Materials Characterization 127 (2017) 296–310

Contents lists available at ScienceDirect

Materials Characterization

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

Microstructural and textural characterization of Zircaloy-4 processed by

rolling at different temperatures

Devasri Fuloria a, Nikhil Kumar a, R. Jayaganthan a,b,⁎, S.K. Jha c, D. Srivastava d

a
Department of Metallurgical and Materials Engineering, Centre of Nanotechnology, IIT Roorkee, Roorkee 247667, India
b
Department of Engineering Design, Indian Institute of Technology Madras, Chennai 600036, India
c
Nuclear Fuel Complex Limited, Hyderabad 501301, India
d
Materials Science Division, Bhabha Atomic Research Centre, Mumbai 40085, India

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

Article history: In the present work, the effect of rolling at room (298 K) and cryogenic temperatures (77 K) on the microstructural
Received 24 September 2016 and textural evolution of the as-received Zircaloy-4 bar along the planes parallel to the extrusion direction (ND - ED)
Accepted 19 February 2017 and in the transverse direction (ND - TD) has been investigated. The as-received Zircaloy-4 was subjected to various
Available online 24 February 2017
rolling reductions of 25%, 50%, 70% and 90% which is corresponding to true strains of 0.29, 0.69, 1.2, and 2.3, respec-
tively. A detailed analysis of microstructures and textures of the deformed alloy has been carried out through the
Keywords:
Zircaloy-4
electron backscattered diffraction (EBSD) and the XRD texture. Microstructures and textures of the samples rolled
Electron backscattered diffraction along the extrusion direction (ND - ED) at lower strains showed a few extension twinning (f1012g h1011i) along
Bulk texture with ba N prismatic slip at room temperature, and a combination of extension twinning, ba N prismatic, bc + a N
Room temperature pyramidal, and basal slips at cryogenic temperature. While along the transverse direction (ND - TD), at lower strains,
Cryogenic temperature extension twinning exhibited a dominant role at both the temperatures. This was eventually changed to slip
dominant activity (ba N prismatic, bc + a N pyramidal and basal) from medium to high strains along both the
directions (extrusion & transverse) at both the temperatures (RT & CT).
© 2017 Published by Elsevier Inc.

1. Introduction Another area favouring the microstructural engineering by grain re-

finement in bulk alloys to grain sizes in the ultrafine grain (UFG) regime
Zirconium and its alloys are extensively used in the fabrication of in (100–1000 nm) and/or in the nanograin regime (below 100 nm) is a
core structural components of nuclear reactors owing to their excellent promising method for achieving enhanced mechanical properties as
high temperature creep and corrosion resistance, low cross section for per the Hall-Petch relationship [6]. The numerous severe plastic defor-
neutron absorption and good mechanical properties [1–3]. The fuel mation (SPD) techniques well-known for the production of UFG mate-
cladding for channel boxes in boiling water reactors (BWRs), and inter- rials are high pressure torsion (HPT), twist extrusion (TE), multi
mediate grid applications in pressurized water reactors (PWRs) are directional forging (MDF), equal channel angular pressing (ECAP), accu-
made up of Zircaloy-4. As the Zircaloy cladding experiences the extreme mulative roll bonding (ARB), cyclic extrusion and compression (CEC),
temperature conditions imposed by the radioactive fuel and the exterior repetitive corrugation and straightening (RCS) etc. [7,8]. While these
coolants, therefore, in order to ensure the reliability of cladding tube techniques have been widely used to fabricate thermally stable ultra-
under the hostile environment reactor conditions, its structural integri- fine/nanostructured grain morphology with enhanced mechanical
ty is of great concern [4]. Following this, continuous efforts are being properties [8], the demerits of these techniques are associated with
made towards the enhancement of mechanical properties of Zircaloy- the requirement of expensive and complicated die design and low pro-
4. The different processing routes including: pilgering, extrusion and ductivity [9]. Therefore, besides SPD techniques, rolling at lower tem-
forging have been utilized over the years to manufacture components peratures has also developed as a possible route for engineering
with improved in-reactor performance [5]. material in the UFG or nanograin regime [10] by the suppression of dy-
namic recovery [11] which leads to the multiplication of high density
defects in the matrix of the deformed materials, thus, enhancing the
⁎ Corresponding author at: Department of Metallurgical and Materials Engineering,
mechanical properties. The deformation via rolling at lower tempera-
Centre of Nanotechnology, IIT Roorkee, Roorkee 247667, India. tures for various alloys such as Ti, Cu and Al have been studied exten-
E-mail address: [email protected] (R. Jayaganthan). sively [10–12]. Additionally, in the recent years, several authors/

http://dx.doi.org/10.1016/j.matchar.2017.02.020
1044-5803/© 2017 Published by Elsevier Inc.
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 297

researchers have also studied the effect of cryorolling on the microstruc- are corresponding to true strains of 0.29, 0.69, 1.2, and 2.3, respectively.
tural evolution and mechanical properties of Zirconium alloys as a result Initially, the samples for cryorolling were dipped in liquid nitrogen for
of effective grain refinement [4,13–19]. about 15 mins and then rolled by giving a reduction of 0.2 mm per pass
The Zr alloy components namely cladding tubes and grids in light till the desired reductions were achieved in subsequent passes. Further,
water reactors and channels in boiling water reactors in the form of the samples for cryorolling and room temperature rolling were quenched
tubes or plates/sheets are commonly fabricated by the rolling process. in liquid nitrogen and water respectively, for about 5–10 min after every
Further, the stress–strain condition in tube reduction processes having pass in order to attain thermal equilibrium with liquid nitrogen and
thickness to diameter ratio higher than one, generally employed in the water. To prevent heat losses due to friction, MoSi2 was used for lubricat-
fabrication of Zircaloy cladding [20] is same as that in plate/sheet rolling ing the rolls. The rolled samples were designated as RTR and CR for room
processes of Zircaloy. Therefore, the typical evolved texture is bimodal and cryogenic temperature deformation, respectively.
basal texture in both the processes [21]. Texture development in Zircaloy The microstructures of the alloy deformed up to various percentages
is imperative for two reasons, first, the texture evolved at any strain step of reduction were examined by electron back scattered diffraction
will affect the ease of succeeding strain increment, and second, the final (EBSD) on a field emission gun scanning electron microscope FEI
texture developed in the finished products will substantially affect their Quanta 200 FEG-SEM/EBSD. The samples for EBSD were prepared by
in-service performance as the properties such as yield strength, creep electropolishing in a solution of 20 ml perchloric acid in 80 ml methanol.
strength, fatigue and stress corrosion cracking are strongly dependent A step size of 0.1 μm was used for all the deformed samples. TSL-OIM
on texture [2,22]. In order to have an exhaustive understanding on the software was used for data acquisition and analysis. Bulk texture mea-
texture development of Zircaloy, a thorough knowledge on the operable surements were carried out on a PANalytical™ X'Pert PRO MRD system
deformation systems and deformation mechanisms are required. instrument using Cu Kα radiation for RTR and CR samples. Standard
Various twinning and slip systems are the operable deformation Schulz method in reflection mode [31] was used for pole figure mea-
modes in this alloy [20]. Slip and twinning are a non-elastic deformation surements. Four in complete pole figures, namely (0002), (1010),
processes that governs the plastic anisotropic response of zirconium al- (1011), (1012) were measured. The orientation distribution functions
loys. However, twinning unlike slip, reorient the lattice, thereby leading (ODFs) were calculated from the experimental pole figures using the
to a notable influence on the flow stress and strain hardening rate of a MTEX-4.3.1 module in MATLAB R2015b by imposing an orthorhombic
material either by providing “softer” orientation, such as f1122gh1123i sample symmetry.
contraction twin, or a “harder” orientation, such as f1012gh1011i
3. Results
extension twin [23,24]. Among the various slip systems available

