Materials Characterization 175 (2021) 111061

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

Shock-induced twinning in polycrystalline vanadium: I. twinning stress

A. Hazan a, G. Hillel a, S. Kalabukhov a, N. Frage a, E.B. Zaretsky b, L. Meshi a, *
a
Department of Materials Engineering, Ben-Gurion University of the Negev, P.O.Box 653, Beer Sheva 84105, Israel
b
Department of Mechanical Engineering, Ben-Gurion University of the Negev, P.O.Box 653, Beer Sheva 84105, Israel

A R T I C L E I N F O A B S T R A C T

Keywords: The shock-induced twinning at room temperature was studied using 3 mm thick vanadium samples of com­
Vanadium mercial purity (99.8 wt%), softly recovered after planar impact loading by copper impactors with velocities
Impact loading ranging from 262 to 610 m/s. Microscopic (Light and Scanning Electron) examinations of the samples’ cross-
Plastic deformation
sections revealed twins in a strip of vanadium grains, located 100–900 μm apart from the impacted sample
Twins
Twinning stress
surface. Transmission electron microscopy characterization allowed concluding that these twins are produced by
Electron microscopy a/6 〈111〉{211} glide in subsequent {211} planes. The number of twins, Ntw, per unit area varied from its
maximum value, measured at the distance h = 0.2–0.3 mm from the impacted sample surface, to Ntw = 0 at h =
0.7–0.9 mm apart from the surface. Juxtaposition of the presently obtained Ntw(h) dependencies with previously
reported spatial distribution of the shear stress, τ(h), in shock-loaded vanadium samples made it possible to
determine twinning stress in vanadium as: τ (Ntw = 0) = τtw = 0.68(±0.03) GPa.

1. Introduction vanadium samples of commercial purity (99.8%), softly recovered after

Vanadium is an important alloying element in many steels and ti­
tanium alloys which are used as structural materials, cutting tools, nu­
clear installations and, even, in medicine. Having Body Centered Cubic
(BCC) lattice (a = 0.303 nm) and, accordingly, high Peierls stress [1,2],
vanadium is relatively hard material. At the same time, its ductility is
much higher and stacking fault energy lower with respect to other BCC
metals [3,4]. These properties stimulated research on inelastic behavior
of vanadium since the end of 50-ies [e.g., 1,5–8] up to the present [e.g.,
[9–18]]. In these studies, a special focus was on dislocation mechanisms,
responsible for plastic deformation of vanadium. It is generally agreed,
that glide systems in vanadium are the same as in other BCC metals, i.e.
Burgers vectors of dislocations,b = a/2〈111〉, coincide with the shortest
interatomic distance, while the glide can occur both at {110} and {211}
planes [e.g., 1,6,7,14,18]. Preference of a glide family of planes depends
on crystal (grain) orientation and test temperature [1,2,7,19], strain rate
[11] and presence of impurities [8]. At the same time, it was found that,
in addition to the glide, low-temperature (around 77 K) plastic defor­
mation of vanadium is associated with appearance of considerable
amount of twins [1,3,5,6,11,20]. It was reported that these twins had
{211} twin planes. Consequently, the twinning schemes, suggested in
the literature, were of 〈111〉{211} type [20,21].
Recently, a fair amount of deformation twins was reported to exist in
impact (high strain rate) loading [22]. It is noteworthy that the impact
loading was performed at room temperature (i.e., above 77 K).
Following high strain rate (2500 s− 1) loading of vanadium samples at
room-temperature - no deformation twins were found [11], although it
is known that intense impact (shock) loading of metals may result in the
appearance of twins. For example, in nickel and copper, the deformation
twins were found in recovered samples after loading up to 30 and 14.5
GPa, respectively [23]. In brass, the deformation twins appear after
loading up to 17 GPa [24]. At the same time, the impact stress in the
experiments [22], where vanadium samples were found twinned, was
moderate, i.e., it did not exceed 4 GPa.
The appearance of twins in moderately shocked vanadium at room
temperature provided a motivation for the present study. Comprehen­
sive characterization of the impact response of vanadium in [22] was a
firm mechanical basis for this study, while metallographic examinations,
including light and electron microscopy of recovered vanadium samples,
made it possible to quantify the amount and geometry of shock-related
twins as well as identify their crystallographic characteristics.
Section 2 of the present paper describes the process of preparation of
the vanadium samples for planar impact testing. The testing is accom­
panied by VISAR-instrumented (Velocity Interferometer System for Any
Reflector [25]) continuous monitoring of the velocity of rear sample
surface and followed by soft recovery of the shocked samples. Section 3

* Corresponding author.
E-mail address: louisa@bgu.ac.il (L. Meshi).

