that the recovery preceded the recrystallization fol- The microstructure was also observed to have a necklace structure,
lowed by the rearrangement of dislocations to form a low energy typical for the dynamic recrystallization, and bulging grain
configuration. A mixture of fine dynamically recrystallized (DRX) boundaries which indicate that new grains nucleate at the grain
grains, small refined lamellar colonies and other particles present boundaries. This implies that the nucleation mechanism is by the
along the grain boundaries were observed at the centre area of the discontinuous dynamic recrystallization (DDRX). The grain
TieAl pancake. On the other hand, the incomplete DRX micro- boundary bulging was attributed to the rapid strain hardening as a
structure with coarse and lamellar colonies was observed in the result of the increase in the dislocation density at the early stages of
microstructure at the edge of the pancake. These observations were hot deformation. At 0.8 strain and the same deforming temperature
attributed to the temperature drop and the inhomogeneous plastic and strain rate (1323K (1049.85  C)/0.05 S-1), the deformed grains
flow (strain variation) during hot forging across positions of the were completely replaced by the fine and equiaxed DRX grains,
TieAl pancake, 1.9 at centre area and 1 at the edge. The micro- however, work hardened recrystallized grains were still present. It
structure showing the grain distribution of three sections of the was also observed that at higher deformation temperatures
TieAl pan cake in the hot forged Tie45Ale7Nb-0.3W alloy is pre- (1473 K) (1199.85  C), constant strain (0.8) and varying strain rates
sented in Fig. 4. the microstructure of the alloy was characterized with larger grain
Zhang et al. [35] studied the deformation behavior of a high Nb size and heterogeneity. The DRX grain size and volume fraction
content containing TieAl based alloy in the a þ g two phase region. decrease with increase strain rate. It was also noted that defor-
Studies have shown that the thermal deformation of the high Nb mation twinning of the g-phase during the hot deformation created
content containing TieAl based alloy (TNB) takes place in the a þ g the nucleation sites for DDRX and promoted the occurrence of DRX
two phase field region. The deformed structure in the TNB alloys is grains for alloys deformed at 1473 K (1199.85  C)/0.001 S-1/0.8.
usually inhomogeneous containing the remnant lamellar structure The studies show that the increase in deformation strain and
which is detrimental to the mechanical properties of the alloy. The temperature favor the recrystallization in TieAl based alloys.
test material (Tie44Ale8Nbe0.2We0.2Be0.1Y alloy) was produced However, the temperature drop and the inhomogeneous plastic
with a Vacuum Arc Remelting furnace and subsequently hot flow across the TieAl based alloy can influence the recrystallization
isostatic pressed at 1300  C/130 MPa for 3 h under argon atmo- kinetics. Also the difference in stacking fault energies between the
sphere. The thermo-physical simulation was carried out using the g and the a2 phase which constitutes the microstructure of the
Gleeble 1500D at temperatures 1225  C and 1275  C to 70% total alloys can influence the recrystallization kinetics if deformed in the
reduction at a strain rate of 0.05 S-1. A common tube-type heat- two-phase region. The g phase which has a lower stacking fault
treatment furnace was adopted to assess the high-temperature energy than a2 phase, is favoured to undergo dynamic recrystalli-
phase composition through water quenching. It was observed zation while the a2 phase with relatively higher stacking fault en-
that the as-cast and heat treated microstructures had near lamellar ergy, dynamic recovery.
structure - consisting of g phase and a2 phase. The deformed
structure is observed to possess blended lamellar and fine recrys- 4.3. Recrystallization mechanisms in Mg based alloys
tallized grains at the investigated temperatures (1225 and 1275  C).
However, at higher temperatures the volume fraction of the a2 Mg alloys are becoming the most preferred light weight alloy for
phase increased along with the coarsening of a2 laths. On the other several structural and commercial applications because of their low
hand, g laths break down to form recrystallized grains at the density, good castability, high specific strength and good damping
deformation temperatures and do not require high local strain for properties [85,86]. However, the major hindrance to the wide-
the dynamic recrystallization to occur. This is because the stacking spread utilization of Mg alloys for engineering is the limited plastic
 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33 27

Fig. 4. Microstructures of the as-forged Tie45Ale7Nbe0.3W alloy: (a) effective strain distributions along the radius direction simulated by DEFORM-3D software, (b) near the edge
of the forged pancake, (c) at the midpoint of the radius, and (d) in the central area (Curled from Li et al. [84] with permission from Elsevier).