in Zircaloy, the 〈a〉 prismatic slip f1010gh1210i) is reported as the 3.1. Microstructure and Bulk Texture of the As-received Alloy
easiest mode which is generally operative at all ranges of temperatures,
while, the other slip systems such as the 〈a〉 basal slip ðð0002Þh1120iÞ The as-received Zircaloy-4 in the hot extruded and annealed state
and the 〈c + a〉 pyramidal slip ðf1011gh1123iÞ are effective at and exhibited two different textures along the planes parallel to the extru-
above room temperature [25] and these slip systems if activated easily sion and transverse directions which are designated as ND - ED and
would provide five independent slip systems that may result in a homoge- ND - TD. The grains along the extrusion direction were dominant in
neous strain [26]. But due to the insufficient number of slip systems below basal 〈0001〉 orientations, while the grains in the transverse direction
and at room temperature, these alloys are highly sensitive to twinning, showed non-basal (h1010i and h2110i) orientations mostly as reported
particularly below room temperature. The different twinning modes in earlier works [32,33].
observed in these alloys are extension twins of the type f1012gh1011i The various texture components generally observed in HCP metals
[34,38,46] are represented in Fig. 1. Bulk texture measured by XRD for
and f1121gh1126i , and contraction twins of the type f1122gh1123i
as-received Zircaloy-4 sheet is shown in Fig. 2(a–d). Fig. 2(a) represents
and f1011gh1012i [27,28]. During loading, extension twinning occurs
the texture along the extrusion direction. The (0002) pole figure showed
when the ‘c’ axis is elongated, while contraction twinning occurs when
a weak basal pole intensity near ND with some spread of 15°–20°
the ‘c’ axis is contracted [29], and the activation of a slip mode or a twin
along the ND - TD and ND - RD planes. While along the transverse direc-
mode depends on the critical resolved shear stress value (CRSS). Further,
tion, the ð1010Þ pole figure showed a very strong intensity of h1010i
the instantaneous CRSS depends upon the applied strain, strain rate, tem-
directions aligned with the ND in a way such that all the basal planes
perature, level of purity and grain size, and the CRSS for slip is extremely
normal 〈0001〉 are perpendicular to the extrusion axis (Fig. 2(c)).
sensitive to temperature, while for twinning, it is independent of temper-
This texture is known as cylindrical texture which is generally found in
ature [30]. Therefore, it is important to study the deformation mechanisms
extruded hexagonal materials [34]. Further, the quantitative estimation
operating at low temperatures in case of such a highly textured Zircaloy. In
of texture evolution was carried out by calculating the complete ODFs
the present work, a comprehensive study on microstructural and textural
for each condition using the measured incomplete pole figures. The
evolution following rolling up to various percentages of reductions along
ODF sections corresponding to φ2 = 0° and 30° along the extrusion di-
the extrusion (ND – ED) and transverse directions (ND – TD) of as-re-
rection (Fig. 2(b)) showed an overall weak texture intensity with
ceived bar of Zircaloy-4 at room (RT) and cryogenic (CT) temperatures
some commonly observed components such as A f0001gh1010i at
is presented. The various deformation modes affecting the microstructural
{φ1 = 0°, φ = 0°, φ2 = 0°}, C f1120gh1010i at {φ1 = 0°, φ = 90°,
and textural evolution in samples rolled along the extrusion and trans-
φ2 = 0°}, f1120gh0001i at {φ1 = 90°, φ = 90°, φ2 = 0°}, and f1010gh0
verse directions at both the temperatures are investigated using electron
001i at {φ1 = 90°, φ = 90°, φ2 = 30°} (as represented in Fig. 1), and
backscattered diffraction (EBSD) and bulk texture techniques.
some other texture intensities of f1215gh1010i at {φ1 = 0°, φ =
32°, φ2 = 0°}, f1212gh1010i at {φ1 = 0°, φ = 55°, φ2 = 0°}, and f0112g
2. Experimental h4221i at fφ1 ¼ 10°, φ = 47 ° , φ2 = 30 ° }. While the transverse direc-
tion (Fig. 2(d)) exhibited the dominant presence of f1010g fiber
The as-received Zircaloy-4 having chemical composition (wt%) (1.5 texture.
Sn, 0.2 Fe, 0.2 Cr and balance Zr) was procured from Nuclear Fuel
Complex, Hyderabad, INDIA, in the hot extruded and annealed state. 3.2. Microstructure Evolution of the Deformed Zircaloy-4
Sheets having 30 mm × 33 mm cross-section and 3 mm thickness
were rolled at room temperature (298 K) and cryogenic temperature A detailed analysis of the microstructural evolution is carried out
(77 K) for different reductions, namely 25%, 50%, 70% and 90% which through EBSD. The inverse pole figure (IPF) maps of Zircaloy-4
298 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Fig. 1. The standard texture components for HCP metals [34,38,46].

deformed up to various percentages of reductions (25%, 50%, 70% and characterized by a misorientations 85.22° about the h1120i axis [35]
90%) along the extrusion and transverse directions at room and were identified as the primary twins formed as a result of rolling at
cryogenic temperatures are shown in Figs. 3–6. The microstructural both the temperatures (298 K and 77 K) along both the directions
evolution up to 50% reduction along the extrusion direction was hetero- (extrusion and transverse) at lower strains.
geneous, containing some elongated and small sized grains at both At higher reductions, namely from 70% to 90%, the microstructures
room and cryogenic temperatures as shown in Fig. 3(a, b) and Fig. 5(a, along both the directions (extrusion & transverse) were highly
b). The elongated grains were of mainly basal orientations while small deformed and were marked with significant grain refinement at both
sized grains had non–basal orientations. Further, we observed few de- the temperatures (Figs. 3(c, d)–6(c, d)). Further, the evolution of frac-
formation twins which were formed locally in grains with non–basal tion of low angle grain boundaries (LAGBs) and high angle grain bound-
orientations up to 50% reduction (marked with white color). The micro- aries (HAGBs) for the samples deformed at both the temperatures along
structures along the transverse direction showed deformation twinning the extrusion and transverse directions is shown in Fig. 7(a, b), and the
up to 70% and 50% reductions at room and cryogenic temperatures, re- corresponding values are listed in Table 1 and Table 2. At room temper-
spectively (Fig. 4(a, b) and Fig. 6(a, b). However, the fractions of twin ature, the evolution of fraction of LAGBs and HAGBs were approximately
boundaries evolved were decreased with the increase in reduction. It similar up to 50% rolling reduction along both the directions (extrusion
was observed that the extension twins on the plane f1012g which is & transverse). After 70% reduction along the extrusion direction, a high

