Original Contributions: The Softening Factor C of Commercial Titanium Alloy Wires

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International Journal of
MATERIALS RESEARCH

Zeitschrift für METALLKUNDE

Original Contributions
A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

A.F. Jankowskia , J.M. Chamesa , A. Gardeaa , R. Nishimotoa , E.M. Branniganb


a Sandia National Laboratory, Livermore, CA USA
b Los Alamos National Laboratory, Los Alamos, NM USA

The softening factor cb of commercial titanium


alloy wires

tions [5, 6] than other implant materials. However, a low


The strain-rate sensitivity exponent m and activation volume wear resistance coupled with the motion of implants relative
t* are often used to characterize the strain-rate sensitivity of to the implant site implies [7] deficient in-service lifetimes
strength behavior in metals and alloys. Complications can [8] as observed for total hip implants. Although oxide and ni-
arise when the m and t* values become indeterminate, due tride coatings both increase surface hardness and improve
to factors such as an inherent scatter in the mechanical prop- corrosion resistance, Ti-implants remain at risk of tensile
erty data. The study of commercial Ti-alloy wires is consid- failure, or rejection by the body during osseo-integration
ered wherein to overcome this limitation, the formulation of when bone grows around the alloy implant. The use of nio-
the Kocks–Mecking (K–M) model is modified to provide a bium (Nb) as a solute addition is reported [9, 10] to enhance
parameter cb that characterizes the microstructural scale re- biocompatibility in comparison to Ti-6Al-4V alloy due to
sponsible for the observed plasticity and work hardening be- decreased toxicity and allergic reactions [11]. Beyond qua-
havior. The softening factor cb is found to be independent of si-static tensile testing [12], the strain-rate sensitivities of
strain-rate for the Ti-alloy wires of this study. It is proposed commercial Ti, Ti-6Al-4V, and Ti-6Al-7Nb wires have re-
that cb can offer a versatile and complementary computation ceived relatively little attention. Higher strain-rate loading
to the activation volume t* since its formulation includes the conditions from 10–3 to 102 s–1 are of interest [13, 14] for bio-
yield and ultimate strength values along with the plastic medical applications. Thus, the assessment of strain-rate de-
strain. For the tensile testing of Ti-alloy wires, a low cb-value pendent strength for commercial-grade biocompatible Ti al-
of 14 is calculated for Ti-6Al-4V that is consistent with >10 % loys is of practical interest [15] for improved reliability and
plasticity during work hardening whereas a high cb-value of longer life of both orthopedic and dental implants. For this
135 for Ti-6Al-7Nb corresponds with <4 % plasticity. purpose, the assessment of strength behavior for biocompati-
ble Ti-alloys as a function of strain rate is pursued through
Keywords: Softening factor; Work hardening; Plastic the tensile testing of commercially available spooled wire.
strain; Ti alloys It is anticipated that complications may arise in the computa-
tional analysis of the strain-rate sensitivity exponent m and
activation volume t* as formulated from continuum models
1. Introduction due to an inherent variability of the wire material and appar-
ent scatter in stress–strain results.
Titanium (Ti) alloys are used in the aerospace, marine, The classic use of the Kocks–Mecking (K–M) model
chemical, athletic, and biomedical industries [1]. The quasi- [16] provides an understanding of the work hardening rate
static mechanical properties of grade 5 Ti-6Al-4V are similar of materials that undergo extensive plastic deformation.
to those of bone with excellent osseo-integration compatibil- The stress–strain relationship from mechanical tests can be
ity [2 – 4]. In addition, Ti alloys cause fewer allergic reac- replotted in a different form. Specifically, a K–M plot de-

990 Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

picts the variation of work hardening rate H, i. e. dr/de, with


stress r where the work-hardening is evaluated at specific
conditions of temperature and strain rate. Often, and of spe-
cific interest, are the progressive stages of plasticity that are
observed, during homogeneous deformation, prior to local-
ization. Here, a K–M plot may result [14, 16] with the ap-
pearance of a decrease in the work hardening rate in three
distinct stages, i. e. III–IV–V. Recent applications of the
K–M model include the assessment of work hardening be-
havior in Cr–Mo steel [17] and the evaluation of strain
hardening to determine dynamic recrystallization [18].
Although numerous constitutive models have been devel-
oped to replicate the plasticity behavior, the formulation of
an activation volume for the onset of plasticity is not ad-
dressed, as noted above. Starting with the K–M model,
Morris Jr. has developed [19] a formalism for the operative Fig. 1. A Considère plot of the stress r versus strain e behavior (red
scale of microstructure during work hardening as identified curve) that provides the relationship with slope dr/de, i. e. of the dashed
by the structural softening factor cb. The tensile testing of curve, in Eq. (5).
commercial Ti-alloy wires is pursued across four-orders of
magnitude in strain rate that enter the lower range of condi- the Hall–Petch equation which relates ry to grain size hg as
tions of interest for biomedical application. The conditions
selected for this study will suffice to benchmark the use of ry ¼ ro þ Ky  hg 1=2 ð1Þ
a 3-variable input to uniquely determine a structural scaling
factor cb that proves indeterminate using fewer variables. where Ky is the Hall–Petch slope. Similarly, the cleavage
The yield strength, plastic strain, and ultimate strength are fracture stress rf for high-strength steels can be expressed as
now used to determine a characteristic softening factor cb rf ¼ Kf  hg 1=2 ð2Þ
to the microstructure, and its dependence on strain-rate.
An equation used for predicting the ductile–brittle transi-
2. Morris, Jr. modification of Kocks–Mecking tion temperature TB is expressed as
formulation
TB ¼ To  KB  hg 1=2 ð3Þ
An approach to increase the strength of an alloy is through
the thermal evolution of its microstructure. Heat treat- If the strength is assumed to be a linear function of tempera-
ments are used to selectively evolve a strengthening preci- ture, then the coefficient KB governs the ductile–brittle tran-
pitate-phase from a homogeneous alloy. The precipitate sition. KB is derived after subtracting Eq. (1) from (2), solv-
particle may be coherent or incoherent with its matrix ing for hg–1/2, and then substituting into Eq. (3) as
phase as dependent upon the processing method. An engi-
KB ¼  Kf  Ky  ðdr=dTÞ1