https://doi.org/10.1016/j.matchar.2021.111061
Received 21 December 2020; Received in revised form 21 March 2021; Accepted 22 March 2021
Available online 25 March 2021
1044-5803/© 2021 Elsevier Inc. All rights reserved.
A. Hazan et al.
describes the experimental results in two subsections. The first subsec­
tion contains the outcome of Light and Scanning Electron microscopy
examinations (LM and SEM, respectively) of un-shocked and shocked
vanadium samples. In the second subsection, presently recorded velocity
histories are analyzed together with the velocity histories obtained in
[22] for vanadium samples of the same type. The goal of this subsection
is to specify the shear stresses acting at different cross-sections of the
examined samples. In Section 4, the results of Section 3 are discussed
and, then, summarized in Section 5.
2. Materials and experimental
Following [22], vanadium of commercial purity (99.8 wt%) was
obtained from Goodfellow Cambridge Ltd. (Cambridge, UK) as a plane-
parallel plate of nominal thickness 3.15 mm. The plate was cut into 14
mm × 14 mm squares, using an Electric Discharge Machining (EDM) and
then, turned down to diameter 12.51+0.005
0.000 mm by CNC lathe. In order to
release the rolling-related residual stress, the samples were annealed at
1000 ◦ C for 1 h in evacuated quartz ampules under an Ar atmosphere
(10− 4 Torr). In order to prevent lateral unloading of the shocked sample
(see next Subsection), the annealed samples were inserted into pre­
heated up to 300 ◦ C shrink-fit rings, made of the same vanadium plate.
At room temperature, inner and outer diameters of the rings were equal
to 12.500.000
− 0.005 and 23 mm, respectively. In order to release shrinking
stress of about 30–50 MPa [26], the sample-ring assembles underwent
stress recovery at 200 ◦ C for one hour and then ground down to ~3 mm
thickness and 0.5 mrad plane-parallelism.
2.1. Impact loading of vanadium samples
Three annealed samples were impact loaded by plane-parallel 0.5
and 1 mm thick copper impactors, accelerated in 6 m long smooth barrel
laboratory gun of 25 mm caliber up to velocities 262, 309 and 610 m/s.
A two-axes gimbal-like sample holder, located 15 mm from the gun
muzzle, provided impactor/sample misalignment better than 0.5 mrad.
The impact velocity was measured (with an uncertainty of less than 1%)
by two pairs of electrical charged pins (one flush with and one protruded
1 mm from the sample front surface) and by two in-barrel optic fiber
stations. These measures allowed creating strictly unidimensional strain
boundary conditions at the impacted sample surface. The velocity of the
rear, un-impacted, sample surface was continuously monitored by
VISAR [25] with 439.2 m/s/fringe constant. The experimental config­
uration is shown schematically in Fig. 1a. VISAR signals were recorded
by TDS 7104 1-GHz bandwidth digital oscilloscope with sampling rate
2.5 Giga-sample/s. The tested samples of annealed vanadium are
marked as VA262, VA309 and VA610, where VA denotes annealed va­
nadium and the number - velocity of an impactor in m/s.
Prior to the impact testing, the density ρ0 (Archimedes method) and
longitudinal cl and shear cs speeds of sound (Pulse-echo technique, 5-
MHz transducers) of all vanadium samples were determined. The re­
sults of these measurements together with the calculated bulk speed of
Fig. 1. Scheme of the impact loading of vanadium samples (a) and sectioning of the softly recovered sample (b). LM, SEM and TEM - are light, scanning electron and
transmission electron microscopies, respectively.
2
Materials Characterization 175 (2021) 111061
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
sound cb = c2l − 4/3c2s , longitudinal E’ = ρ0c2l , shear G = ρ0c2s , bulk B
= ρ0c2b moduli and Poisson’s ratio ν = (1 − 2G/E’)/(2 − 2G/E’) are listed
in Table 1. Since the difference between the properties of studied sam­
ples does not exceed the uncertainty of the property measurement, the
mean values of the properties, given in the bottom line of Table 1, were
used for the experimental data treatment.
2.2. Metallographic examination of vanadium samples
Vanadium samples, softly recovered [27,28] after VA262, VA309
and VA610 tests, and an un-impacted annealed sample were cut as
shown in Fig. 1b and underwent metallographic examinations. For Light
(LM) and Scanning Electron Microscopy (SEM), the samples were
mounted in acrylic, grinded on 1200, 2500 and 4000 grit SiC papers,
polished with 3 μm diamond paste and, finally, by 0.25 μm colloidal
silica. The polished samples were etched for 15–20 s with solution
containing 30 ml of H2O, 30 ml of 65% nitric acid, 30 ml of 32% hy­
drochloric acid and 15 ml of 40% hydrofluoric acid. LM ZEISS Axiovert
25, equipped with Paxcam3 camera and ability to apply Thixoment
software [29,30] for image analysis, was used. An FEI Verios 460 L high
resolution SEM with Oxford Instruments electron back scattered
diffraction (EBSD) detector was used for thorough microstructural study
and twin evaluation. For EBSD analysis, samples were additionally
polished electrolytically (3 V, 3 s) using 590 ml methanol (CH3OH), 6 ml
of H2O, 350 ml of bi-butoxyethanol (C6H14O2) and of 54 ml of perchloric
acid (HClO4) solution on LectroPol-5 Machine, Struers.
The LM and SEM images of an un-impacted sample are shown in
Fig. 2. It is apparent that prior to the impact loading, vanadium samples
consisted of 10–100 μm equiaxial grains and were absolutely twin-free.
Transmission Electron Microscopy (TEM) investigation was carried
out using a JEOL JEM-2100F TEM operating at 200 kV equipped with
JED-2300 T Energy Dispersive Spectrometer (EDS), scanning coils and
GATAN 806 high angle annular dark field (HAADF) detector. TEM
samples were prepared using Helios G4 UC Focused Ion Beam (FIB) at
several orientations – both parallel to the impacted surface and in cross-
section (which is the same orientation as shown in Fig. 1b).
3. Results
3.1. Metallographic examination of shocked vanadium samples
The cross-sections of three samples, VA262, VA309 and VA610,
softly recovered after shock loading exhibited deformation twins. Even
after the weakest impact, VA262, the amount of twins in shocked va­
nadium was significant, see Fig. 3. As in Fig. 2a, the black horizontal
ribbon at the upper part of the LM image of Fig. 3 represents acrylic
mounting, bottom border of which is adjacent to the impacted sample
surface. Some 100 μm apart from the surface, the twins start to appear. It
is noteworthy, that in all three tested samples the appearance of twins
was preceded by 50–70 μm-wide gray strip. Metallurgical features,
A. Hazan et al. Materials Characterization 175 (2021) 111061

Table 1
Mechanical properties of vanadium samples annealed at 1000 ◦ C for 1 h. The figures in parentheses correspond to the uncertainty of the last digit of the measured
property.
Test ρ0 , cl , cs , cb , E’ , G, B, ν
kg/m3 km/s km/s km/s GPa GPa GPa
VA262 6130(5)a 6.05(2) 2.80(2) 5.11(4) 224(2) 48.0(5) 160(2) 0.364(3)
VA309 6130(5) 6.08(2) 2.80(2) 5.15(4) 227(2) 47.9(5) 163(2) 0.366(3)
VA610 6130(5) 6.07(2) 2.78(2) 5.15(4) 226(2) 47.4(5) 163(2) 0.367(3)
Mean 6130(5) 6.07(3) 2.79(3) 5.14(5) 226(3) 47.8(8) 162(3) 0.366(4)
a
Figure in parentheses corresponds to the uncertainty of the last digit of the measured parameter.

Fig. 2. LM (a) and SEM (b) images of the un-shocked vanadium sample. Black band at the top of the left image is due to the interface with the acrylic mounting. Both
images are twin-free.