formability of these alloys at room temperature. This is attributed structure of dynamically recrystallized grains around the initial
to their HCP crystal structure and low stacking fault energy [85]. grain boundaries. However, these observations were subject to
Over the years, research efforts have been channeled into changing strains and temperatures. The size of the recrystallized
improving the formability of Mg alloys by grain refinement through grain was observed to increase with the increasing temperature,
alloying and thermomechanical processing. Recrystallization pro- while the volume fraction of the recrystallized grains decreased
cesses have been established to play a key role in microstructural under the same temperature condition. The increase in strain rate
changes during thermomechanical processing (TMP) of Mg alloys. was also observed to correlate with the increase in the volume
Grain refinement and improvement in mechanical properties dur- fraction of recrystallized grains. The presence of unclear wavy
ing TMP of Mg alloys are often attributed to dynamic recrystalli- boundaries and near-bulging boundaries which create new
zation because of their low stacking fault energy. Currently, studies recrystallized grains along these boundaries indicates a discontin-
are still ongoing to understand the recrystallization mechanisms of uous dynamic recrystallization as the primary mechanism of
Mg alloys with a view to tailor the microstructure for improved recrystallization. This mechanism is also evident in the dependence
engineering properties. of DRX on the strain intensity, since larger strains would result in
Ebrahimi et al. [87] investigated the flow behavior and the increased grain boundary distortion (bulging) giving room for a
microstructural evolution of an AZ91 alloy subjected to thermo- larger fraction of new recrystallized grains. Fig. 5 shows the neck-
mechanical testing. The test alloy was homogenized at 420  C for lace structure which is an evidence of the dynamic recrystallization
24 h and water quenched. Subsequently, compression test speci- in the AZ91 Mg alloy.
mens were machined with a height to diameter ratio of 1.5. The hot Xu et al. [21] studied the deformation behavior and dynamic
compression test was carried out at temperatures ranging between recrystallization of the AZ61 Mg alloy. Dynamic recrystallization
350 and 420  C at a strain rate of 0.1 S-1 under strains of 0.3 and 0.5. during hot deformation has been reported to play a key role in
The deformed specimens were water quenched for less than 5 s to the improvement of the grain structure and mechanical prop-
preserve the deformed microstructure. It was observed that all the erties of Mg alloys. This study was therefore embarked on to
test specimens had microstructures that showed a necklace grain study the effect of different strain rates and temperatures on the
28 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

10 S
1 strain rate, indicating that the dynamic recrystallization

commences at higher temperatures in this alloy. Also, substructures
formed in the alloys during hot deformation were used to quantify
the stored energy for deformation in the alloys. It was established
that at high strain rates MgeGd had higher stored energy while
AZ31 alloy had higher stored energy at lower strain rates. This in-
dicates that the dynamic recrystallization is enhanced in Mg alloys
with RE additions when subjected to high strain rates.
Biswas et al. [89] studied the property enhancement attainable
for pure Mg subjected to room temperature equal channel angular
extrusion (ECAE). The pure Mg was hot rolled to a thickness of
5 mm, then processed with an ECAE die of 90 inter-channel angle.
The processing was done at a speed of 1 mm S
1, and at a tem-
perature of 250  C for the first 4 passes. The processing temperature
was, however, reduced for subsequent passes (200  C for the 5th
pass, 150  C for the 6th pass, 100  C for the 7th pass and 25  C for
the 8th pass). It was observed that the microstructure of the Mg
processed at 250  C had equiaxed grains with serrated grain
Fig. 5. Necklace structure obtained after hot deformation of AZ91 Mg alloy at 325  C at boundaries depicting the occurrence of dynamic recrystallization.
peak strain (Curled from Ebrahimi et al. [87] with permission from Elsevier). This observation was associated with the migration of low angle
boundaries into high angle boundaries in the prismatic and pyra-
midal planes consistent with the continuous dynamic recrystalli-
microstructural behavior of AZ61 alloys. The test material (AZ61) zation (CDRX). However, the new grains on the basal plane were
with cylindrical compression specimens was subjected to a test associated with the nucleation on prior deformed grains which
on a Gleeble-1500 thermo-mechanical simulator. The test was indicates the transformation from CDRX to the discontinuous dy-
conducted within a temperature range of 220 and 380  C at namic recrystallization (DDRX) in this plane. At lower processing
intervals of 40  C and strain rate of 0.001e1 s
1. All test speci- temperatures (less than 250  C), a mixture of equiaxed and elon-
mens were quenched in water after thermomechanical testing. gated grains were observed in the microstructure indicating a
The microstructural variability of the studied alloy at 380  C/ partial dynamic recrystallization. This is attributed to the occur-
0.01 s
1 under various strains was observed using optical mi- rence of the recovery alongside the recrystallization during defor-
croscopy. It was reported that small amount of dynamic mation at these temperatures. Recovery associated with strain
recrystallized (DRX) grains appear near the initial grain bound- softening was mostly observed in the prismatic and pyramidal
aries at 0.1 strain, but as the strain increases to 0.22, a mixture planes as the processing temperature reduced. The fraction of
of fine DRX and coarse grains form a necklace around the initial recrystallized grains and the recovery reduced with the decreasing
grain boundaries. At 0.5 strain the coarse grains were almost processing temperatures in the basal plane.