neering application for structural materials is found for ð4Þ
the case of ultra-high strength steels [19 – 23], i. e. the case
for supersteels. A method to process inexpensive, low-al- The coefficient KB is positive when Ky > Kf, as is the case
loy steels to very-high strength is to refine microstructure for iron. The ultimate tensile strength ru is found in the
by incoherent phase transformations as, e. g., by applica- stress–strain diagram of Fig. 1 at the location where neck-
tion of thermo-mechanical controlled processing (TMCP) ing begins to occur. In the Considère criterion for determin-
during the austenite–ferrite transformation on cooling. ing tensile strength, a point on the true stress–true strain
The presence of incoherent precipitate particles permits curve is graphically located that has a sub-tangent of unity.
the matrix to deform plastically while maintaining its in- That is, r = ru when
herent ductility. Nanostructures in pure supersteels are un-
likely since ultra-high strength via an ultra-refined grain dr=de ¼ r=ð1 þ eÞ ð5Þ
size is not likely without an extreme loss of ductility. The onset of plastic instability occurs as the rate of speci-
However, it can be shown that metallurgical approaches men thinning exceeds the rate of strain hardening, i. e. when
to mitigate limited ductility are available through the use
of multiphase or metastable microstructures. To this end, dr < ð1 þ eÞ ð5aÞ
a modified K–M model as developed by Morris, Jr. [19]
considers the size effects present to optimize strength for By taking the differential of Eq. (5a) with respect to de
the case of incoherent fine-grained ferrite. A structural pa-
rameter cb, i. e. a softening factor, is formulated through dr=de < 1 ð5bÞ
use of the yield strength ry, ultimate strength ru, and the The useful tensile ductility of a specimen is its uniform
plasticity ep of the alloy. The inclusion of these three pa- elongation, that terminates with the onset of necking, i. e.
rameters can provide further insight into plastic deforma- the plastic instability which occurs at the ultimate strength
tion, in addition to or in lieu of the computation [24] of
ru. The ultimate strength is determined in a test on a cylind-
an activation volume t*.
rical specimen by the true stress r, and the work hardening
The equations (1–10) that follow for the modified K–M
function H that equals dr/de according to the Considère
model are formulated [19] beginning with consideration of

Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11 991


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

criterion as loy structures as well. The experimental measurement of


ry, ru, and ep allows for the determination of whether or
Hu ¼ ½dr=deu ¼ ru ð6Þ not the underlying structural parameter, i. e. the softening
factor cb, is invariant with the applied strain rate.
The true strain e at the instability point is determined by
evaluating the integral from ry to ru, that’s given by the ex-
3. Experimental methods
pression
Z The materials used in the tensile experiments were pure
e¼ ðde=drÞ  dr ð7aÞ Ti (0.994 purity), Ti-6Al-4V (grade 5), and Ti-6Al-7Nb weld-
ing wires as-received in spool form. The pure Ti and Ti-6Al-
After substituting Eq. (6) into Eq. (7a), an expression for e 4V wires were hot drawn, whereas the Ti-6Al-7Nb wire was
is then cold drawn. Metallographic samples were prepared in direc-
Z tions both along (axial) and transverse (radial) to the 1.0–
e¼ ½1=HðrÞ  dr ð7bÞ 1.2 mm diameter wire axis. A 0.5 lm colloidal diamond sus-
pension was used to produce the final polished surface. The
materials were examined using a Rigaku Miniflex for X-ray
The work hardening function H (r) for many metals and al- diffraction (XRD) analysis, a JEOL JSM7600F scanning elec-
loys is described by a linear equation of the K–M form, as tron microscopy (SEM), and a JEOL JXA8200 electron-probe
micro-analyzer (EPMA). The samples were tested in tension
H ¼ H o  cb  r ð8aÞ
over a range of strain rates produced using timed displacement
where Ho is a constant, and cb is the softening factor param- of crosshead beams in a Test ResourcesTM universal tester.
eter. Rewriting Eq. (8a) to solve for Ho at r = ru, noting the XRD scans of polished axial and radial surfaces of each
equivalence of Eq. (6), it is found that material were conducted using a diffractometer operated in
the h/2h mode with monochromatic CuKa radiation as gen-
H o ¼ H þ cb  r ð8b:1Þ erated at 30 kV/20 mA. The XRD scans were collected over
a 2h-range of 308–908 using a Dh increment of 0.058 and
2 s dwell-time interval. The scans revealed the crystalline
Ho ¼ Hu þ c b  ru ð8b:2Þ
Bragg reflections of the constituent alloys, the presence of
texturing along the drawn wire axis, and the possible pre-
H o ¼ ru þ c b  ru ð8b:3Þ sence of multiple phases.
The microstructural features of the samples were revealed
The work hardening function H is determined from from the axial and radial surfaces with the secondary-electron
Eqs. (8a) and (8b.3) as imaging mode of an SEM. The low-angle, secondary-electron
detector (below-the-lens) imaging (LEI) mode enhanced sur-
H ¼ ru þ cb  ðru  rÞ ð8cÞ
face relief from the polished samples that were treated using
For the case of an incoherent fine-grained ferrite, it’s as- a low-contrast, Kroll’s etchant – a dilute acid solution of 6 %
sumed that the hardening behavior is approximated by a nitric and 2 % hydrofluoric as swabbed onto each sample sur-
single constitutive equation since there are no competing face for 10–15 s. A mean linear-intercept calculation was
effects from the microstructure. By substituting Eq. (8c) used to determine the average size of the constituent micro-
into Eq. (7b), the strain e is derived from ri to ri as a func- structure. The size calculation can include a shape factor
tion of the reduced stress r* as since the grains are assumed to be a geometric variant of
spheres–to–cubes. The elemental composition of each alloy
e ¼ ð1=cb Þ  lnf½1þ cb  ð1 ri  Þ=½1þ cb  ð1 ri  Þg ð9Þ was determined both by energy dispersive spectroscopy
(EDS) with the SEM using characteristic X-rays, and by wa-
where r* = r/ru. The true strain ep, from the yield point to velength dispersive spectroscopy (WDS) with a EPMA.
the instability, can then be determined by evaluating the so- The mechanical properties were determined using ten-
lution to the integral from ry to ru, as sile test wire samples each 250 mm in length. The dia-
meters of each Ti, Ti-6A-4V, and Ti-6Al-7Nb wire were
ep ¼ ð1=cb Þ  ln½1 þ cb  ð1  ry  Þ ð10Þ measured where nominal values were 1.19 mm, 0.88 mm,
where ri* = ri /ru. In general, the observed trend is that as and 1.02 mm, respectively. The wire samples were tensile
r* approaches one, the corresponding value for eu goes to mounted according to ASTM standards using a wire spool
zero. This is a boundary condition, i. e. r* equals one when grip to produce a gage length of 92–122 mm. Loading oc-
curs over a strain rate range of 10–5 to 10–1 s–1. To achieve
ru = ry and Eq. (10) gives a corresponding value of zero for
this range, a nominal total displacement of 24 mm was ap-
ep equaling (1/cb) · ln[1]. Again, ep represents the amount of
plied over time intervals that range from 5 to 4 000 s.
plastic strain between the yield point and ultimate strength.
These values were consistent with limits for the minimum
With respect to application of nanostructured supersteels,
and maximum velocities of the tensile test instrument.
the optimal dual-phase structure [19] for enhanced strength
Tensile testing was used to determine the plastic strain ep,
and plasticity could be composed of small martensitic is-
yield stress ry, and ultimate strength ru from measure-
lands intermixed with incoherent ferrite. Although the mod- ments of load P, initial wire diameter, gage length, and
ified K–M model is developed for determining the soften- displacement of the wire during loading. A linear regres-
ing factor of two-phase alloys, there is no exclusion that sion analysis was used to isolate the elastic loading re-
prohibits application to the plastic behavior of complex al- gime. For consistency with the modified K–M model, it