Fig. 2. (0002) and ð1010Þ pole figures and orientation distribution function represented as φ2 =0°&φ2 =30°section of as-received Zircaloy-4 along (a, b) ND – ED plane and (c, d) ND – TD
plane.
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 299

Fig. 3. EBSD (IPF) maps of Zircaloy-4 after RTR along ND – ED plane (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction, respectively.

fraction of HAGBs was observed whereas, along the transverse direc- KAM profiles after rolling up to various percentages of reductions
tion, fraction of LAGBs was increased, though it remained less than the (25%, 50%, 70% and 90%) at room and cryogenic temperatures along
fraction of HAGBs evolved. Finally, after 90% reduction, an increase in both the directions are shown in Fig. 8(a–d). It was observed that at
fraction of LAGBs corresponding to extrusion direction, and nearly room temperature, the average KAM values were low (b 1°) up to 25% re-
same fraction of LAGBs from preceding reductions corresponding to duction along the extrusion direction (Fig. 8(a)) and up to 50% reduction
transverse directions were observed (Fig. 7(a)). At cryogenic tempera- along the transverse direction (Fig. 8(b)), while these were high (1°–1.5°)
ture, up to 25% rolling reduction, the fraction of LAGBs and HAGBs from 50%–90% (Fig. 8(a)), and 70%–90% (Fig. 8(b)) reductions along the
evolved in an approximately similar fashion along both the directions extrusion and transverse directions, respectively. At cryogenic tempera-
and showed high fraction of HAGBs. After 50% reduction, the fraction ture, the average KAM values were comparatively higher than that
of LAGBs was increased along the extrusion direction while the fraction observed at room temperature and lie between 1°–1.5° for rolling reduc-
of HAGBs remained high along the transverse direction. Further, from tions from 25%–70%, and 1.5°–2° for 90% reduction along the extrusion
70% - 90% rolling reductions, the evolution of fraction of LAGBs and and transverse directions, respectively (Fig. 8(c, d)). Further, the average
HAGBs along both the directions were approximately same, albeit GAM and GOS values (Fig. 9(a–d) and Fig. 10(a–d)) observed after vari-
with much high fraction of LAGBs after 90% rolling reduction along ous rolling reductions (25%, 50%, 70%, and 90%) were high, with GAM
both the directions (Fig. 7(b)). In order to investigate the in-grain mis- values lying in the range between 0.5°–1.5° at room temperature and
orientations developed during rolling at room and cryogenic tempera- between 1°–2° at cryogenic temperature along both the extrusion
tures along the extrusion and transverse directions, kernel average (Fig. 9(a, c)) and transverse direction (Fig. 9(b, d)), and a GOS value
misorientation (KAM), grain average misorientation (GAM), and grain N3° for all the samples deformed at room and cryogenic temperatures
orientation spread (GOS) were estimated. KAM calculation includes along both the directions (Fig. 10(a–d)). Therefore, the in-grain misorien-
the misorientation between a grain at the center of the kernel and all tation studied through KAM, GAM and GOS showed that with the pro-
points at the perimeter of the kernel with the provision that misorienta- gressive reductions, strain accumulation was high along both the
tions exceeding some tolerance value (N5°) were excluded from the av- directions at room and cryogenic temperatures which is a typical feature
eraging calculation [36]. GAM and GOS on the other hand represents the shown by highly deformed materials. However, the in-grain misorienta-
average misorientation between all neighboring pairs of points in the tion developed at cryogenic temperature was quite high following rolling
grain and average deviation between measurement points in a grain along both the directions which was also substantiated by a higher frac-
and the average grain orientation respectively [37]. The comparative tion of LAGBs evolved after 90% reduction at cryogenic temperature.
300 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Fig. 4. EBSD (IPF) maps of Zircaloy-4 after RTR along ND – TD plane (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction, respectively.

3.3. Bulk Texture of the Deformed Zircaloy-4 50%–70%, the texture was significantly weakened and basal poles were
concentrated at the center with some spread around it in the transverse
Texture studies were performed on the samples of Zircaloy-4 rolled as well as in the rolling directions (Fig. 12(b, c)). Finally, after 90% rolling
at room and cryogenic temperatures along the extrusion and transverse reduction along the transverse direction, the texture evolution was same
directions. The ð0002Þ and ð1010Þ pole figures of Zircaloy-4 rolled up to as observed along the extrusion direction after 90% reduction but with a
various percentages of reductions (25%, 50%, 70%, and 90%) at room higher intensity (Fig. 12(d)).
temperature along the extrusion and transverse directions are shown Further, the ð0002Þ and ð1010Þ pole figures of Zircaloy-4 rolled up to
in Fig. 11(a–d) and Fig. 12(a–d). Along the extrusion direction, after various percentages of reductions (25%, 50%, 70%, and 90%) at cryogenic
25% rolling reduction, two series of weak peaks were observed, one in temperature along the extrusion and transverse directions are shown in
the ND - TD plane and the other in the ND - RD plane. The peak in the Fig. 13(a–d) and Fig. 14(a–d). After 25% rolling reduction along the ex-
ND - TD plane was inherited from the initial texture along the extrusion trusion direction, the (0002) pole figure showed a TD split texture
direction, while the peak in the ND - RD plane was due to the activation which is also known as a T–type texture (Fig. 13(a)). After 50% reduc-
of extension twins of the type f1012gh1011i (Fig. 11(a)). After 50% tion, some instability in texture showing a large spread along the ND -
rolling reduction, same texture pattern with slightly improved basal RD plane was observed (Fig. 13(b)) which regained its stability after
pole intensity was observed (Fig. 11(b)). Further after 70% reduction, 70% reduction, and exhibited a TD split texture (Fig. 13(c)). Finally,
basal pole intensity was increased and the basal poles were mainly con- after 90% reduction, the texture intensity was improved and regained
centrated towards the center (along the ND) with a small split along the the value obtained after 25% reduction with the evolution of two series
ND - RD plane (Fig. 11(c)). Finally, after the highest rolling reduction of of peaks namely a strong peak showing a split along the TD plane while
90%, basal poles were mainly concentrated along the ND with some a lower intensity peak showing a split along the RD plane (Fig. 13(d)).
spread of 15°–20° towards the TD (Fig. 11(d)). The similar texture as ob- Such type of textures for several Zircaloys are reported in the literature
tained after 90% reduction was reported by Gurao et al. [38] after final [39,40]. Further, at cryogenic temperature along the transverse direc-
step pilgering of Zircaloy-4 due to the significant contribution of basal tion after 25% reduction, the texture evolution was same as that ob-
slip along with prismatic and b c + a N pyramidal slip. While rolling served at room temperature for the same amount of deformation,
along the transverse direction with initial h1010i fiber texture (Fig. 2(c, showing a strong intensity of basal poles concentrated towards the ND
d)) after 25% reduction, led to the reorientation of b c N axis of the grains with some spread along the TD (Fig. 14(a)). After 50% deformation,
by 90°, thereby leading to the formation of a strong b0001N basal fiber the process of beginning of splitting of the basal poles was observed
texture as shown in Fig. 12(a). As the reduction was increased from (Fig. 14(b)) which ended after 70% reduction with the evolution of a
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 301