completely replaced with fine recrystallized grains. Further in- The studies show that Mg alloys though possessing HCP struc-
crease in strain (0.9) eliminated all coarse grains previously ture and limited slip systems, can be grain refined because of its low
present and resulted in the creation of wavy boundaries in the stacking fault energy and capacity to undergo dynamic recrystal-
microstructure. It was also established from the studies that lization. However, the dynamic recrystallization mechanism could
high temperatures and low strain rates favored full evolution of depend on the plane of deformation e deformation along the basal
the DRX homogenous structure in the alloy. plane would likely yield DDRX compared to when deformation is
Stanford et al. [88] studied the effect of rare earth (RE) elements along the prismatic and pyramidal planes where CDRX is a greater
on the hot deformation behavior of two Mg based alloys. RE ele- likelihood. The size of the recrystallized grains generally increases
ments are known to improve the mechanical properties of Mg al- with the increasing temperature, while the volume fraction of
loys by causing changes in the texture and enhancing slip in this recrystallized grains increase with the strain rate. Also, RE additions
alloy system. Despite the recorded success of incorporating RE into depending on particular strain rates, can affect the temperatures at
Mg alloy systems, there have been little reported on the effect of RE which the dynamic recrystallization occurs in Mg alloys.
elements on the hot deformation characteristics of Mg alloys. The
study was carried out using two Mg alloys (AZ31 and Mg-1.5Gd) 4.4. Recrystallization mechanisms in high entropy alloys
with the similar static recrystallization kinetics. Test samples
from the alloys were machined and the test was carried out at High entropy alloys (HEAs) are metallic systems which have
different temperatures and strain rates in the plane strain more than one principal element in the alloy mixture giving them
compression condition using a Gleeble-3500 thermo-mechanical more significant entropies of mixing resulting in superior engi-
simulator. Microstructures of test samples from the two alloys neering properties compared to conventional alloys [90]. These
subjected to the same testing conditions (400  C and 0.001 S-1, alloys solidify as simple solid solutions with single phases despite
0.1 S-1, 10 S
1) were observed to have fractions of hot deformed the presence of multiple elements attributed to the overwhelming
grains surrounded by necklace structures associated with dynamic effect of entropies of mixing of the principal elements to the
recrystallization. The only exception was the MgeGd sample sub- enthalpy of the compound formation [23,91]. These properties have
jected to the lowest strain rate which had a large fraction of made high entropy alloys ((HEAs) of great interest to material sci-
dynamically recrystallized grains with well-defined sub-bound- entists for use in advance coatings, solder and brazing fillers,
aries. However, at a lower deformation temperature (300  C) and electronics and other specialized high and low temperature appli-
same strain rate of 0.1 S-1, there were no recrystallized grains in the cations [92]. Currently, studies are ongoing to understand the
MgeGd alloy while the AZ31 alloy showed a necklace of DRX mechanical behavior of the HEAs and related phase transformation
structure at grain boundaries. Extremly fine DRX grains were phenomena in these alloys with a view to enhance its applicability
observed in the MgeGd alloy after a deformation at 400  C and in service.