992 Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

was considered that the wire begins to yield at the propor- structure and the appearance of precipitate phases. Each sam-
tional limit – to permit full measurement of plasticity dur- ple was viewed along the axial and radial directions, as
ing work hardening. Once the non-linear behavior began, shown in Fig. 2. The pure Ti wire has an elongated grain
the measure of plastic strain to failure was recorded. structure in the Fig. 2a axial view, and a refined grain struc-
ture in the Fig. 2d orthogonal, radial view. Particles are pres-
4. Experimental results and analysis ent that could be attributed [25 – 27] to a Ti-hydride and/or
impurity-stabilized b-phase. A primary a-phase structure is
The microstructure and composition of each wire material seen in Fig. 2b and e Ti-6Al-4V and Fig. 2c and f Ti-6Al-
were examined using X-ray diffraction and electron micro- 7Nb samples as was found in prior studies [28, 29]. An esti-
scopies. Tensile testing was used to determine the value mate is made for the grain size hg of the matrix without the
for the softening factor cb. Comparison of cb with the acti- shape factor since the true shape geometry of the grains is un-
vation volume for plastic deformation was made along with known. The radial images were measured to provide mean
its variation with the strain-rate. linear-intercept hg values of: 1.1 ± 0.1 lm for the elongated
structure of pure Ti; 3.1 ± 0.3 lm for the equiaxed structure
of Ti-6Al-4V; and 1.9 ± 0.2 lm for the slightly elongated
4.1 Structure and Composition
structure of Ti–6Al–7Nb. Microstructures similar to the
SEM micrographs were obtained in the LEI imaging mode cold-drawn condition observed in Fig. 2b and e are found
using a working distance of 8 mm, and a 5 keV incident elec- [25, 26] in forged samples. Surface relief is evident with a
tron beam. The LEI mode enhanced definition of the grain second particulate phase at, or near, the grain boundaries.

Fig. 2. Scanning electron micrographs of the Ti, Ti-6Al-4V, and Ti-6Al-7Nb alloy wires as imaged in the LEI mode along the (a–c) axial, and (d–f)
radial sections, respectively.

Table 1. Weight % analysis of the Ti-alloy wires from EDS and WDS analysis.