Fig. 5. EBSD (IPF) maps of Zircaloy-4 after CR along ND – ED plane (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction, respectively.

TD split texture showing a significantly reduced intensity (Fig. 14(c)). φ2 ¼0°g, f1210gh3031i at fφ1 ¼ 7:5°, φ=90° , φ2 =0°}, f0112gh2110i
Finally, this TD split texture evolved after 70% reduction was further at fφ1 ¼0°, φ=42° , φ2 =30°} and f0110gh0002i at fφ1 ¼ 90°, φ=90°,
strengthened after 90% reduction (Fig. 14(d)). The ODFs corresponding φ2 =30°} were observed (Fig. 15(d)). While along the transverse direc-
to φ2 equal to 0°and 30° after RTR up to various percentages of reduc- tion, {0001} fiber including both the A and D components remained as
tions (25%, 50%, 70% and 90%) along the extrusion and transverse direc- the dominant component from 25%–90% reduction (Fig. 16(a–d))
tions are shown in Fig. 15(a–d) and Fig. 16(a–d). Along the extrusion along with some other minor components such as f0110gh4221i at
direction after 25% reduction, an overall weak intensity of basal fiber fφ1 ¼ 7:5°, φ = 90 ° , φ2 = 30 ° } andf01110gh1763i at fφ1 ¼ 80°−90 ° ;
with A f0001gh1010i component at {φ1 = 0°, φ = 0 ° , φ2 = 0°} along
φ ¼ 10°; φ2 ¼ 30°g corresponding to 50% reduction (Fig. 16(b)), f0110g
with some other texture components such as f1214gh1010i at fφ1 ¼
h4221i at fφ1 ¼ 7:5°, φ= 90 ° , φ2 =30° } corresponding to 70% reduc-
0°; φ = 40°, φ2 = 0 ° }, f0113gh2110i at {φ1 = 0°, φ = 32 ° , φ2 = 30°},
tion (Fig. 16(c)), and finally f1215gh1010i at fφ1 ¼ 0° , φ = 32 ° ,
f0110gh4221i at fφ1 ¼ 7:5°, φ = 90 ° , φ2 = 30° } and f0110gh2113i at
φ2 =0°}, f1210gh3031i at fφ1 ¼7:5°, φ=90° , φ2 =0°}, f0112gh2110i
fφ1 ¼ 30°, φ = 90 ° , φ2 = 30°} were observed (Fig. 15(a)). From 50%–
at fφ1 ¼ 0° , φ = 42 ° , φ2 = 30°} and f0110gh0002i at fφ1 ¼ 90° ,
70% reductions, basal fiber with A f0001gh1010i at {φ1 = 0°,
φ=90° , φ2 =30°} corresponding to 90% reduction (Fig. 16(d)). Further,
φ=0° , φ2 =0 °} as a major component was further strengthened, and
the ODF sections after CR up to various percentages of reduction along the
D f0001gh1120i at {φ1 = 0°, φ= 0 ° , φ2 = 30 ° } as a minor component extrusion and transverse directions are shown in Fig. 17(a–d) and Fig.
was evolved and strengthened along with the evolution of some other
18(a–d). It was observed that the texture components close to f0117gh1
minor components such as f1215gh1010i at fφ1 ¼ 0° , φ = 32 ° ,
765i at fφ1 ¼ 80°, φ=15° , φ2 = 30°} and f0110gh0002i at fφ1 ¼ 90°,
φ2 =0°}, f0115gh2110i at {φ1 = 0°, φ = 22 ° , φ2 = 30 ° } and f0113g φ = 90 ° , φ2 = 30°} were common and were present from 25% to 90%
h2110i at {φ1 =0°, φ=30° , φ2 =30°} corresponding to 50% reduction rolling reductions (Fig. 17(a–d)). In addition, f1215gh1010iat fφ1 ¼0°,
(Fig. 15(b)), and f121 15gh1010i at fφ1 ¼ 0°, φ=12° , φ2 =0°}, f0119g φ = 32° , φ2 = 0 ° } and f1210gh3031iat fφ1 ¼ 7:5°, φ = 90° , φ2 = 0 ° }
h2110i at {φ1 = 0°, φ = 12 ° , φ2 = 30 ° } and f0115gh2110i at {φ1 = 0°, were observed after 25%, 70% and 90% reductions (Fig. 17(a, c, d)),
φ = 22 ° , φ2 = 30 ° } corresponding to 70% reduction (Fig. 15(c)), and f12112gh2312i at {φ1 = 80°, φ = 15°, φ2 = 0 ° } was observed in
respectively. Finally, after 90% reduction, both A f0001gh1010i and 25% to 70% rolled samples (Fig. 17(a–c)). Further, some other compo-
D f0001gh1120i along with other components close to f121 15gh1010i nents such as f1212gh211203i at fφ1 ¼ 5° , φ = 55 ° , φ2 = 0 ° } after
at fφ1 ¼ 0°; φ ¼ 12°; φ2 ¼ 0°g,f1215gh1010i at fφ1 ¼ 0°; φ¼ 22°−55°; 25% reduction (Fig. 17(a)), and f1214gh1010i at fφ1 ¼ 0°; φ ¼ 40°;
302 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Fig. 6. EBSD (IPF) maps of Zircaloy-4 after CR along ND – TD plane (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction, respectively.