Fig. 3. LM (a) and SEM (b) images of the shocked vanadium sample (VA262 test). Black band at the top of the left image is the interface between the acrylic
mounting and shocked sample surface. The gray strip just below the mounting precedes the appearance of twins. Beyond some 850 μm apart from the impacted
surface, the grains are twin free. Image (b) was taken in the highest twin density area of the VA262 sample.

found in these gray strips, are the topic of the Part II of this series of
papers.
The amount of twins in the grains, being initially very modest, grows
rapidly with the distance and achieves its maximum somewhere be­
tween 250 and 350 μm apart from the impacted surface. Beyond this
limit - the amount of twins decreases as a function of distance from the
surface, and, at the distance of 850–1000 μm (depends on impact
strength) - the grains, again, become twin-free, see Fig. 3a.
Quantification of the LM images of the twinned cross-sections of the
shocked samples, namely determination of the number of twins, Ntw, per
unit area and the fraction of the area occupied by the twins, both as a
function of the distance h from impacted surface, were performed using
DotCount (http://reuter.mit.edu/software/dotcount), SolidWorks and
Measurement Log in Photoshop commercial software, respectively. The
results of these measurements are shown in Fig. 4. As it is apparent from
Fig. 4, twin-related parameters demonstrate similar variation with the
distance from the impacted surface. Although, it should be noted that
extrapolation of the initial parts of the dependencies up to the Ntw =
0 axis gives slightly different distances h0 (30 μm at the strongest and 70
μm at the weakest test) at which twin generation begins. Such “delay” in
the twin generation can be attributed to the accumulation of some
amount of plastic deformation as a prerequisite of the onset of twinning.
The state of the material at the impact surface is characterized by the
highest values of the shear stress and elastic strain. The plastic defor­
mation of the surface-adjacent layer, either by glide or by twinning, may
start immediately. In fact, this brings into operation only glide mecha­
nism, i.e., intense motion and multiplication of dislocations. This glide,
in turn, produces some surplus of dislocations, dissociation of which
launches the twinning. The dependencies, shown in Fig. 4a, evidently
correlate with the impact velocity, which is related to the stress acting in
the sample and governing formation of twins. The technique used for
determination of the stress states in different regions of the shocked (and

3
A. Hazan et al. Materials Characterization 175 (2021) 111061

10
2.5 10 12
a b
VA610 10
2 1010

area fraction o ccupied by twins , %

VA610

8
twin density Ntw, m-2

10
1.5 10

10
1 10

VA309
4

5 109
2
VA262
VA262
VA309
0 0
0 0.2 0.4 0.6 0.8 1 0 0.2 0.4 0.6 0.8 1
distance from impacted surface h, mm distance from impacted surface h, mm

Fig. 4. Number of twins per square meter Ntw (a), and area fraction occupied by the twins (b) as a function of the distance from impacted surface. Circles, squares and
diamonds correspond to the parameters measured at the cross-sections of VA610, VA309 and VA262 samples, respectively. Error bars correspond to the typical
uncertainties of the measured parameters.

twinned) vanadium samples is described in the next Subsection.
3.2. Free surface velocity histories. Shear stress acting in the shocked
vanadium samples
Presently recorded rear surface velocity histories of shock-loaded
vanadium samples are shown in Fig. 5 together with a velocity history
of 3 mm thick vanadium sample (VA514), tested at room temperature in
[22]. Although the impact velocity in test performed in [22], 514 m/s,
was slightly lower than that performed on VA610 sample (610 m/s) in
current research, Fig. 5 and inset within show that these results corre­
late. The velocity histories of all presently (and earlier) tested vanadium
samples contain an elastic precursor wave with a spike-like front part
with an amplitude uspike
HEL (HEL – Hugoniot elastic limit) followed by a
velocity minimum uminHEL, which is ensued by a plastic wave, terminated at
Hugoniot state with velocity uH. The presence of such a spike, at the
front part of the elastic precursor wave, is associated with an intense
multiplication of plastic deformation carriers (e.g., dislocations) under
shear stresses acting at the top and immediately behind the precursor
wave front [31, p. 41–44]. The compressive stress, σ spike
HEL , at the top of the
precursor wave corresponds to the elastic-plastic transition of the ma­
terial and is related to the measured uspike
HEL values as [31]

1
σ spike spike
HEL = ρ0 cl uHEL (1)
2
In isotropic material, σ spike
HEL acting in the impact direction and being,
by definition, the highest principal normal stress, is associated with the
maximum shear stress τspike
HEL acting at the planes 45 inclined to the
◦

impact direction
G spike
τspike
HEL = σ (1a)
E’ HEL
Accordingly, for post-spike minimum, the compressive and shear
stresses may be estimated as:
1
σ min min
HEL = ρ0 cl uHEL (2)
2

and
G min
τmin
HEL = σ (2a)
E’ HEL
Although Eqs. (1 - 2a) are necessary for treatment of the metallo­
Fig. 5. Free surface velocity histories of presently tested 3 mm samples of
graphic results, they are unable to provide an information about tem­
annealed vanadium (solid lines) and velocity history of 3 mm annealed vana­
dium sample of Ref. [22] (dashed line). The velocities of copper impactors (in poral/spatial distribution of the shear stress through the shocked
m/s) are given in the tests’ designations next to the waveforms. Arrows show sample. This information is obtained below basing on the results pre­
the waveforms’ parameters used in the treatment of the experimental data. The sented in [22].
inset shows magnified front parts of the waveforms. As a result of an impact, the shock wave, generated at the