X-ray line Ti-6Al-4V Ti-6Al-7Nb

matrix particle matrix particle

WDS EDS EDS WDS EDS EDS

Ti-Ka1 89.20 92.9 82.5 85.80 86.4 74.1


Al-Ka1 6.30 3.4 2.6 6.27 6.2 4.7

V-Ka1 4.45 3.7 14.1 0.25 – –

Nb-La1 – – – 7.41 7.4 18.2

Fe-Ka 0.05 – 0.8 0.27 – 3.0

Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11 993


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

For example, b-precipitates are seen [30] at grain boundaries ing along the axial direction is evident in the XRD scan of
in a primary (90 %) a-phase matrix for Ti-6Al-4V heated to Fig. 3. Additional reflections in Fig. 1 for the pure Ti wire
550 8C, held at temperature, and then slow cooled. Similar match those reported [32, 33] for the a-phase, where the
images with a more-refined grain structure are seen in peak positions are computed using lattice parameters
images of the Ti-6Al-7Nb alloy wire, Fig. 2c and f. a = 0.2952 nm and c = 0.4681 nm. The XRD scan from the
Composition analysis of the matrix and particulate phases, radial direction has a (10.0) texture, complementary to the
as seen in Fig. 2e and f was first conducted using EDS analy- (00.2) texturing found for the axial scan.
sis. The characteristic X-ray peaks up to 10 keV were col- The addition of alloying elements as Al, V, and Nb to the
lected as emitted from the matrix and particle phases. The a-phase of Ti can produce multiple phases and slightly
X-ray peaks of interest used in the analysis were the change [25, 34 – 37] the lattice parameters of the a-phase
1.49 keV Al-Ka1, 2.17 keV Nb-La1, 4.51 keV Ti-Ka1, and to a = 0.292–0.293 nm and c = 0.466–0.472 nm. The possi-
4.95 keV V-Ka1. The weight percent values are listed in Ta- ble increase in c and slight decrease in a for the a-phase Ti
ble 1 as computed using corrected intensities of the charac- alloy wires will tend to shift the (00.2) peak to a lower 2h
teristic X-rays. A measured precision of ±0.5 wt.% occurs position, and increase the 2h position of the (20.1) peak,
for this EDS analysis. It is seen that the Al content is slightly both of which are seen in Fig. 3 when comparing the alloy
less in the matrix than the nominal value for the Ti-6Al-4V to pure Ti scans. In addition, the presence of a face-cen-
wire. In general, X-ray composition maps of the Ti-6Al-4V tered-cubic (fcc) Ti(Al) c-phase is reported [38 – 41] for na-
and Ti-6Al-7Nb second phase particulates indicate a diffuse nocrystals and severely plastically-deformed, ball-milled
enhancement of V and Nb, respectively, that may be evi- powders. The position of the c-phase (111) and (200) re-
dence for b-segregation [26]. In addition, the presence of flections in Fig. 3 are computed using a lattice parameter
characteristic 0.62 keV L111l, 0.71 keV L111ab, 0.72 keV a = 0.409 nm [38, 40], whereas a 0.440 nm value gives a
L11ab, 6.40 keV Ka, and 7.06 keV Kb1 peaks for Fe are found (111) reflection at a 2h position of 44.28. Alternatively, the
in the EDS spectra from isolated particles. These EDS wt.% 44.28 peak position can be fitted to a common Ti-hydride
composition values listed in Table 1 are consistent with prior phase. The peak positions for a body-centered-cubic (bcc)
WDS microprobe measurements [31] of a- and b-phases in a b-phase in the Ti-6Al-4V [37] and Ti-6Al-7Nb [34] alloy
(grade 5) Ti-6Al-4V alloy, where the matrix was found to be wires are shown in Fig. 3 as they would appear using a lat-
6.7 wt.%Al-1.4 wt.%V and the particles were 2.9 wt.%Al- tice parameter a = 0.329 nm. No distinct b-phase peaks are
15.4 wt.%V-1.3 wt.%Fe. The present WDS measurements observed in the XRD scans of Fig. 3, except possibly a very
of composition are taken from matrix areas of polished (but diffuse (110) reflection.
not etched) wire cross-sections – where 5 are from the radial,
and 10 are from the axial sections of each sample. A statisti-
cal difference was not found between the composition values 4.2 Mechanical properties
of the radial and axial sections. A precision of ±0.04 wt.% A single wire tensile test contains regions that include: an
was measured for the WDS analysis. The WDS composition initial nonlinear, pre-loading range where the wrapped ends
values listed in Table 1 appear equivalent to the nominal val- of the wire are brought under tension to remove slack; a lin-
ues of each wire material. In addition, WDS measurements ear loading range of Hookean elastic behavior; and a plastic
of the pure Ti wire reveal an average impurity composition deformation range where yielding and strain hardening oc-
of 0.09 wt.%Al-0.30 wt.%V-0.02 wt.%Nb-0.05 wt.%Fe. cur until failure. The logarithmic variation of change in
The Ti wire is a polycrystalline, hexagonal close-packed yield strength ry with increasing strain rate is used to deter-
(hcp) structure, i. e. the a-phase. Basal plane (00.2) textur- mine the coefficient m for strain-rate sensitivity through the

Fig. 3. X-ray diffraction scans in h/2h mode


of the Ti, Ti-6Al-4V, and Ti-6Al-7Nb alloy
wires as examined in the axial and radial sec-
tions.

994 Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

Dorn relation. The yield strength will vary due to several


factors that include surface finish and grain size, i. e. the
Hall–Petch effect. However, specific effects of grain size
and surface finish are not considered in this analysis. A typ-
ical tensile load P versus displacement z curve is shown in
Fig. 4 for a 1.19 mm dia. pure Ti wire as tested at a strain
rate of 1.19 · 10–2 s–1. The Fig. 4 load–displacement P–z
data is plotted that includes some of the initial pre-loading
regime. The dashed-linear (red) curves are used to extrapo-
late the position of the origin (i. e. zero elastic displace-
ment); and determine the proportional yield limit Py, the ul-
timate strength Pu, and the amount of plastic strain.
Tensile test results of representative samples for each
wire material are shown in the Fig. 5 stress–strain plots with
corresponding strain rates indicated in the legend. The top
curve set is for Ti-6Al-7Nb, the middle set is for Ti-6Al-
4V, and the bottom curve set is for pure Ti. The yield point
Fig. 4. A load P–displacement z curve for the tensile testing of a pure is determined using the proportional limit, rather than offset
Ti wire using a strain rate of 1.19 · 10–2 s–1.
method, since the effects of work-hardening are significant
for the wire tests. The tensile strengths measured are: 570–
680 MPa for commercially pure Ti; 710–830 MPa for the
Ti-6Al-4V alloy; and 850–1 070 MPa for the Ti-6Al-7Nb
alloy. The amount of plastic strain is reduced from greater
than 0.10 for the Ti and Ti-6Al-4V wires, to less than 0.04
for Ti-6Al-7Nb. In general, the Fig. 5 stress–strain plots
show that the yield strength ry increases slightly with in-
creasing strain rate. Limited ductility is expected and found
for the cold drawn, i. e. Ti-6Al-7Nb, wire material.
An alternative means to represent the stress–strain results
for the Ti-alloy wire tensile tests is through the use of a
K–M plot. The representative curves in Fig. 6 are plotted
from several stress–strain curves of Fig. 5. The stress range
shown in Fig. 6 is plotted as it begins with a rapid decrease
in the coefficient H equaling dr/de for the work hardening
rate. A progressive decrease in the slope of the Fig. 6 curves
is found through a succession of approximately linear re-
gions. The three classic K–M work hardening stages are
found for the Ti-6Al-4V curve in Fig. 6 for the test conducted
Fig. 5. Stress r (MPa) versus strain e (mm · mm–1) curves plotted for at a 4.57 · 10–2 s–1 strain rate. These linear regions corre-
the tensile test results of Ti-6Al-7Nb, Ti-6Al-4V, and pure Ti wires. spond to applied stress levels up to 850 MPa for stage III,
from 850 to 975 MPa for stage IV, and from 975 MPa to
necking for stage V. The saturation stress is seen to increase
through III as the applied strain rate increases, i. e. the K–M
curve for a material shifts to higher stress with increasing
strain rate. The presence of at least stages III – IV appear for
the pure Ti wire. However, with its reduced plasticity, only
stage III is apparently observed for the Ti-6Al-7Nb wire, as
is reported elsewhere [18] for similar Nb-addition Ti–Al al-
loys. Stage III is associated with the trapping of dislocations,
whereas the saturation stress is a result of dislocation annihi-
lation. As for grade-1 pure Ti, in general, the transition from
the stage III – IV occurs at a few percent of plasticity, and
from stage IV to V beyond *10 %.
The effect of strain-rate sensitivity on strength is quanti-
fied using a classic continuum approach with the ln-scale
relationship of the Dorn equation, as
m ¼ dðln ry Þ=dðln e_ Þ ð11Þ