φ2 ¼ 0°g; f1210gh5051i at fφ1 ¼5°; φ¼90°; φ2 ¼0°g;f12112gh111017i components close to f1210gh3031i at fφ1 ¼ 7:5° , φ = 90 ° , φ2 = 0 ° }
at fφ1 ¼ 60°; φ ¼ 15°; φ2 ¼ 0°g; f1120gh0001i at {φ1 = 90°, φ = 90°, and f0110gh0002i at fφ1 ¼ 90°, φ=90° , φ2 =30°} from 25% to 90% re-
φ2 = 0 ° } and f0116gh8914i at fφ1 ¼ 40° , φ = 17 ° , φ2 = 30 ° } after ductions (Fig. 18(a–d)). However, the basal fiber texture intensity was
50% reduction (Fig. 17(b)) were observed. While along the transverse continuously decreased up to 70% reduction (Fig. 18(a–c)), and thereafter
direction, the ODF section corresponding to φ2 equal to 0°and 30° showed it was again increased for 90% reduction (Fig. 18(d)). Additionally, we ob-
dominant {0001} basal fiber with both A and D components along with served some other components such as f1120gh0001i at {φ1 = 90°,

Fig. 7. Fraction of LAGBs and HAGBs evolved in Zircaloy-4 after rolling up to various percentages of reduction (25%, 50%, 70% and 90%) along (a) ND – ED and ND – TD planes at room
temperature, and (b) along ND – ED and ND – TD planes at cryogenic temperatures.
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 303

Table 1 changes in texture with the successive rolling reductions at room and
Showing fraction of LAGBs and HAGBs evolution after rolling up to various rolling reduc- cryogenic temperatures along the extrusion and transverse directions
tions (%) along the ND – ED and ND – TD planes at room temperature.
were characterized by calculating the volume fraction of the 0002 fiber
S·no. Rolling reduction Fraction of LAGBs Fraction of HAGBs which was present as the major texture component in nearly all the de-
(%) formed samples and is shown in Fig. 19(a, b). The percentage volume
ND – ED ND – TD ND – ED ND – TD
plane plane plane plane fraction of basal fiber component after rolling at both the temperatures
1. 25 0.070 0.077 0.929 0.923 along the extrusion direction was continuously increased while along
2. 50 0.074 0.063 0.926 0.937 the transverse direction, it was high after 25% reduction only after
3. 70 0.048 0.235 0.952 0.765 which it was decreased up to 70% reduction and then, it was increased
4. 90 0.217 0.190 0.783 0.809 again after 90% reduction.

Table 2 4. Discussion
Showing fraction of LAGBs and HAGBs evolution after rolling up to various rolling reduc-
tions (%) along the ND – ED and ND – TD planes at cryogenic temperature.
4.1. Microstructure Evolution Deformed Samples
S·no. Rolling reduction Fraction of LAGBs Fraction of HAGBs
(%) Rolling at room and cryogenic temperatures along the extrusion and
ND – ED ND – TD ND – ED ND – TD
plane plane plane plane transverse directions having dominant basal and non-basal orientations
1. 25 0.052 0.071 0.948 0.929
initially, at low to medium strains (from 25% to 50% reduction) showed
2. 50 0.193 0.044 0.807 0.956 some locally formed extension twins of the type f1012gh1011i along
3. 70 0.168 0.189 0.832 0.811 with some slip activity. The prismatic 〈a〉 slip f1010gh1210i is
4. 90 0.607 0.407 0.393 0.593
the easiest activated mode and is operative at all ranges of tempera-
tures, while the f1012gh1011i extension twins are observed as the
most commonly detected twinning mode in the HCP metals [29]
φ = 90°, φ2 = 0 ° } from 25% to 50% reduction (Fig. 18(a, b)), f0110g
which was observed in the present work also as the only twinning
h4221i at fφ1 ¼ 7:5°, φ = 90 ° , φ 2 = 30 ° } after 25% reduction (Fig.
mode up to 50% reduction at both room and cryogenic temperatures
18(a)), f1215gh1010i at fφ1 ¼ 0°, φ = 32 ° , φ 2 = 0 ° } from 70% to along both the extrusion and transverse directions (Figs. 3(a, b)–6(a,
90% reduction (Fig. 18(c, d)), and components close to f12118gh2311i at b)). However, their number fractions were higher along the transverse
fφ1 ¼ 70°−90°, φ = 10 ° , φ2 = 0 ° } and f01110gh1763i at fφ1 ¼ 80°, direction at both the temperatures due to its initial texture being dom-
φ = 10 ° , φ2 = 30 ° } after 90% rolling reductions (Fig. 18(d)). Further, inant in non-basal orientations. A small shear magnitude and the lowest

Fig. 8. KAM profile of Zircaloy-4 after rolling up to various percentages of reduction (25%, 50%, 70% and 90%) along ND – ED (a) and ND – TD (b) planes at room temperature, and along ND –
ED (c) and ND – TD (d) planes at cryogenic temperature.
304 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Fig. 9. GAM distribution in Zircaloy-4 after rolling up to various percentages of reduction (25%, 50%, 70% and 90%) at room temperature (a, b) and at cryogenic temperature (c, d) along the
ND - ED and ND - TD planes, respectively.

critical resolved shear stress value (0.17σs) [35] might be related with while at higher strains (above 50% reduction) with the increase in
the activation of f1012gh1011i extension twins. Though, the activation grain refinement, the increasing CRSS prevented further twinning activ-
of a specific twinning system depends upon the crystallographic orien- ity and hence b c + a N pyramidal slip along with prismatic and basal slip
tation of the grains also [41]. dominated the deformation, thereby distorting the previously formed
Further, Christian et al. [42] have reported that the activation of twin boundaries which gradually transformed into ordinary grain
f1012gh1011i type of extension twins is easier in compression of boundaries. Therefore, from this it can be concluded that both the suffi-
cient slip of b a N prismatic, b c + a N pyramidal and bc N basal disloca-
the extruded HCP materials having f1010g fiber texture. Under the
tions at higher strains led to the increase in fraction of LAGBs after 90%
rolling condition, the material was subjected to a compressive strain in
reductions evident from Fig. 7(a, b), which finally led to the develop-
ND and a tensile strain in RD. As stated above, the initial texture compo-
ment of high in-grain misorientations at high strains as evident from
nents in our Zircaloy-4 sheets along the extrusion and transverse direc-
KAM (Fig. 8(a–d), GAM (Fig. 9(a–d)) and GOS (Fig. 10(b–d)) at both
tions can be characterized as the weak {0001} fiber and a strong f1010g
room and cryogenic temperatures, with higher in-grain misorientations
fiber textures, respectively (Fig. 1(a–d)). As the tensile strain was perpen-
development at cryogenic temperature.
dicular to the majority of 〈0001〉 bc N axis along the extrusion direction
and parallel to 〈0001〉 b c N axis along the transverse direction, there-
fore, the formation of extension twins along the extrusion direction was 4.2. Texture Evolution in Deformed Samples
difficult and was observed in few grains with non-basal orientations only.
Further at higher strains (70%–90% reduction), the increase in frac- During the process of deformation along the extrusion and trans-
tion of LAGBs as shown in Fig. 7(a, b), showed that the slip activity verse directions at room and cryogenic temperatures, the texture evolu-
was more prominent along both the directions (extrusion & transverse) tion showed maximum intensities in the (0002) pole figures
at both temperatures. The change in activation preference from twin- throughout (Figs. 11(a–d)–14(a–d)). The (0002) pole figure also
ning to slip at higher reduction is related with the grain size evolution. showed a significant amount of spread around the stable end orienta-
The CRSSs for both twinning and slip can be defined by Hall–Petch rela- tions with the increasing deformation strains. This large spread around
tionship which is given as σCRSS =σ0 + Kd−0.5, in which the slope KT for the stable end orientation indicated further possibility of reorientation
twinning is usually higher than the slope KS for slip [43]. It is reported of the grains with the successive deformation [38]. After a comparison
that the Hall–Petch slope for twinning is almost ten times than that of the textures evolved along the two directions (extrusion & trans-
for slip in case of Zirconium alloys [28]. Therefore, a decrease in grain verse) following rolling at room and cryogenic temperatures, the tex-
size at higher strains would increase the CRSS for twinning greater tures developed in Zircaloy-4 from 25% to 90% reductions were
than that for slip. It is noted that in the present study up to medium influenced by both the different processing temperatures and the differ-
strains (50% reduction), twinning played a major role in deformation ent processing directions having different initial textures. It was
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 305