4
A. Hazan et al. Materials Characterization 175 (2021) 111061

copper‑vanadium interface, starts to propagate through the vanadium the value u∞HEL = 150 m/s, which corresponds to the shear stress τHEL =
∞

sample towards its rear surface. The initial, at the impact interface, 0.59 GPa. (ii) Particle velocity in vanadium sample was assumed to be
stress σ0HEL = σelastic
H (recall that the subscript H corresponds to the final, one half of the free surface velocity [31]. (iii) The initial value of particle
Hugoniot, state of the shocked material) is determined by an intersec­ velocity u0HEL, at the impact interface, h = 0, is determined by the impact
tion of extensions of elastic parts of the Hugoniots of colliding materials velocity uimp and by the intersection of extensions of elastic parts of
[32], as it is shown schematically in Fig. 6. vanadium and copper Hugoniots (Fig. 6):
Due to the different material’s compressibilities in elastic and plastic
ρCu Cu
0 cl
states, initial stress discontinuity splits into an elastic precursor wave u0HEL = V V
u
Cu imp
(3)
(ρ 0 cl+ ρCu0 cl )
with amplitude σHEL* propagating into the sample (and impactor, as
well) with velocity close to cl and a plastic wave with an amplitude σH* (iv) Between h = 0 and h = 3 mm- the velocity uHEL decays expo­
> σHEL* and velocity close to bulk speed of sound cb < cl. The initial nentially as
elastic stress value, σ 0HEL, is very high, while corresponding shear stress ( ) ( )
τ0HEL = Gσ 0HEL/E’is usually of the order of magnitude of the theoretical
( 0 ) h ( ) h
uHEL = u∞ ∞
HEL + uHEL − uHEL exp − *
= 150 + u0HEL − 150 exp − * ,
shear strength of material. At any rate, it is much higher than the shear h h
stress τstatic
HEL = Y/2, determined based on the yield strength Y, measured
(4)
in quasi-static (e.g., tensile or compression) tests. During propagation of
where h* is the only fitting parameter.
the elastic wave through the material, the stress at HEL σ HEL* decays
The expression (4) fits reasonably well (with Pearson correlation
towards its quasi-static value σstatic HEL , which is by one-two orders of
coefficient better than 0.93) three data series studied in [22], while the
magnitude lower than σ 0HEL. The shear stress at HEL τHEL* = GσHEL*/E’
parameter h* was found to be dependent linearly on the velocity uimp of
also decays with propagation distance h; the shear stress excess, τHEL* −
the copper impactor. This made it possible to find the dependencies of
τstatic
HEL , is spent on plastic deformation of the material, namely on dislo­
the shear stress on propagation distance, τHEL(h), for each impact test of
cation motion/multiplication and/or twinning. The elastic precursor
the present study in the form τHEL = τ∞HEL + Δτ exp (− h/h*):
wave propagates through pristine annealed vanadium where twins are
( )
absent (see Fig. 2) and dislocation density is low. The appearance of h
VA262 : τHEL = 0.59 + 0.51 × exp −
twins is evidently a result of shear stresses, associated with (i) elastic 0.43
precursor wave, τel, and (ii) plastic wave, τpl . The former may be ( )
h
determined as a mean value of τspike min
HEL and τHEL(Eqs. 1a and 2a), i.e.,τHEL = VA309 : τHEL = 0.59 + 0.71 × exp − , (5)
0.44
(τspike
HEL + τ min
HEL )/2. τ pl value may be estimated basing on the vanadium ( )
density ρHEL at the foot of plastic wave; the difference between free VA610 : τHEL = 0.59 + 1.97 × exp −
h
sample surface velocities at the foot, umin HEL, and at the top, uH, of the
0.52
plastic wave [33]; and knowledge of linear vanadium Hugoniot [34].
In the present work, metallographic examination of vanadium sam­ where units of τHEL and h are GPa and mm, respectively.
ples, shock-loaded by copper impactors having velocities 262, 309 and As apparent from Eqs. (5), the shear stressτHEL, associated with an
610 m/s, were performed. In [22], three sets of waveforms were ob­ elastic precursor wave, varies between τ0 = τHEL + Δτ = 1.1 and τ∞ HEL =

tained from annealed vanadium samples with thicknesses varying from 0.59 GPa for the weakest test,VA262, and between τ0 = 2.56 and τ∞ HEL =

0.2 to 3 mm. Those sets, however, were obtained after loading of the
vanadium samples by impactor having different, than measured here,
velocities, namely 241 ± 3 m/s, 514 ± 7 m/s, and 650 ± 5 m/s. As an
example, two velocity histories, recorded in [22] after loading of 0.228
and 1.040 mm thick vanadium samples by 0.5 mm copper impactors
having velocity of about 514 m/s, are shown in Fig. 7a. Note that the
0.59GPa for the strongest test, VA610. Fig. 7b shows schematically such
conversion of the recorded waveform into travelling (and decaying)
pulse of the shear stress. The time interval δtsm between the free surface
velocity spike (uspike) and the following velocity minimum (umin) can be
accepted as the width of the shear stress pulse.
Immediately after the velocity minimum, umin HEL, the velocity of the

thickness of the sample in [22] is, actually, the distance from the
impacted surface which is equal to the wave propagation distance h.
The waveforms of three series, studied in [22], were treated based on
the following considerations. (i) After 2 mm traverse the mean velocity
uHEL = (uspike min
HEL + uHEL)/2, independently of an impact strength, arrives at
Fig. 6. Initial (σ elastic
H , σ0HEL), intermediate (σH*, σ*HEL) and stationary (σ H, σHEL)
values of Hugoniot compressive stress and stress at HEL.
free sample surface starts to grow towards uH, associated with the top of
the plastic wave, Fig. 7a. The plastic ramp is accompanied by the in­
crease δτ of the shear stress which achieves its maximum δτmax = 3ρHELs
(uH − umin 2
HEL) /64 [33] at the half-height of the plastic wave, i.e., at u =
min
(uHEL + uH)/2. The parameter s, representing linear vanadium Hugoniot
Us = C0 + sup, where Us is the shock and up is the particle velocity, is
equal to 1.242 [34]. It should be noted that estimation of δτ makes sense
only in the case of stationary wave, where stress relaxation processes are
completed [35]. The velocity histories, recorded in [22], after loading of
2 and 3 mm vanadium samples with copper impactors, having velocity
of about 514 m/s, can be considered as close to stationary. The values of
δτmax estimated for these tests are δτmax = 0.05 ± 0.01 GPa and δτmax =
0.07 ± 0.01 GPa for h = 2 and h = 3 mm, respectively. In our case, the
propagation distances of an interest are even smaller than h = 1 mm
(which is the location of the most distant from the impacted surface
twins). At such propagation distance, the shear stress addition, associ­
ated with the plastic wave front, seems to be lower than the uncertainty
of the shear stress estimates in Eq. (5). Neglect of the δτmax may be
partially compensated by usage of time interval δtpl = h(1/cb − 1/cl)
between the elastic precursor front and the half-height of the plastic
wave, instead of δtsm, as the measure of the duration of the shear stress
pulse in Fig. 7b. It is noteworthy that the decay of the travelling shear
stress pulse with propagation distance is accompanied by its temporal/
spatial widening.
These uncertainties are, however, not the only shortcoming of the