 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33 29

Sathiaraj et al. [93] studied the effect of heavy cryorolling on in the matrix due to the atomic size differences. This severe
the evolution of the microstructure and texture during annealing lattice distortion energy reduces the driving force for the
of equiatomic CoCrFeMnNi high entropy alloy. The high entropy nucleation and growth of new grains in the deformed matrix. The
equiatomic as-cast alloy was homogenized at 1100  C for 6 h to sluggish diffusion of atoms as a result of the whole solute matrix
enhance the chemical homogeneity. Samples from the homoge- also reduces the grain boundary migration rate since the effective
nized alloy were cold rolled to a 50% reduction to get a wrought migration of boundaries depends on the effective diffusion of
microstructure and subsequently full annealed at 800  C for 1 h in atom in the matrix and the effective jumping of boundaries [94].
a salt bath furnace. After that they were subjected to both cold and The whole solute matrix also results in a low stacking fault en-
cryorolling to a total of 90% reduction in thickness in about 10e11 ergy (SFE) of HEAs which promotes the deformation of twins
passes. The cold-rolled and cryorolled samples were isochronally during cold working and increases the nucleation sites for new
annealed for 1 h in the temperature range between 700 and grains during annealing.
1200  C. Fully recrystallized state was observed in cold-rolled and High temperature deformation behavior and dynamic recrys-
cryorolled annealed samples at 700  C and discernible grain tallization of CoCrFeMnNi HEA were similarly studied by Stepanov
growth was observed in both samples at higher annealing tem- et al. [97]. The test material was subjected to an uniaxial
peratures (1000 and 1200  C). It was also observed that the cry- compression test to 75% height reduction (z 1.4 true strain) in the
orolled samples had a lower average grain size (1.3 mm) compared temperature interval 600e1100  C In the study the discontinuous
to the cold-rolled samples (1.6 mm) after annealing at 700  C; and dynamic recrystallization (dDRX) was observed to be associated
the absolute difference in the average grain size of both samples with the microstructural evolution in the CoCrFeMnNi HEA for all
increased with the increase in the annealing temperature. The deformation temperatures and was noted to agree well with the
finer microstructure of the cryorolled sample is attributed to the low SFE of the alloy. At temperatures above 800  C dDRX was linked
retention of the high dislocation density and nano-twins forma- to intensive bulging of initial grain boundaries and the nucleation
tion during cryorolling of the high entropy alloy. This is because of new grains along the initial grain boundaries which gradually
the significantly fragmented structure and the twin boundaries consume the old deformed grains. The dDRX at temperatures
associated with the nano-twins formation in the cryorolled sam- below 800  C was associated with the shear band formation and
ple act as potential nucleation sites for recrystallization in the the intensity of shear deformation decreased along with volume
alloy. Sluggish diffusion was also reported to be responsible for fraction of material undergoing the shear straining as the defor-
minor changes in the microstructure of the cold rolled and cry- mation temperature decreased.
orolled alloy samples at lower annealing temperatures. Discon- Guo et al. [98] studied the hot deformation characteristics of a
tinuous recrystallization was concluded to be the primary refractory HEA (MoNbHfZrTi) using isothermal compression tests
mechanism for the recrystallization in the cryorolled high entropy with varying strain rates in the temperature range of 800e1200  C.
alloy after annealing since the new fine recrystallized micro- MoNbHfZrTi HEA have low density, low cost and structural ability at
structure was formed by the nucleation and growth. high temperatures, which are the major attractions for materials
Tsai et al. [94] studied the deformation and annealing behavior suitable for high temperature applications. A study of this nature is,
of a ductile Al0.5CoCrCuFeNi HEA subjected to hot forging and cold hence, essential for understanding the deformation behavior of the
rolling. They observed that the deformed (50% cold rolled) refractory HEA at high temperatures. It was observed from the study
Al0.5CoCrCuFeNi was softened after annealing at 900  C for five (5) that the microstructural evolution in the MoNbHfZrTi was depen-
hours and this was attributed to the recovery and the recrystalli- dent on both the strain rate and the deformation temperatures. Low
zation. However, the recrystallization time in the HEA was longer strain rates and high deformation temperatures were observed to
than in traditional alloys and the recrystallization temperatures favor the dynamic recrystallization of the grains in the alloy. This is
exceeded estimates of empirical formula used for traditional alloys, because these conditions promote the decrease in the critical dislo-
indicative of the high recrystallization resistance of the Al0.5CoCr- cation density and consequently the critical strain for DRX in the
CuFeNi HEA. The resistance of the HEA studied to the recrystalli- alloy. Also low strain rates and high deformation temperatures can
zation was attributed to the low twin boundary energy which provide time and energy for the grain boundary migration, which
reduces the driving force of the recrystallization, and sluggish aids the occurrence of DRX. The DRX which occurred during the
diffusion which makes the grain boundary migration slow and the microstructure evolution of MoNbHfZrTi HEA after the hot defor-
movement of dislocation difficult. mation was observed to be discontinuous (DDRX) and continuous
Bhattacharjee et al. [95] investigated the effect of annealing on (CDRX). At 800  C, extensive bulging grain boundaries with high
the microstructure and texture evolution of severely deformed angles which are closely related to strain induced grain boundary
CoCrFeMnNi HEA in the temperature range of 650e1000  C. The orientation was observed, indicative of the DDRX nucleation mech-
test alloy after production was subjected to the homogenization anism. Also, numerous subgrain boundaries with low angle ones,
treatment at 1100  C for 6 h. The homogenized samples were were observed at the same temperature (800  C) as typical features
cold rolled to 50% reduction in thickness and subsequently of CDRX. However, the mechanism of CDRX reduced with the
annealed. The annealed samples were afterwards cold rolled to increasing deformation temperatures (between 100 and 1200  C)
90% reduction in thickness at room temperature. It was observed and the decreasing strain rates and this was evident in the acceler-
from the study that the test material subjected to 90% cold rolling ated transformation of low angle grain boundaries to high angle
had averagely recrystallized grains when annealed at 650  C, and ones.