The data plots of ln e_ versus ln ry for all of the wire tensile


Fig. 6. A Kocks–Mecking plot of the variation of work hardening dr/
tests are shown in Fig. 7. The scatter in the data is anticipated
de (MPa) versus stress r (MPa) for several of the tensile test results in and is attributable to the variation in the samples cut from the
Fig. 5 for the pure Ti, Ti-6Al-4V, and Ti-6Al-7Nb wires. spool of wire material, i. e. the commercial grade wire materi-

Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11 995


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

als may have some inhomogeneity in structure including some


variations along the gage length in composition, diameter, sur-
face finish, and grain size. The mechanical behavior of the test
material is of interest with all of the inconsistencies therein,
since an objective is to determine whether or not the use of
the softening factor cb introduced in Eq. (8a) provides insight
to the scale of the underlying structure responsible for the
strain-rate dependent strength behavior. From the slope of
the linear curves in Fig. 7, the strain-rate sensitivity values
for the Ti and Ti-6Al-4V wires are positive with similar expo-
nents of mTi = 0.014 ± 0.006, and mTi6Al4V = 0.014 ± 0.008,
respectively. A near zero, i. e. perhaps a negative, exponent
mTi6Al7Nb of –0.008 ± 0.007 is computed for the full Ti-6Al-
7Nb data set with its inherent scatter in the tensile data.
The activation volume t* for the onset of plasticity can
be computed from the strain rate sensitive strength behavior
Fig. 7. The exponent m for the strain-rate sensitivity is the slope of the
using the following Cahn–Nabarro [24] relationship, as
linear-curve fit of the ln–ln plots for Ti-6Al-7Nb (top curve), Ti-6Al-
4V (middle curve), and pure Ti (bottom curve). t ¼ ðkB  T Þ  ½dðln e_ Þ=dðry Þ ð12Þ

At room temperature, the product of Boltzmann’s constant kB


and temperature T equals 4.142 · 10–21 J (or 4.142 MPa · nm3).
The activation volume t* is the product of kB · T with
the slope of linear curves plotted in Fig. 8 for r versus
ln. The values of t* computed for Ti and Ti-6Al-4V are
0.207 ± 0.117 nm3, and 0.230 ± 0.090 nm3, respectively.
These t* values correspond to 26 –29 dislocation volumes
(of b3) when assuming a typical Burger’s vector b equal to
0.2 nm. A value of t* for the Nb alloy is indeterminate using
eqn. (12) since q(ry) * 0 (hence mTi6Al7Nb * 0), i. e. there is
no statistical variation of strength ry with strain rate.
The modified K–M relationship provides a measurement,
in addition to t*, for evaluating the scale of the underlying
microstructure responsible for plasticity during tensile test-
ing. The softening coefficient cb is determined by fitting
Eq. (10) with measured values of the plastic strain, yield,
and ultimate strength using tensile test results such as those
shown in the Fig. 5 curves. The variation of cb with the strain
rate is plotted in Fig. 9. The cb-values are seen to be approxi-
Fig. 8. The activation volume t* is computed from the slope of the mately constant across the strain rate range used in these ten-
linear-curve fit to the yield strength variation with ln strain rate for
Ti-6Al-4V (middle curve), and pure Ti (left curve).
sile tests. The strain-rate invariant cb-values are evidenced by
the near-zero slope to the linear curve fit of versus cb for each
material. The constant cb value as a function of is analogous
to the constant value for the activation volume t*. Although
no activation volume was determined for Ti-6Al-7Nb from
the scattered data plot in Fig. 8, it is possible to determine a
cb-value using Eq. (10). The cb-values for pure Ti, Ti-6Al-
4V, and the Ti-6Al-7Nb wires are 19, 14, and 135, respec-
tively. The parameters computed for the strain-rate sensitiv-
ity factor m using Eq. (11), the activation volume t* using
Eq. (12), and the softening factor cb as fit using Eq. (10) are
listed for all of the wire materials in Table 2.

5. Discussion

The microstructures of the wires revealed in the analysis of


SEM images shown in Fig. 2 are consistent with an a-phase
matrix, and a dispersion of impurities that decorate grain
boundaries. The orthonormal XRD scans of Fig. 3 show
crystallographic texturing consistent with a wire-drawn
Fig. 9. The softening coefficient cb is plotted as function of the strain stock material. A refined grain size of a few microns in the
rate during wire tensile testing of Ti-6Al-7Nb (green data), Ti-6Al-4V microstructure results from wire drawing process as well.
(red data), and pure Ti (blue data). There is a V and Nb enrichment found in the particulates,

996 Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

Table 2. Parameters m, t*, and cb calculated for the Ti-alloy wires.

wire material strain-rate sensitivity factor m activation volume t* (nm3) softening factor cb