5
A. Hazan et al. Materials Characterization 175 (2021) 111061

Fig. 7. (a) Free surface velocity histories recorded for 0.228 and 1.040 mm thick samples of annealed vanadium shock-loaded by 0.5 mm copper impactors having
velocity of about 514 m/s [22]. (b) Schematic representation of the shear stress pulses, associated with elastic precursor waves, in these tests is shown both as a
function of time after the impact and as a function of the precursor propagation distance, h, which is equal to the sample thickness. Note that the particle velocity,
upH, in Fig. 6 is one half of the recorded maximum sample free surface velocity - uH.

conversion scheme illustrated in Fig. 7b. It is unlikely, that after passage
of both - the elastic precursor wave and the plastic wave, flocking after
the elastic one, − the shear stress in the section will be completely
relaxed. The shock generated defects (dislocations, twins, etc.) will
continue to interact with the stress residue as long as the shear stress
exceeds τstatic
HEL , while the quantitative characteristics of this postponed
relaxation are beyond the reach. Based on these considerations and
taking into account that nucleation of twins requires much greater shear
stress than that required for the twin growth [36], the number of twins
Ntw per unit area (as not affected by the shear stress residue) was chosen
in the next Section as a main characteristic of the twins’ population.
4. Discussion
As stated above, the twins were found in the shocked samples at the
distance of h = 0.1 − 0.85 mm from the impacted surface. In order to
illustrate twin dispersion orientation-wise, EBSD maps (inverse pole
figures) were taken from VA262 and VA610 samples and analyzed, see
Fig. 8 (it should be noted that un-shocked EBSD maps were twin free,
thus are not shown here). Increase in the twin density as a function of the
velocity is evident. In VA262 and VA309 samples no twins were found
beyond the distance h = 0.85 mm. (The lowest number of twins, six, in a
stripe of 0.1 × 0.63 mmwas found in the VA262 sample at a distance
0.75–0.85 mm from the impacted surface.) In the sample VA610, the
twin density also decreased as a function of h (Fig. 4), but complete
vanishing of twins in vanadium grains is expected at greater h values.
Unfortunately, due to the spallation voids, a reliable count of twins in
VA610 sample at h greater than 1 mm was impossible.
The specific orientation of twins inside the matrix grain is clear.
Superimposed twin-matrix electron diffraction (ED) pattern (see
Fig. 9b), obtained from the area of the VA262 sample (as an example),
shown in Fig. 9a, allows identification of the matrix/twin mutual plane
as {211}. For comparison, TEM Bright Field (BF) image of the twins in
the VA610 sample is shown in Fig. 9c. Average width of the twins de­
creases, as compared to the VA262 sample (see Fig. 9a), and their
density increases. Superimposed matrix-twin ED patterns taken from
this area (not shown here), also point on the same {211} plane as a twin
plane. The indexing of the superimposed ED patterns, taken from the
VA610 sample, was extremely difficult due to the coexistence of more
than three patterns and double diffraction effects.
As it is apparent from Figs. 3 and 4, the reliable estimation of twin
number for calculation of twin density Ntw can be performed further
than the distance h0≥ 100 μm from the impacted surface. Taking into
account that plastic deformation starts at immediate proximity of the

Fig. 8. EBSD maps (inverse pole figures with a legend, presented on the right) of the (a) VA262 and (b) VA610 samples.