Fig. 10. GOS distribution in Zircaloy-4 after rolling up to various percentages of reduction (25%, 50%, 70% and 90%) at room temperature (a, b) and at cryogenic temperature (c, d) along the
ND - ED and ND - TD planes, respectively.

observed that rolling at room temperature led to the development of a temperature, a greater affinity for TD split/T-texture throughout along
basal texture along with a weak RD split/R-texture throughout along the extrusion direction, while a basal texture from low to intermediate
the extrusion direction, and a basal texture with varying intensity strains, and TD split/T-texture at higher strains along the transverse di-
throughout along the transverse direction. Similarly, at cryogenic rection were observed. It is believed that the texture evolved after any

Fig. 11. (0002) and ð1010Þ pole figures of Zircaloy-4 rolled along ND – ED plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at room temperature.
306 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Fig. 12. (0002) and ð1010Þ pole figures of Zircaloy-4 rolled along ND – TD plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at room temperature.

strain step in the present work was a result of the previous texture ðf1012gh1011iÞ would tilt the c axis from TD to a direction in the plane
which was again a function of initial texture, deformation strain and ND - RD [44]. This was also substantiated by the evolution of a texture
temperature that led to the activation of different operable systems component close to M f0110gh2113i at fφ1 ¼ 30°, φ=90° , φ2 =30 °}
(slip and twinning) as per their ease of activation and resulted in the after 25% reduction (Fig. 15(a)) which is reported as a product of
evolution of a final stable texture. The mechanisms leading to the devel- twinning [44–46]. Further, the texture evolution from 50% to 70% reduc-
opment of various textures after deformation at different temperatures tions (Fig. 11(b, c)), showing increasing intensity of basal poles towards
(room & cryogenic) along the two different directions (extrusion & ND along with an increasing intensity of c poles split in the ND - RD plane
transverse) are as follows. Texture evolution at room temperature
indicated the contribution of basal glide, f1010gh1120i prismatic glide,
along the extrusion direction at low strains (25% reduction) showing a
f1011gh1120i and f1011gh1123i pyramidal glide, and f1012gh1011i
weak peak in the ND - RD plane (Fig. 11(a)) indicated the twinning of
twinning. Philippe et al [39]. by performing Taylor simulations of
orientation C ðf1120gh1010iÞ as observed in as-received alloy texture
the rolling textures of Ti and Zr reported that the combined action of
along this direction (Fig. 2(b)). It is reported that the component C
ba N prismatic, b a N and b c + a N pyramidal glides, and f1012gh1011i
which has c axis parallel to the TD after undergoing extension twinning

Fig. 13. (0002) and ð1010Þ pole figures of Zircaloy-4 rolled along ND – ED plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at cryogenic temperature.
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 307

Fig. 14. (0002) and ð1010Þ pole figures of Zircaloy-4 rolled along ND – TD plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at cryogenic temperature.

twinning leads to the RD split/R-type textures (showing a split of c poles to 70% requiring accommodation of deformation strain along bc N axis
in the ND - RD plane), and the addition of basal glide to the combination could be only possible by the activation of bc + a N pyramidal slip
of these deformation systems rotates the c poles towards the ND. After (Fig. 12(b, c)) [21]. Finally, the texture evolved after 90% reduction
90% reduction, the texture evolved suggested the activation of ba N (Fig. 12(d) indicated the significant role of basal slip along with ba N
basal slip along with b c + a N pyramidal and ba N prismatic slips [38, prismatic and b c + a N pyramidal slips [38,39].
39] (Fig. 11(d)). Texture evolution along the transverse direction at At cryogenic temperature, textures along the extrusion direction
room temperature after 25% reduction indicated the dominant role of (Fig. 13(a–d)) from low to high strains showing a TD split/T-type tex-
extension twins of type f1012gh1011i, which by activating in grains ture (bc N poles split along the ND - TD plane) with some spread
with the bc N axis nearly perpendicular to the axis of the applied (small to large) in the ND - RD plane suggested the activation of
compressive load rotated the b c N axis of the grains by 85.22°, thereby bc + a N pyramidal slip system. It is reported that the splitting of the c
making it parallel to the direction of maximum compressive force [47] poles and tilting by 20°to 40° towards TD in the final stable orientations
(Fig. 12(a)). As the majority of bc N axis became parallel to the compres- could be achieved by pyramidal slip with b c + a N Burger's vector, on
sive load after 25% reduction, therefore, the further reductions from 50% the f1121g or f1011g plane [39,48] and the evolution of a final T -

Fig. 15. Orientation distribution function represented as φ2 =0°&φ2 =30° section of Zircaloy-4 rolled along ND – ED plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at room
temperature.
308 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Fig. 16. Orientation distribution function represented as φ2 =0°&φ2 =30° section of Zircaloy-4 rolled along ND – TD plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at room
temperature.

type texture is usually formed by the combined action of prismatic slip Likewise, TD split/T-type texture from low to intermediate strains is at-
baN, pyramidal slip b c + aN, basal slip, and compressive/tensile twin- tributed to prismatic ba N and pyramidal b c + a N slip systems with
ning [39,41,46]. While along the transverse direction from low to inter- minor contribution of the extension twinning, while at higher strains,
mediate strains (25% to 50% reductions) as shown in Fig. 14(a, b), basal the contribution of basal slip could not be ignored as the activation of
fiber texture due to the combined action of f1012gh1011i extension basal slip at high strain as well as high strain rate in zirconium and tita-
twins, b a N prismatic slip,ba N and bc + a N pyramidal slips were ob- nium has been recently reported [38,49]. In addition, the ODFs sections
served [39], and a TD split/T-type texture at higher strains (70%–90% re- corresponding to φ2 = 0° and 30° after 90% reduction along the extru-
ductions) (Fig. 14(c, d)) due to the combined activity of prismatic slip sion and transverse directions showed a high intensity of basal fiber tex-
baN, pyramidal slip b c + aN, and basal slip were observed. Thus, basal ture with A and D as the clear texture components along with a strong
texture from low to intermediate strains is accounted for extension intensity close to f1215gh1010i at fφ1 ¼ 0°, φ = 32 ° , φ2 = 0 ° } (Figs.
twins, b aN prismatic glide, baN and bc + a N pyramidal glide while at 15(a–d), 16(a–d)), 17(a–d) and 18(a–d)). However, an overall lower
higher strains, basal slip has also had a significant contribution. volume fraction of basal fiber texture as a dominant component is