Ti 0.014 ± 0.006 0.207 ± 0.117 19


Ti-6Al-4V 0.014 ± 0.008 0.207 ± 0.117 14

Ti-6Al-7Nb –0.008 ± 0.007 0.230 ± 0.090 135

as measured using EDS and listed in Table 1 where the IV, until saturation of that particular system, as e. g.,
composition values are similar to those reported for microp- (10.0), occurs. Further twinning continues in stage V as de-
robe measurements of Ti-6Al-4V alloys [31]. formation shifts to a new system as, e. g., (11.0). Although
The wire is a commercial product that has inherent struc- the commercial wires for this study do not show the exten-
tural and composition variations which leads to an inherent sive plasticity reported for grade-1 pure Ti [43], these three
scatter in the range of tensile behavior for each type of stages are observed as seen in Fig. 6. The appearance of
material as seen in the data plots of Fig. 7 and 8. Specifically, multiple stages of work hardening is readily seen as well
the Ti-6Al-4V yield strength ranges from 710 – 830 MPa, for pure Ti in the stress–strain results of tensile tests at var-
and the Ti-6Al-7Nb wires have yield strengths of 850 – ious strain rates [42]. The tensile behavior of the Ti and
1 070 MPa. Tensile test results for the Ti-6Al-7Nb wires are Ti-6-4 wires is consistent with this reported behavior
consistent with an equiaxed a-phase microstructure [29] that wherein Stage III of the K–M behavior is associated with
has a concurrent strength of 910 – 980 MPa. The plasticity of the trapping of dislocations. In addition, the presence of
the hot-drawn pure Ti and Ti-6Al-4V wires exceeds 10 %, stages III and IV is reported [44] in a K–M plot for the work
whereas the cold drawn Ti-6Al-7Nb wires is less than 4 %. hardening behavior of Mg–Li alloys under tension. The
The limited ductility of the Ti-6Al-7Nb wires is consistent strain to failure of 6–16 % is not extensive but is similar to
with its cold-drawn processing versus the greater plasticity the commercial wires tested in the present study.
found for hot-drawn pure Ti and Ti-6Al-4V wires. Modeling efforts have evolved to further evaluate the strain
The strain rate sensitivity coefficients m computed using hardening rate effects in plastically deformed metal alloys be-
Eq. (11) for the Ti-alloy wires are low, as seen in Fig. 6, at yond the basic K–M formulation. Extension of the K–M mod-
less than 0.015 for all samples over a strain rate range el to include the dependence of solute concentration on cross
of 10–5-to-10–1 s–1. This behavior is typical for pure Ti and slip is considered in the hardening behavior of the Fe–Al alloy
Ti-6-4 with m values of 0 – 0.03 that can be computed [42] system under tension [45]. The interplay, i. e. coupling, be-
across each stage of work hardening. Activation volumes tween the edge and screw dislocation density at cell walls
t* of 26–29 (b3) dislocations are determined using Eq. (12) and within the cells, respectively, is used in modeling efforts
from a Cahn–Nabarro analysis [24] for the onset of plasti- to evaluate the dynamics of plasticity beyond stage III [42,
city in Ti-6Al-4V and pure Ti, respectively. However, the 46 – 48]. Edge dislocations climb in the cell walls whereas
t*-value is indeterminate for the Ti-6Al-7Nb data using screw dislocations undergo cross-slip within the cell interiors
Eq. (12) since q(ry) * 0. Despite this shortcoming, the mod- where the interplay between these two attributes is assumed
ified Morris, Jr. model [19] proves useful to evaluate the to occur under the same total strain rate. Efforts to develop
scale of microstructure responsible for plastic deformation. strain-hardening models for Ti–Al alloy behavior using K–M
The softening factor cb is computed using Eq. (10) as a func- plots [18] again evidence a sequence of deformation modes
tion of the yield strength ry, ultimate strength ru, and plastic similar to this study for Ti-6Al-7Nb alloy wires, wherein an
strain ep. A constant value for cb is revealed with respect to a initial rapid work hardening is observed. Whereas an extended
variation in strain rate for each wire material in the Fig. 9 range of plasticity beyond initial yielding is reported for the
data plots. The softening factor cb-values of 14, 19, and 135 hot deformation of Ti–Al alloys that have a complex micro-
are computed for Ti-6Al-4V, pure Ti, and Ti-6Al-7Nb, re- structure with multiple phases which undergo recrystallization
spectively. Although the SEM images of Fig. 2 show similar [18], this scale of behavior is not seen in Fig. 5 for the room-
microstructures, the lower cb value is consistent with a temperature testing of the hot-drawn, single-phase Ti-alloy
greater amount of work hardening and plasticity for wires of this study. The current model [19] is not intended to
Ti-6Al-4V. Conversely, rapid work hardening behavior is simulate the details of strain hardening wherein the evolution
observed for the Ti-6Al-7Nb alloy leading to its larger cb of deformation modes with applied stress evidence changing
value. This later result would indicate a greater t* value as mechanisms of dislocation-based deformation. The derivation
well, that would be consistent with a near zero value in the presented is intended to provide a scale for the microstructure
computation of m for Ti-6Al-7Nb, as shown in Fig. 7. in the coefficient cb that underlies the deformation behavior
The microstructure for the drawn wire would be consis- from yielding to the ultimate strength as evaluated at the plas-
tent with elongated grains, wherein cell interiors would tic instability using the Considère criterion. Whereas cb can be
have low dislocation density and the grain boundaries uniquely determined, a traditional approach to evaluate an ac-
would have high dislocation density. To assess deformation tivation volume for deformation proves problematic for the
mechanisms that are operative during plasticity, a K–M deformation behavior for the untreated, commercial Ti alloy
work hardening rate analysis is reported for measurements wires. The Morris, Jr. model [19] provides another method to
of grade-1 pure Ti under tension [43]. For tensile deforma- assess the work hardening behavior, and is capable of provid-
tion, the stage III with a rapid, continuous decrease in H ing a microstructural parameter cb that unifies the complex be-
has dislocation glide. This is followed by twinning in stage havior of Ti-alloy wires. The use of the Morris, Jr. model may

Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11 997


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

be particularly suitable for the assessment of the observed var- [10] E. Eisenbarth, D. Velten, M. Müller, R. Thull, J. Breme: Bioma-
iation [49] in mechanical behavior of alloys including Ti-6Al- ter. 25 (2004) 5705 – 5713. PMid:15147816;
DOI:10.1016/j.biomaterials.2004.01.021
4V produced by additive manufacturing wherein a character- [11] M. Semlitsch, F. Staub, H. Weber: Biomedizinische Technik/
istic microstructure may be identified through use of a param- Biomed. Eng. 30 (1985) 334 – 339.
eter as the cb-coefficient. DOI:10.1515/bmte.1985.30.12.334
[12] A.A. Salem, S.R Kalidindi, R.D. Doherty: Acta Mater. 51 (2003)
4225 – 4237. DOI:10.1016/S1359-6454(03)00239-8
6. Conclusions [13] D.R. Chichili, K.T. Ramesh, K.J. Hemker: Acta Mater. 46 (1998)
1025 – 1043. DOI:10.1016/S1359-6454(97)00287-5
A greater understanding of the microstructure associated [14] T.M. Wright, W.C. Hayes: Medical Biol. Eng. Comp. 14 (1976)
with the mechanical behavior of commercial Ti-alloy wires 671 – 680. DOI:10.1007/BF02477046
[15] R. Strietzel, A. Hosch, H. Kalbfleisch, D. Buch: Biomater. 19
is of interest for a variety of applications such as structural (1998) 1495 – 1499. DOI:10.1016/S0142-9612(98)00065-9
implant biomaterials. Analysis of the mechanical behavior [16] H. Mecking, U.F. Kocks: Acta Metall. 29 (1981) 1865 – 1875.
of commercially available Ti, Ti-6Al-4V, and Ti-6Al-7Nb DOI:10.1016/0001-6160(81)90112-7
wires is conducted for tensile tests conducted over strain [17] J. Christopher, B.K. Choudhary, M.D. Mathew, T. Jayakumar:
rates of 10–5–10–1 s–1 to further exploration of strength be- Mater. Sci. Eng’g. A 575 (2013) 119 – 126.
DOI:10.1016/j.msea.2013.03.044
haviors of interest. [18] M. Bambach, I. Sizova, S. Bolz, S. Weiß: Metals 6 (2016) 204 –
1. Yield strengths are measured that are material dependent 222. DOI:10.3390/met6090204
which vary from 570 to 1 070 GPa. The wide range of me- [19] J.W. Morris, Jr.: \Is there a future for nanostructured steel?", in
chanical behavior for each material type complicates con- 16th International Society for Offshore and Polar Engineering,
ISOPE Conf. Proc. (2007) pp. 2814 – 2818.
ventional evaluation, as by the parameters of the activation [20] J.W. Morris, Jr., C.S. Lee, Z. Guo: Iron Steel Instit. Jpn. Inter. 43
volume t* and the strain rate sensitivity coefficient m. (2003) 410 – 419. DOI:10.2355/isijinternational.43.410
2. The use of the modified K–M model proves successful [21] J.W. Morris, Jr.: Iron Steel Instit. Jpn. Inter. 48 (2008) 1063 –
for the evaluation of a strain-rate independent structural pa- 1070. DOI 10.2355/isijinternational.48.1063.
rameter – the softening factor cb, that provides insight to the DOI:10.2355/isijinternational.48.1063
[22] D.H. Shin, B.C. Kim, K.T. Park, W.Y. Choo: Acta Mater. 48
underlying scale of microstructure in these wires as com- (2000) 3245 – 3252. DOI:10.1016/S1359-6454(00)00090-2
puted using the yield ry and ultimate ru strength along with [23] J. Zhao, Z. Jiang: Prog. Mater. Sci. 94 (2018) 174 – 242.
the plastic strain eu during work hardening. DOI:10.1016/j.pmatsci.2018.01.006
3. Small cb values are consistent with greater plasticity and [24] J.W. Cahn, F. Nabarro: Philos. Mag. A 81 (2001) 1409 – 1426.
DOI:10.1080/01418610108214448
work hardening, whereas large values are consistent with ma- [25] D.B. Shan, Y.Y. Zong, T.F. Lu, Y. Lv, J. Alloys Compd. 427
terials that exhibit less plasticity and a rapid strain hardening (2007) 229 – 234. DOI:10.1016/j.jallcom.2006.02.058
behavior. In this study, a high cb-value of 135 is computed [26] R. Li, L. Riester, T.R. Watkins, P.J. Blau, A.J. Shih: Mater. Sci.
for Ti-6Al-7Nb that rapidly strain hardens with <4 % plastic Eng. A 472 (2008) 115 – 124. DOI:10.1016/j.msea.2007.03.054
[27] L.M. Gammon, R.D. Briggs, J.M. Packard, K.W. Batson, R. Boy-
strain, whereas a low cb-value of 14 is found for Ti-6Al-4V er, C.W. Domby: \Metallography and microstructures of titanium
that strain hardens with a greater ductility of 10 % plastic and its alloys", in: ASM Handbook Vol. 9 Metallography and
strain. Microstructure, ASM International, Metals Park, OH (2004)
pp. 899 – 917. DOI:10.31399/asm.hb.v09.a0003779
Sandia National Laboratories is a multi-mission laboratory managed and [28] M.P. Chávez-Díaz, M.L. Escudero-Rincón, E.M. Arce-Estrada,
operated by National Technology and Engineering Solutions of Sandia, R. Cabrera-Sierra: Materials 10 (2017) 445 – 1 – 10.
LLC., a wholly owned subsidiary of Honeywell International, Inc., for PMid:28772804; DOI:10.3390/ma10040445
the U.S. Department of Energy’s National Nuclear Security Administra- [29] P.C. Collins, B. Welk, T. Searles, J. Tiley, J.C. Russ, H.L. Fraser:
tion under contract DE-NA0003525. Los Alamos National Laboratory is Mater. Sci. Eng. A 50 (2009) 174 – 182.
operated by Los Alamos National Security LLC for the U.S. Department DOI:10.1016/j.msea.2008.12.038
of Energy’s NNSA under DOE contract DE-AC52-06NA25396. [30] R. Pederson: Microstructure and phase transformation of Ti-6Al-4V,
Licentiate thesis, Luleå Univ. Technol., Luleå, Sweden (2002) p. 21.
References [31] J.W. Elmer, T.A. Palmer, S.S. Babu, E.D. Specht: Mater. Sci.
Eng. A 391 (2005) 104 – 113. DOI:10.1116/1.2204926
[1] N. Poondla, T.S. Srivatsan, A. Patnaik, M. Petraroli: J. Alloys [32] H.R.Z. Sandim, B.V. Morante, P.A. Suzuki: Mater. Res. 8 (2005)
Compd. 486 (2009) 162 – 167. 293 – 297. DOI:10.1590/S1516-14392005000300012
DOI:10.1016/j.jallcom.2009.06.172 [33] M. Jafari, M. Vaezzadeh, S. Noroozizadeh: Metall. Mater. Trans.
[2] L. Le Guehennec, A. Soueidan, P. Layrolle, Y. Amouriq: Dental A 41 (2010) 3287 – 3290. DOI:10.1007/s11661-010-0393-1
Mater. 27 (2007) 844 – 854. PMid:16904738; [34] J. Gallego, T.S. Pinheiro, R.Z. Valiev, V. Polykova, C. Bolfarini,
DOI:10.1016/j.dental.2006.06.025 C.S. Kiminami, A.M. Jorge Jr., W.J. Botta: Mater. Res. 15
[3] J. Breme, E. Steinhauser, G. Paulus: Biomater. 9 (1998) 310 – 313. (2012) 786 – 791. DOI:10.1590/S1516-14392012005000100
DOI:10.1016/0142-9612(88)90024-5 [35] P. Rangaswamy, M.B. Prime, M. Daymond, M.A.M. Bourke,
[4] M. Browne, P.J. Gregson: Biomater. 21 (2000) 385 – 392. B. Clausen, H. Choo, N. Jayaraman: Mater. Sci. Eng. A 259
DOI:10.1016/S0142-9612(99)00200-8 (1999) 209 – 219. DOI:10.1016/S0921-5093(98)00893-4
[5] D.J. Gawkrodger: Br. J. Dermatol. 153 (2005) 479 – 485. [36] J. Yang, H. Yu, J. Yin, M. Gao, Z. Wang, X. Zeng: Mater. Des.
PMid:16120131; DOI:10.1111/j.1365-2133.2005.06821.x 108 (2016) 308 – 318. DOI:10.1016/j.matdes.2016.06.117
[6] P. Skowronek, P. Olszewski, W. Świe˛szkowski, M. Sibiński, [37] T. Zhu, M. Li: J. Alloys Compd. 481 (2009) 480 – 485.
M. Synder, M. Polguj: BMC Musculoskel. Disord. 18 (2017) DOI:10.1016/j.jallcom.2009.03.019
426 – 1 – 5. PMid:29100511; DOI:10.1186/s12891-017-1784-x [38] Z.P. Chen, Z. Wen, Q. Jiang: Solid State Commun. 132 (2004)
[7] C. Guo, J. Zhou, J. Zhao, L. Wang, Y. Yu, J. Chen: J. Tribol. Lett. 747 – 750. DOI:10.1016/j.ssc.2004.09.061
42 (2011) 151 – 159. DOI:10.1007/s11249-011-9756-z [39] D.L. Zhang, D.Y. Ying: Mater. Lett. 52 (2002) 329 – 333.
[8] T.M. Grupp, T. Weik, W. Bloemer, H.P. Knaebel: BMC Muscu- DOI:10.1016/S0167-577X(01)00355-X
loskel. Disord. 11 (2010) 3 – 1 – 12. PMid:20047653; [40] Q. Yu, J. Kacher, C. Gammer, R. Traylor, A. Samanta, Z. Yang,
DOI:10.1186/1471-2474-11-3 A.M. Minor: Scr. Mater. 140 (2017) 9 – 12.
[9] H. Matsuno, A. Yokoyama, F. Watari, M. Uo, T. Kawasaki: Bio- DOI:10.1016/j.scriptamat.2017.06.033
mater. 22 (2001) 1253 – 1262. [41] H.C. Wu, A. Kumar, J. Wang, X.F. Bi, C.N. Tomé, Z. Zhang, S.X.
DOI:10.1016/S0142-9612(00)00275-1 Mao: Sci. Rep. 6 (2016) 24370 – 1 – 8. DOI:10.1038/srep24370