6
A. Hazan et al.
Fig. 9. (a) BF TEM of the twin (brighter) and matrix taken from the VA262 sample. (b) Superimposed ED pattern taken from the area shown in (a) at 011
orientation of both matrix and the twin. Mutual (211) plane is determined by indexing. (c) Typical BF TEM of the matrix and twins in the VA610 sample.
shock-loaded surface one can conclude that initiation of twinning should
be preceded by some small, but finite, plastic strain γ 0, realized by glide,
i.e., some dislocation density surplus (with respect to dislocation density
of the annealed material) should exist as a prerequisite for initiation of
twinning. In principle, it is expected that twins should be initiated in the
region of high dislocation density [37]. In this case, such place is in the
close vicinity to the impacted surface where twins did not form. It is
plausible to assume that initiation of twinning requires an amount of
plastic strain, meaning that high dislocation density is not enough; some
dislocation motion is needed. Evidently, this matter requires further
investigation.
All three Ntw(h) dependencies, shown in Fig. 4a, demonstrate fast
growth beyond h0 which, however, is ceased somewhere between 0.2
and 0.3 mm distance from the impacted surface. Starting from its
maximum, the Ntw(h) decreases monotonically towards almost complete
disappearance of the twins. The decline of Ntw(h) resembles the decay of
the shear stress τHEL at the top of elastic precursor wave with propaga­
tion distance h, Eq. (5). In Fig. 10, three twin density dependencies
Ntw(h) are plotted as a function of the shear stress, τHEL(h), for all tests.
Fig. 10. Twin densityNtw(h)values obtained in VA610 (circles), VA309
(squares), and VA262 (diamonds) tests as a function of the shear stress τHEL(h)
in corresponding test. Dashed line is the mutual linear fit of the points of the
descending branches of the three dependencies Ntw(h).
7
Materials Characterization 175 (2021) 111061
[ ]
The post-maximum (see Fig. 4a) Ntw(h) points of all three tests
evidently belong to a single Ntw(τHEL) dependence, which can be
described by the expression
[ ]
twins
Ntw 2
= 2.01 × 1010 × (τHEL − 0.68)[GPa], (6)
cm
with Pearson correlation coefficient better than 0.99. Therefore, the
shear stress value τtw = 0.68(±0.03) GPa should be considered as
twinning stress in vanadium.
It was mentioned above that some plastic glide, i.e., motion and
multiplication of dislocations, is one of the causes of twinning initiation
at small, less than 0.1 mm, distances h. It is likely that one of the reasons
for twinning initiation at larger h is the same dislocation motion/
multiplication. Usually, discussed mechanisms of twinning initiation are
based on a dislocation pileups at the head of which shear stress is high
enough for initiation of twinning [38–40]. At the presence of shear stress
τ, the head of a pileup is a stress concentrator; for the pileup containing
m dislocation loops and stopped by a grain boundary, the stress in the
vicinity of the pileup head, i.e. in the adjacent grain, is τ ’ = mτ. This
“overstress” favors nucleation of the twins at the grain boundary. At
least one end of the vast majority of twins, observed in the cross-sections
of all three samples, is fasten to the grain boundary (see Figs. 3 and 8).
Such mechanism, however, depends on the number of dislocations in the
pileup (hence, substantial scatter of experimentally measured twinning
stresses) and requires an occurrence of the dislocation slip prior the
twinning. The latter condition is severe in the case of shock loading: the
elastic precursor wave runs through the pristine (annealed, in the pre­
sent case) material. Although the initial plastic strain rate γ̇, associated
with arrival of the precursor, is very high - the occurrence of slip (motion
and multiplication of dislocations) requires some finite time. (Note, that
both the shear stress and the plastic strain rate immediately become
lower than their initial values.) As it was shown in Subsection 3b, the
time interval δtpl (h) = h(1/cb − 1/cl ) may be accepted as the time
available both for twinning and slip at distance h from the impacted
surface. This allows estimating the amount of plastic deformation (both
twinning and slip), which can be produced just behind the elastic pre­
cursor front. It was shown by Duvall [41] that in acoustic approxima­
tion, the decay of the τHEL with propagation distance may be described
as:
( )2
dτHEL 4 G
= − ρ0 cl γ̇, (7)
dh 3 E’
where γ̇ is initial (at the top of the elastic precursor wave) plastic strain
rate. It should be noted that Eq. (7) was derived without any assumption
concerning the mode, either glide or twinning or both, of the plastic
strain. Combining (7) and (5) gives
A. Hazan et al.
( )2
3 E’ Δτ
(
h
) nucleation of twins in quasi-static, either compressive or tensile, tests is
γ̇(h) = *
exp − * (8)
4 G ρ0 c l h h
Therefore, the plastic strain, accumulated at the sample cross-section
at the distance h from the impact surface, is γ(h) ≈ γ̇(h)δtpl (h). The plastic
strain γ grows very fast from 0 at h = 0 to some finite value at h ≈ 0.2
mm, and then, up to h = 0.8 mmstays virtually constant and equal to
γ VA262 = 0.0048 ± 0.0005, γVA309 = 0.0069 ± 0.007and γVA610 = 0.023
± 0.001 in the case of VA262, VA309 and VA610 samples, respectively.
Since fraction of plastic deformation, associated with the twins, is small
(see Fig. 5b) and does not exceed 7% for VA610 test and 1.5% for two
other tests - the figures in the previous sentence may be employed in
√̅̅̅
Orowan’s formula, γ ≈ ρbL ≈ ρb, for estimation of dislocation den­
sities ρ and average distances L ~ 1/√ρ between dislocations just behind
the precursor wave front. (It is assumed that the total dislocation density
ρtot and the density ρm of mobile dislocations coincide.) The corre­
sponding values are ρVA262 ≈ 3.7 × 1014m− 2, ρVA309 ≈ 7.6 × 1014m− 2,
ρVA610 ≈ 8.9 × 1015m− 2, and LVA262 ≈ 52 nm, LVA309 ≈ 36 nm,LVA610 ≈
11 nm. Taking into account that dislocation density in an annealed
material is unlikely to be greater than1011m− 2, even an insignificant
fraction of shock-generated dislocation surplus may prompt the nucle­
ation of twins. At the same time, the number m of dislocations in newly-
created pile-ups seems to be not very large. Its upper bound is given by
the ratio of the shear stress capable of generating twins at the VA610 test
(with highest impact velocity) to the twinning stress τtw = 0.68 GPa and
by the distance ratio LVA262/LVA610, i.e. m < 3 − 5.
Given the presently obtained value of the twinning stress at room