Fig. 17. Orientation distribution function represented as φ2 =0°&φ2 = 30° section of Zircaloy-4 rolled along ND – ED plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at
cryogenic temperature.
 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310 309

Fig. 18. Orientation distribution function represented as φ2 =0° & φ2 = 30° section of Zircaloy-4 rolled along ND – TD plane up to (a) 25%, (b) 50%, (c) 70%, and (d) 90% reduction at
cryogenic temperature.

present after rolling along both the directions. Therefore, it can be con- and b c + a N pyramidal glide, f1012gh1011i extension twinning, and
cluded that the different textures evolved with the successive rolling basal glide particularly at high strain.
strains were functions of different temperatures and different initial
textures adopted in the present work which by activating the various 2. The microstructures and textures evolved at cryogenic temperature
combinations of deformation systems at room and cryogenic tempera- along the extrusion direction from low to high strains were due to
tures led to the variation in texture evolution along the two directions the combined action of ba N prismatic slip, ba N and b c + a N pyrami-
(extrusion & transverse)). dal slips, basal slip, and extension twins while along the transverse
direction from low to high strains, textures were due to the com-
5. Conclusions bined action of f1012gh1011i extension twins, ba N prismatic slip,
baN and bc + a N pyramidal slips, and basal slip, the latter being ob-
Zircaloy-4 was subjected to various percentages of rolling reductions served at high strain.
such as 25%, 50%, 70% and 90% at room and cryogenic temperatures 3. The evolution of high fraction of LAGBs also supported the sufficient
along the extrusion and transverse directions which is corresponding to b a N prismatic, b c + a N pyramidal, and basal slip activity. The in-
the ND - ED and ND - TD planes, respectively. The microstructural and tex- grain misorientations investigated through the KAM, GAM & GOS
tural evolution following rolling along both the directions were analyzed were increased which is the usual trend followed by the deformed
through EBSD and Bulk texture, and following conclusions are made. material.
4. The (0002) pole figures and the ODFs sections corresponding to
1. The microstructures and textures evolved at room temperature φ2 = 0° and 300 revealed an overall lower volume fraction of basal
along the extrusion and transverse directions at low strain were at- fiber texture component after 90% reduction in all the deformed con-
tributed to extension twinning and b a N prismatic slip, and from in- ditions which being a stable texture is generally observed in Zr alloy
termediate to high strains they were due to b aN prismatic glide, b aN tubes, rods and plates.

Fig. 19. Variation in volume fraction of basal fiber with the various percentages of rolling reductions (25%, 50%, 70%, and 90%) of Zircaloy-4 along (a) ND – ED and ND – TD plane at room
temperature and (b) along ND – ED and ND – TD plane at cryogenic temperature.
310 D. Fuloria et al. / Materials Characterization 127 (2017) 296–310