the degree of recrystallization increased with the increasing It can be summed up from the works on HEAs that low strain
annealing temperature. Discontinuous recrystallization was rates and high deformation temperatures favor the dynamic
observed for the HEAs studied, and the microstructures were recrystallization. However, the recrystallization kinetics in HEAs is
completely recrystallized at higher annealing temperatures and generally slower than in the traditional alloys. This is noted to be
had shown strong resistance to the grain growth which is in largely due to either the low twin boundary energy observed in the
agreement with observations from other low SFE materials [96]. deformed HEAs, which reduces the driving force for the recrystal-
The observations made are attributed to the high lattice distor- lization or/and the sluggish diffusion of the whole solute matrix of
tion energy inherent in the whole solute matrix of HEAs which is HEAs, which generally makes the grain boundary migration slow
a result of the individual strain energy possessed by every atom and the movement of dislocations difficult.
30 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33

4.5. Recrystallization mechanisms in shape memory alloys recrystallization. The mean grain size increases with the increase in
the deformation temperature at a given strain rate, while it de-
Shape memory alloys (SMAs) are metallic materials which have creases with the increase in the strain rate at a given temperature.
the ability to recover their dimensional integrity after being deformed Basu et al. [104] studied the effect of the dynamic recrystalli-
to certain strain levels when subjected to temperatures [99,100]. zation in the austenite e martensite phase transformation in Ni eTi
These alloys have two important characteristics which qualify their e Fe shape memory alloys subjected to hot working. The studied
suitability for both engineering and commercial applications, namely alloy was homogenized at 1000  C for 12 h and then furnace cooled.
the shape memory effect (temperature sensitivity) and the pseu- Hot compression tests were subsequently conducted on the alloy
doelasticity (stress sensitivity) [101]. Several alloys have displayed the samples which were deformed to approximately 50% reductions at
key characteristics aforementioned in addition to inherent engi- temperatures 750, 850 and 950  C; and strain rates of 10 and
neering properties, but NiTi, Cu based and Fe based alloys have been 100 S
1. The deformed samples were quenched immediately after
the key alloys of interest in these fields due to their approachable the test. It was observed that the strain localization was dominant
levels of strain recoveries [102,103]. These alloys are presently used in in the alloys deformed at lower temperatures, while serrations of
fire safety alarms, pipe coupling, biomedical (stents and surgical in- grain boundaries and relatively fine, nearly equiaxed grains were
struments) and other domestic applications [100]. Recently, a lot of observed in alloys deformed at higher temperatures. The nearly
research has been focused on achieving nanostructured SMAs to meet equiaxed grains were present surrounded by the high angle grain
certain requirements for advanced applications. Therefore, studies boundaries with large orientation spread and also grain mis-
focussing on the effect of thermomechanical processing on the orientations compared to the other recrystallized grains. It was also
microstructure and properties of SMAs are of significant importance observed that the size and fraction of dynamic recrystallized grains
to the present day material scientists. increased with the increase in the strain rate and working tem-
Jiang et al. [103] investigated the dynamic recovery and dynamic perature. This was evident from the decrease in dislocation den-
recrystallization of NiTi SMA subjected to hot compression defor- sities in the alloy as working temperature increased. The dynamic
mation. A NiTi bar of the study material was solution treated at recrystallization was, however noted to suppress the austenite to