temperature, τtw = 0.68 GPa, the reason for the absence of twins in
vanadium after quasi-static [1,2,5–7] or split Hopkinson pressure bar
(SHPB) [11] testing becomes clear. In all experiments of these types, the
vanadium samples are loaded “from below”; the stress applied to the
sample grows either gradually (quasi-static test) or stepwise (SHPB
testing) from zero to vanadium yield point, which, at room temperature
is not greater than 0.4–0.5 GPa. Therefore, the elastic-plastic transition
may be accomplished based on dislocations only. In the case of low-
temperature (77 K), loading the yield and twinning stresses of vana­
dium seems to be close (see, e.g. [1,2]); the plastic deformation utilizes
both, dislocation and twin, paths. This situation resembles that of the
shock testing: the pristine material is loaded far above its both twinning
and yield thresholds - making competition/combination of the two paths
possible.
5. Conclusions
The shock-induced twinning in vanadium was studied using 3 mm
thick samples of commercial (99.8 wt% V) purity, softly recovered after
impact loading by copper impactors having velocities 262 to 610 m/s.
Microscopic examination of the recovered samples revealed presence of
twinned grains. The twinning begins some 0.1 mm apart from the
impacted surface and is terminated at the distance of 850–1000 μm from
the surface.
Calibration of the spatial-temporal distribution of the shear stress in
shock-loaded vanadium samples made it possible to obtain the depen­
dence of twin density Ntw on shear stress τHEL associated with the elastic
precursor wave, generated in the vanadium samples by planar impact
loading. Starting from the distance of about 250 μm from the impacted
surface, Ntw decreases linearly with the decrease of the shear stress and
vanishes completely at the distance of about 850–1000 μm from the
impacted surface, as soon as the shear stress decreases down to τel = 0.68
(±0.03) GPa. Since beyond this threshold no twins were found, the stress
τtw = 0.68 GPa may be considered as the twinning stress in vanadium.
The method of determination of twinning stress, τtw, used in current
research, is based on calibration of the shear stress in shock-loaded
sample combined with metallographic examination of shocked and
softly recovered samples. The obtained τtw value seem to be accurate.
The stress concentration by dislocation pileup, responsible for
8
Materials Characterization 175 (2021) 111061
hardly predictable. As a result, the literature data on τtw of a definite
metal are characterized by substantial scatter. Uncertainty of the pres­
ently suggested measurement of τtw is determined by statistical errors of
metallographic features` measurements and of the shear stress deter­
mination in shock experiment. These uncertainties can be easily reduced
to a few percent. At the same time, the experiments performed presently
at room temperature may be done at either elevated or reduced tem­
peratures, providing, thus, an information on temperature dependence
of τtw, which is hardly possible to achieve by conventional methods used
for τtw estimation. Reasonable candidates for such study, except vana­
dium, are other BCC metals, such as tantalum, niobium and iron.
Declaration of Competing Interest
We wish to confirm that there are no known conflicts of interest
associated with this publication and there has been no significant
financial support for this work that could have influenced its outcome.
We confirm that the manuscript has been read and approved by all
named authors and that there are no other persons who satisfied the
criteria for authorship but are not listed. We further confirm that the
order of authors listed in the manuscript has been approved by all of us.
We confirm that we have given due consideration to the protection of
intellectual property associated with this work and that there are no
impediments to publication, including the timing of publication, with
respect to intellectual property. In so doing we confirm that we have
followed the regulations of our institutions concerning intellectual
property.
We understand that the Corresponding Author is the sole contact for
the Editorial process (including Editorial Manager and direct commu­
nications with the office). She is responsible for communicating with the
other authors about progress, submissions of revisions and final
approval of proofs. We confirm that we have provided a current, correct
email address which is accessible by the Corresponding Author and
which has been configured to accept email from (louisa@bgu.ac.il (for
LM).
Acknowledgements
Financial supports from the Israel Science Foundation (grant 441/
18) to E.B. Zaretsky and N. Frage, and the Israeli Ministry of Defense
(grant 8757643) to E.B. Zaretsky are gratefully acknowledged.
References
[1] T.G. Lindley, R.E. Smallman, The plastic deformation of polycrystalline vanadium
at low temperatures, Acta Metall. 11 (5) (1963) 361–371, https://doi.org/
10.1016/0001-6160(63)90161-5.
[2] J. Bressers, M. Heerschap, P. de Meester, Deformation properties of vanadium
single crystal, J. Less Common Metals 22 (3) (1970) 321–326, https://doi.org/
10.1016/0022-5088(70)90082-2.
[3] Gui Li-Jiang, Liu Yue-Lin, Wei-Tian Wang, Zhang Ying, Lü Guang-Hong, Yao Jun-
En, Effects of chromium on structure and mechanical properties of vanadium: a
first-principles study, Chinese Physics B 22 (106109) (2013), https://doi.org/
10.1088/1674-1056/22/10/106109.
[4] Lin H. Yang, MeijieTang, A. John, Moriarty, Chapter 92: dislocations and plasticity
in bcc transition metals at high pressure, Dislocations in Solids 16 (2010) 1–46,
https://doi.org/10.1016/S1572-4859(09)01601-5.
[5] B.A. Loomis, Brittle-Ductile Transition in Vanadium, Iova State University,
Retrospective Theses and Dissertations, 1958. https://lib.dr.iastate.edu/rtd/2258.
[6] W.R. Clough, A.S. Pavlovic, The flow, fracture, and twinning of commercially pure
vanadium, Transactions of the American Society for Metals 52 (1960) 948–970.
[7] J.W. Edington, T.C. Lindley, R.E. Smallman, Strain-ageing of vanadium, Acta
Metall. 12 (9) (1964) 1025–1031, https://doi.org/10.1016/0001-6160(64)90074-
4.
[8] R.W. Thompson, O.N. Carlson, Effect of nitrogen and carbon on the low-
temperature embrittlement of vanadium, J. Less Common Metals 9 (5) (1965)
354–361, https://doi.org/10.1016/0022-5088(65)90117-7.
[9] G.R. Gathers, Hugoniot measurements for vanadium, J. Appl. Phys. 59 (1986)
3291–3293, https://doi.org/10.1063/1.336877.
A. Hazan et al.
[10] R. Rebonato, D.O. Welch, New features of the core structure of screw dislocations