Acknowledgement [23] G.C. Kaschner, C.N. Tomé, I.J. Beyerlein, S.C. Vogel, D.W. Brown, R.J. MacCabe, Role of
Twinning in the hardening response of zirconium during temperature reloads, Acta
Mater. 54 (2006) 2887–2896.
One of the authors would like to thank BRNS, Bombay for their finan- [24] L. Capolungo, P.E. Marshall, R.J. McCabe, I.J. Beyerlein, C.N. Tome, Nucleation and
cial grant to this work through grant No: BRN-577-MMD. growth of twins in Zr: a statistical study, Acta Mater. 57 (2009) 6047–6056.
[25] I.J. Beyerlein, C.N. Tome, A dislocation-based constitutive law for pure Zr including
Temperature effects, Int. J. Plast. 24 (2008) 867–895.
References [26] G.W. Groves, A. Kelly, Independent slip systems in crystals, Philos. Mag. 8 (1963)
877–887.
[1] J.H. Schemel, Astm Manual on Zirconium and Hafniium, 639, Astm International, [27] R.J. McCabe, E.K. Cerreta, A. Misra, G.C. Kaschner, C.N. Tome, Effects of texture, tem-
1977. perature and strain on the deformation modes of zirconium, Philos. Mag. 86 (2006)
[2] K.L. Murty, I. Charit, Texture development and anisotropic deformation of zircaloys, 3595–3611.
Prog. Nucl. Energy 48 (2006) 325–359. [28] S.G. Song, G.T. Gray, Influence of temperature and strain rate on slip and twinning
[3] B.A. Cheadle, C.E. Coleman, H. Litchit, CANDU-PHW pressure tubes: their manufac- behavior of Zr, Metall. Mater. Trans. A 26 (1995) 2665–2675.
ture, inspection, and properties, Nucl. Technol. 57 (1982) 413–425. [29] M.H. Yoo, J.K. Lee, Deformation twinning in h.c.p. metals and alloys, Philos. Mag. 63
[4] A. Sarkar, K.L. Murty, Microstructure–mechanical property correlation of cryorolled (1991) 987–1000.
Zircaloy-4, J. Nucl. Mater. 456 (2015) 287–291. [30] F. Long, F. Xu, M.R. Daymond, Temperature dependence of the activity of deforma-
[5] D. Srivastava, G. Dey, S. Banerjee, Evolution of microstructure during fabrication of tion modes in an HCP zirconium alloy, Metall. Mater. Trans. A 44 (2013) 4183–4193.
Zr-2.5 Wtpct Nb alloy pressure tubes, Metall. Mater. Trans. A 26 (1995) 2707–2718. [31] B.D. Cullity, S.R. Stock, Elements of X-Ray Diffraction, third ed. Prentice Hall, New
[6] N. Hansen, Hall-Petch relation and boundary strengthening, Scr. Mater. 51 (2004) Jersey, 2001.
801–806. [32] D. Fuloria, N. Kumar, S. Goel, R. Jayaganthan, S. Jha, D. Srivastava, Tensile properties
[7] R.Z. Valiev, Y. Estrin, Z. Horita, T.G. Langdon, M.J. Zechetbauer, Y.T. Zhu, Producing and microstructural evolution of zircaloy-4 processed through rolling at different
bulk ultrafine-grained materials by severe plastic deformation, JOM J. Miner. Met. temperatures, Mater. Des. 103 (2016) 40–51.
Mater. Soc. 58 (2006) 33–39. [33] D. Fuloria, P. Nageswararao, R. Jayaganthan, S. Jha, D. Srivastava, An investigation of
[8] Y. Estrin, A. Vinogradov, Extreme grain refinement by severe plastic deformation: a deformed microstructure and mechanical properties of zircaloy-4 processed
wealth of challenging science, Acta Mater. 61 (2013) 782–817. through multiaxial forging, Mater. Chem. Phys. 173 (2016) 12–25.
[9] B.J. Han, Ultrafine grained Fe-32% Ni alloy processed by multiaxial forging, Adv. [34] Y.N. Wang, J.C. Huanga, Texture analysis in hexagonal materials, Mater. Chem. Phys.
Mater. Res. 97 (2010) 187–190. 81 (2003) 11–26.
[10] S.V. Zherebtsov, G.S. Dyakonov, A.A. Salem, V.I. Sokolenko, G.A. Salishchev, S.L. [35] B. Luan, Y.E. Qing, J. Chen, H. Yu, D. Zhou, Y. XIN, Deformation twinning and textural
Semiatin, Formation of nanostructures in commercial-purity titanium via evolution of pure zirconium during rolling at low temperature, Trans. Nonferrous
cryorolling, Acta Mater. 61 (2013) 1167–1178. Metals Soc. China 24 (2013) 2890–2895.
[11] X.X. Wu, Y.L. Gong, S.Y. Ren, J.M. Tao, Y. Long, L.P. Cheng, X.K. Zhu, Effect of annealing [36] S. Biswas, S.S. Dhinwal, S. Suwas, Room-temperature equal channel angular extru-
on mechanical properties of copper alloys deformed at cryogenic temperature, sion of pure magnesium, Acta Mater. 58 (2010) 3247–3261.
Mater. Sci. Forum 745 (2013) 363–370. [37] S.K. Sahoo, V.D. Hiwarkar, I. Samajdar, P. Pant, G.K. Dey, D. Srivastava, R. Tewari, S.
[12] P. Das, R. Jayaganthan, I.V. Singh, Tensile and impact-toughness behaviour of Banerjee, Deformation twinning in zircaloy 2, Mater. Sci. Technol. 26 (2010)
cryorolled Al 7075 alloy, Mater. Des. 32 (2011) 1298–1305. 104–114.
[13] S. Goel, R. Jayaganthan, I.V. Singh, D. Srivastava, G.K. Dey, N. Saibaba, Mechanical and [38] N.P. Gurao, H. Akhiani, J.A. Szpunar, Pilgering of zircaloy-4: experiments and simu-
microstructural characterizations of ultrafine grained zircaloy-2 produced by room lations, J. Nucl. Mater. 453 (2014) 158–168.
temperature rolling, Mater. Des. 55 (2014) 612–618. [39] M.J. Philippe, C. Esling, B. Hocheid, Role of twinning in texture development and in
[14] S. Goel, N. Keskar, R. Jayaganthan, I.V. Singh, D. Srivastava, G.K. Dey, N. Saibaba, Me- plastic deformation of hexagonal materials, Texture Microstruct. 7 (1988) 265–301.
chanical behaviour and microstructural characterizations of ultrafine grained [40] R.G. Ballinger, R.M. Pelloux, The effect of anisotropy on the mechanical behavior of
zircaloy-2 processed by cryorolling, Mater. Sci. Eng. A 603 (2014) 23–29. zircaloy-2, J. Nucl. Mater. 97 (1981) 231–253.
[15] P. Kamalnath, A. Sarkar, Tensile behavior of cryorolled zircaloy-2, J. Mater. Sci. 2 [41] Y.B. Chun, S.H. Yu, S.L. Semiatin, S.K. Hwang, Effect of deformation twinning on mi-
(2012) 138–141. crostructure and texture evolution during cold rolling of CP-titanium, Mater. Sci.
[16] Y. Shi, M. Li, D. Guo, T. Ma, Z. Zhang, G. Zhang, X. Zhang, Tailoring grain size distri- Eng. A 398 (2005) 209–219.
bution for optimizing strength and ductility of multi-modal Zr, Mater. Lett. 108 [42] J.W. Christian, S. Mahajan, Deformation twinning, Prog. Mater. Sci. 39 (1995) 1–157.
(2013) 228–230. [43] M.A. Meyers, O. Vöhringer, V.A. Lubarda, The onset of twinning in metals: a consti-
[17] D. Guo, M. Li, Y. Shi, Z. Zhang, H. Zhang, X. Liu, X. Zhang, Effect of strain rate on mi- tutive description, Acta Mater. 49 (2001) 4025–4039.
crostructure evolutions and mechanical properties of cryorolled Zr upon annealing, [44] H.P. Lee, C. Esling, H.J. Bunge, Development of the rolling texture in titanium, Tex-
Mater. Lett. 66 (2012) 305–307. ture Microstruct. 7 (1988) 317–337.
[18] D. Guo, M. Li, Y. Shi, Z. Zhang, H. Zhang, X. Liu, B. Wei, X. Zhang, High strength and [45] Y. Zhong, F. Yin, K. Nagai, Role of deformation twin on texture evolution in cold-
ductility in multimodal-structured Zr, Mater. Des. 34 (2012) 275–278. rolled commercial-purity Ti, J. Mater. Res. 23 (2008) 2954–2966.
[19] D. Guo, Z. Zhang, G. Zhang, M. Li, Y. Shi, T. Ma, X. Zhang, An extraordinary enhance- [46] N.P. Gurao, S. Suwas, Evolution of crystallographic texture during deformation of
ment of strain hardening in fine-grained zirconium, Mater. Sci. Eng. A 591 (2014) submicron grain size titanium, J. Mater. Res. 26 (2011) 523–532.
167–172. [47] A. Salnas-Rodriguez, Grain size effects on the texture evolution of α – Zr, Acta
[20] E. Tenckhoff, Review of deformation mechanisms, texture, and mechanical anisotro- Metall. Mater. 43 (1995) 485–498.
py in zirconium and zirconium base alloys, J. ASTM Int. 2 (2005) 25–50. [48] E. Tenckhoff, The development of the deformation texture in Zirconium during
[21] L. Chai, B. Luan, D. Xiao, M. Zhang, K.L. Murty, Q. Liu, Microstructural and textural rolling in sequential passes, Metall. Trans. A. 9 (1978) 1401–1412.
evolution of commercially pure Zr sheet rolled at room and liquid nitrogen temper- [49] G.G. Yapici, C.N. Tomé, I.J. Beyerlein, I. Karaman, S.C. Vogel, C. Liu, Plastic flow anisot-
atures, Mater. Des. 85 (2015) 296–308. ropy of pure zirconium after severe plastic deformation at room temperature, Acta
[22] R.G. Ballinger, G.E. Lucas, R.M. Pelloux, The effect of plastic strain on the evolution of Mater. 57 (2009) 4855–4865.
crystallographic texture in zircaloy-2, J. Nucl. Mater. 126 (1984) 53–69.