850  C for 2 h and then quenched in ice. Samples were then cut for the martensite phase transformation in NieTieFe SMAs.
the hot compressive tests at different working temperatures Yin et al. [105] studied the mechanism of the continuous dy-
(600e1000  C) and strain rates (0.001 S-1 and 1 S
1). It was namic recrystallization in a 50Tie47Nie3Fe SMA during hot
observed that the samples deformed at 600  C was characterized compressive deformation. Samples were cut from a hot forged
with a combination of dynamic recovery and dynamic recrystalli- TiNiFe rod for the hot compression tests. The samples were pro-
zation, the dynamic recovery was, however, dominantly evident cessed to 50% overall height reductions at different temperatures
from the presence of high fractions of elongated grains. At 700  C between 750 and 1050  C and strain rates between 0.01 S-1e10 S
1
working temperature, almost complete dynamic recrystallization using a Gleeble 3500 thermo mechanical simulator. It was observed
was observed in the microstructure of the NiTi samples at low that the recrystallized grain region is located between the
strain rates (0.001 S-1 and 0.01 S-1) while dynamic recovery was deformed grain boundaries of deformed grains surrounded with
prevalent at higher strain rates (0. 1 S
1 and 1 S
1). Above 700  C, low angle grain boundaries created from the compression at low
the microstructures of the NiTi samples were characterized with working temperatures and high strain rates. The point to the
the complete dynamic recrystallization. The authors have con- original misorientation in the deformed metals was over 15 and
lcuded that the low strain rates and high working temperatures, the typical boundary rotating angle values corresponded to the
both favor the recrystallization because these conditions provide high angle grain boundaries. Point to point misorientations indic-
time for the accumulation of the energy and facilitate the higher ative of low angle grain boundaries were also observed around the
interface migration for the nucleation and growth of new grains vicinity of the grain boundary. These observations were the de-
and thus, for the dislocation annihilation. Low strain rates and lineates of the gradual transition of low angle grain boundaries to
higher working temperatures also favor the formation of fine high angle grain boundaries during deformation of the samples
equiaxed grains in hot deformed NiTi SMA. indicating the continuous dynamic recrystallization mechanism in
Zhang et al. [24] reported on the simulation of the dynamic the SMAs studied. It was concluded from the study that the DRX
recrystallization in NiTi SMA subjected to hot compression. A NiTi process benefits from the decrease in the strain rate and higher
bar was heated to 850  C and held for 2 h, before being quenched temperatures as these conditions allow greater time for the
into ice water. The NiTi samples were then cut from the solution- movement of the boundaries and dislocations.
treated NiTi bar for the compression tests. The compression ex- Zhang et al. [106] studied the effect of local canning compression
periments were carried out at strain rates ranging from 0.001 to on the dynamic recrystallization behavior of the NiTi SMA. The
1 s-1 and temperatures ranging from 800 to 1000 oC. The samples study was aimed at investigating the effect of three dimensional
were compressed to a total deformation degree of 70% at the true compression stresses from local canning on the dynamic recrys-
strain of 1.2, while one NiTi sample was compressed to a defor- tallization of NiTi SMA. A NiTi SMA bar was used as the starting
mation degree of 40%, where the true strain was 0.5. All the samples material and test samples were obtained by electro-discharge
were quenched into ice water immediately after the compression to machining from the bar. The samples were locally canned using
retain the deformed microstructure. A cellular automation model low carbon steel cans of known dimensions. The cans were sub-
was used to simulate and predict the microstructural evolution, the sequently subjected to hot compression testing at a fixed strain rate
dislocation density evolution, the flow stress and the grain size of 0.05 S-1 and varying temperatures of 600, 700 and 800  C. The
during the DRX of the NiTi alloy. It was deduced from the study that canned NiTi samples were subjected to a total of 75% reduction in
dislocation density propels nucleation of new recrystallized grains height, and thereafter quenched in water at room temperature. The
at pre-existing grain boundaries in the initial microstructure. The authors reported the presence of low angle grain boundaries and
mean dislocation density was observed to be dependent on the changes in texture in the compressed NiTi samples. It was observed
strain rate and the deformation temperature, as it decreases at high that the fraction of recrystallized grains, sub boundaries and
deformation temperatures and low strain rates. These processing deformed structure varied with different treatment temperatures.
conditions (high deformation temperatures and low strain rates) Dynamic recovery and dynamic recrystallization were the domi-
also have an influence on the mean grain size during the dynamic nant softening mechanisms during local canning at lower working
 K.K. Alaneme, E.A. Okotete / Journal of Science: Advanced Materials and Devices 4 (2019) 19e33 31

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