in b.c.c. transition metals using non-local potentials, Phil. Mag. A 60 (6) (1989)
649–665, https://doi.org/10.1080/01418618908212009.
[11] S. Nemat-Nasser, W. Guo, High strain-rate response of commercially pure
vanadium, Mech. Mater. 32 (4) (2000) 243–260, https://doi.org/10.1016/S0167-
6636(99)00056-3.
[12] T.D. Joseph, M. Tanaka, A.J. Wilkinson, S.G. Roberts, Brittle–ductile transitions in
vanadium and iron–chromium, J. Nucl. Mater. 367–370 (A) (2007) 637–643,
https://doi.org/10.1016/j.jnucmat.2007.03.077.
[13] S. Min Han, T. Bozorg-Grayeli, J.R. Groves, W.D. Nix, Size effects on strength and
plasticity of vanadium nanopillars, Scripta Mater. 63 (12) (2010) 1153–1156,
https://doi.org/10.1016/j.scriptamat.2010.08.011.
[14] A. Dilawar, M. Nasreen, M.Z. Butt, Investigation of active slip-systems in some
body-centered cubic metals, J. Mater. Sci. 46 (11) (2011) 3812–3821, https://doi.
org/10.1007/s10853-011-5295-0.
[15] Yuying Yu, Ye Tan, Chengda Dai, Xuemei Li, Yinghua Li, Qiang Wu, Hua Tan,
Phase transition and strength of vanadium under shock compression up to 88 GPa,
Appl. Phys. Lett. 105 (2014) 201910, https://doi.org/10.1063/1.4902374.
[16] G.I. Kanel, S.V. Razorenov, G.V. Garkushin, A.S. Savinykh, E.B. Zaretsky, Stress
relaxation in vanadium under shock and shockless dynamic compression, J. Appl.
Phys. 118 (2015), 045901, https://doi.org/10.1063/1.4927613.
[17] J.M. Foster, A.J. Comley, G.S. Case, P. Avraam, S.D. Rothman, A. Higginbotham, E.
K.R. Floyd, E.T. Gumbrell, J.J.D. Luis, D. McGonegle, N.T. Park, L.J. Peacock, C.
P. Poulter, M.J. Suggit, J.S. Wark, X-ray diffraction measurements of plasticity in
shock-compressed vanadium in the region of 10–70 GPa, J. Appl. Phys. 122 (2017),
025117, https://doi.org/10.1063/1.4994167.
[18] Yan Lu, Xinyu Shu, Xiaozhou Liao, Size effect for achieving high mechanical
performance body-centered cubic metals and alloys, Sci. China Materials 61 (12)
(2018) 1495–1516, https://doi.org/10.1007/s40843-018-9313-2.
[19] R. Creten, J. Bressers, P. Meester, Anomalous slip in high-purity vanadium crystals
deformed in compression, Mater. Sci. Eng. 29 (1) (1977) 51–53, https://doi.org/
10.1016/0025-5416(77)90145-8.
[20] R. Gröger, Z. Chlup, T. Kuběnová, Deformation twinning in vanadium single
crystals tested in compression at 77 K, Mater. Sci. Eng. A 737 (8) (2018) 413–421,
https://doi.org/10.1016/j.msea.2018.09.030.
[21] A. Ojha, H. Sehitoglu, Twinning stress prediction in bcc metals and alloys, Phil.
Mag. Letters 94 (10) (2014) 647–657, https://doi.org/10.1080/
09500839.2014.955547.
[22] E.B. Zaretsky, G.I. Kanel, Tantalum and vanadium response to shock-wave loading
at normal and elevated temperatures. Non-monotonous decay of the elastic wave in
vanadium, J. Appl. Phys. 115 (2014) 243502, https://doi.org/10.1063/
1.4885047.
[23] W.C. Leslie, Microstructural effects of high strain rate deformation, in: R.W. Rohde,
B.M. Butcher, J.R. Holland, C.H. Karnes (Eds.), Metallurgical Effects at High Strain
Rates, Plenum Press, New York – London, 1973, pp. 571–586, https://doi.org/
10.1007/978-1-4615-8696-8.
[24] L.E. Murr, E.V. Esquivel, Observations of common microstructural issues associated
with dynamic deformation phenomena: twins, microbands, grain size effects, shear
bands, and dynamic recrystallization, J. Mater. Sci. 39 (2004) 1153–1168, https://
doi.org/10.1023/b:jmsc.0000013870.09241.c0.
Materials Characterization 175 (2021) 111061
[25] L.M. Barker, R.E. Hollenbach, Laser interferometer for measuring high velocities of
any reflecting surface, J. Appl. Phys. 43 (1972) 4669–4675, https://doi.org/
10.1063/1.1660986.
[26] E.B. Zaretsky, G.I. Kanel, Evidence of ductile response of alumina ceramic under
shock wave compression, Appl. Phys. Lett. 81 (2002) 1192–1194, https://doi.org/
10.1063/1.1499992.
[27] P.S. DeCarli, M.A. Meyers, Design of uniaxial strain shock recovery experiments,
Chapter 22, in: M.A. Meyers, L.E. Murr (Eds.), Shock Waves and High-Strain-Rate
Phenomena in Metals, 1980, pp. 341–373, https://doi.org/10.1007/978-1-4613-
3219-0.
[28] R. Vignjevic, K. Hughes, T. De Vuyst, N. Djordjevic, J.C. Campbell, M. Stojkovic,
O. Gulavani, S. Hiermaier, Lagrangian analysis led design of a shock recovery plate
impact experiment, Int. J. Impact. Eng. 77 (2015) 16–29, https://doi.org/10.1016/
j.ijimpeng.2014.11.002.
[29] A. Kazakov, N. Luong, E. Kazakova, E. Zorina, Thixomet image analyzer for
characterization of 2D and 3D materials structure, Microstruct. Sci. 27 (2000)
133–142.
[30] A. Kazakov, N. Luong, Characterization of semisolid materials structure, Mater.
Charact. 46 (2001) 155–161, https://doi.org/10.1016/S1044-5803(01)00118-8.
[31] G.I. Kanel, S.V. Razorenov, V.E. Fortov, Shock-Wave Phenomena and the
Properties of Condensed Matter, Springer, New York, 2004, https://doi.org/
10.1007/978-1-4757-4282-4.
[32] D.B. Hayes, Polymorphic phase transformation rates in shock-loaded potassium
chloride, J. Appl. Phys. 45 (3) (1974) 1208–1217, https://doi.org/10.1063/
1.1663391.
[33] L.C. Chhabildas, J.R. Asay, Rise-time measurements of shock transitions in
aluminum, copper, and steel, J. Appl. Phys. 50 (4) (1979) 2749–2756, https://doi.
org/10.1063/1.326236.
[34] G.R. Gathers, Hugoniot measurements for vanadium, J. Appl. Phys. 59 (1986)
3291–3293, https://doi.org/10.1063/1.336877.
[35] R. Faules, R.F. Williams, Plane stress waves propagation in solids, J. Appl. Phys. 41
(1) (1970) 360–363, https://doi.org/10.1063/1.1658348.
[36] M.A. Shtremel, Strength of Alloys. Part 2. Deformation, (in Russian) MISiS,
Moscow, 1997. ISBN 5–87623–015-4.
[37] M.N. Hasan, Y.F. Liu, X.H. An, J. Gu, M. Song, Y. Cao, Y.S. Li, Y.T. Zhu, X.Z. Liao,
Simultaneously enhancing strength and ductility of a high-entropy alloy via
gradient hierarchical microstructures, Int. J. Plast. 123 (2019) 178–195, https://
doi.org/10.1016/j.ijplas.2019.07.017.
[38] J.A. Venables, The nucleation and propagation of deformation twins, J. Phys.
Chem. Solids 25 (7) (1964) 693–700, https://doi.org/10.1016/0022-3697(64)
90178-7.
[39] M.A. Meyers, O. Vöhringer, V.A. Lubarda, The onset of twinning in metals: a
constitutive description, Acta Mater. 49 (2001) 4025–4039, https://doi.org/
10.1016/S1359-6454(01)00300-7.
[40] I.J. Beyerlein, C.N. Tome, A dislocation-based constitutive law for pure Zr
including temperature effects, Int. J. Plast. 24 (2008) 867–895, https://doi.org/
10.1016/j.ijplas.2007.07.017.
[41] G.E. Duvall, Propagation of plane shock waves in a stress-relaxing medium, in:
H. Kolsky, W. Prager (Eds.), Stress Waves in Anelastic Solids, Springer-Verlag,
Berlin, 1964, pp. 20–32, https://doi.org/10.1007/978-3-642-88288-3_2.