998 Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11


A.F. Jankowski et al.: The softening factor cb of commercial titanium alloy wires

[42] W.D. Nix, J.C. Gibeling, D.A. Hughes: Metall. Trans. A 16 Correspondence address
(1985) 2215 – 2226. DOI:10.1007/BF02670420
[43] H. Becker, W. Pantleon: Comput. Mater. Sci. 76 (2013) 52 – 58. Alan F. Jankowski
DOI:10.1016/j.commatsci.2013.03.028 Sandia National Laboratory
[44] Y. Zou, L. Zhang, Y. Li, H. Wang, J. Liu, P.K. Liaw, H. Bei, PO Box 969, MS 9161
Z. Zhang: J. Alloys Compd. 735 (2018) 2625 – 2633. Livermore, CA 94551
DOI:10.1016/j.jallcom.2017.12.025 USA
[45] O. Bouaziz, D. Barbier, J.D. Embury, G. Badinier: Philos. Mag. Tel.: 01-925-294-2742
93 (2013) 247 – 255. DOI:10.1080/14786435.202.704419 E-mail: [email protected]
[46] G.V.S.S. Prasad: An Improved Dislocation Density Based Work
Hardening Model for Al-Alloys, Dissertation Master of Science,
Georesources and Materials Engineering, RWTH Aachen Univer-
sity, Aachen, Germany (2007) pp. 3 – 34.
[47] K.F. Karhausen, F. Roters: J. Mater. Process. Technol. 123 (2002)
155 – 166. DOI:10.1016/S0924-0136(02)00081-X Bibliography
[48] G.V.S.S. Prasad, M. Goerdeler, G. Gottstein: Mater Sci. Eng.
A 400 – 401 (2005) 231 – 233. DOI:10.1016/j.msea.2005.03.061 DOI 10.3139/146.111834
[49] S. Gorsse, C. Hutchinson, M. Gouné, R. Banerjee: Sci. Technol. Int. J. Mater. Res. (formerly Z. Metallkd.)
Adv. Mater. 18 (2017) 584 – 610. PMid:28970868; 110 (2019) 11; page 990 – 999
DOI:10.1080/114686996.2017.1361305 # Carl Hanser Verlag GmbH & Co. KG
ISSN 1862-5282
(Received July 2, 2018; accepted May 24, 2019)

Int. J. Mater. Res. (formerly Z. Metallkd.) 110 (2019) 11 999

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