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Materials Science and Engineering A 441 (2006) 112118

Effect of Zr and Sn on Youngs modulus and superelasticity

of TiNb-based alloys
Y.L. Hao , S.J. Li, S.Y. Sun, R. Yang
Shenyang National Laboratory for Material Science, Institute of Metal Research, Chinese Academy of Sciences,
72 Wenhua Road, Shenyang 110016, PR China
Received 12 April 2006; received in revised form 9 July 2006; accepted 14 September 2006

Quaternary Ti(2026)Nb(28)Zr(3.511.5)Sn (wt%) alloys were investigated to evaluate the effects of Zr and Sn on Youngs modulus
and superelasticity of TiNb-based alloys. X-ray diffraction analysis showed that solution-treated alloys have +  , + ,  + ,  , or
microstructures. Zr and Sn increase the lattice parameters of the phase; for orthorhombic  matensite, they increase the lattice parameter a but
decrease both b and c. The martensitic start temperature of the  is depressed by Zr and Sn additions, whereas the formation of athermal is
dependent on Zr and Sn contents. Differential scanning calorimetry (DSC) measurements show that 1 wt% of Nb, Zr or Sn addition decreases the
martensitic start temperature by 17.6, 41.2 or 40.9 K, respectively, due to their negative effect on lattice parameter ratios of the martensite (c/a and
b/a). Tensile tests were used to evaluate Youngs modulus and superelasticity of the solution-treated alloys. Of the studied alloys Ti24Nb4Zr7.5Sn
with single microstructure has the lowest Youngs modulus of 52 GPa and recoverable elastic strain of about 2% at room temperature after cyclic
2006 Elsevier B.V. All rights reserved.
Keywords: Youngs modulus; Superelasticity; Biomedical titanium alloy; Martensitic transformation; Alloying effect

1. Introduction
Titanium and its alloys have been widely used as biomedical
materials to replace disfunctioned hard tissue in human body
due to their light weight, low elastic modulus, high strength
and excellent biocompatibility and corrosion resistance. During
the past decade, both near -type and -type titanium alloys
comprising only non-toxic and non-allergic elements have been
developed in an effort to match high strength with low modulus
so as to further ease stress shielding problem [1,2]. The addition of high concentration of stabilizers to some of the newly
developed alloys resulted in  martensite with orthorhombic
structure under the condition of quenching [35]. The presence
of  martensite, however, reduces hardness and tensile and
fatigue strengths of the alloys [48]. To avoid impairment to
service life, therefore, alloys containing the  martensite are
generally considered unsuitable for making implant devices for
hard tissue replacement.

Corresponding author. Tel.: +86 24 2397 1961; fax: +86 24 2390 2021.
E-mail address: (Y.L. Hao).

0921-5093/$ see front matter 2006 Elsevier B.V. All rights reserved.

On the other hand, the martensitic and reverse transformations concerning the  can be exploited to develop shape
memory titanium alloys for bio-functional applications, as pioneered by Baker and by Duerig et al. [911]. Their results
suggested that shape memory effect is quite sensitive to heating rate and the maximum recovered strain is about 3% under
the condition of salt bath heating with heating rate higher than
10 C/s. Increasing concern over allergic and toxic effects of
Ni ions released from TiNi led to recent research efforts toward
developing Ni-free shape memory or superelastic titanium alloys
In -type titanium alloys, athermal phase is generally
formed in as-quenched conditions [20]. The influence of the
phase on shape memory effect and superelasticity of titanium alloys, however, is not well understood. Moffat and Larbalestier [21] investigated systematically the competing formation between the  martensite and the phase in quenched
binary TiNb alloys. Their results suggested that the phase
precipitates would not favour the formation of  martensite
and would impair shape memory effect and super-elastic properties of titanium alloys. Recent experimental findings [22,23] of
super-elastic deformation in the absence of  martensite is not

Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112118

consistent with the above conclusion. Reversible to phase

transformation or dislocation-free deformation mechanism have
been suggested as possible origins of the superelastic behaviour
The objective of this study is to investigate the effect of Nb, Zr
and Sn on phase formation, Youngs modulus and superelasticity
in as-quenched titanium alloys, in the hope of reducing Youngs
modulus and improving super-elastic properties by alloying with
Zr and Sn.
2. Experimental
Quaternary TiNbZrSn alloys were melted in an arc melting furnace using a tungsten electrode under argon protection
with magnetic agitation. They were melted three times using a
TiSn master alloy and pure Ti, Nb and Zr as raw materials. The
nominal chemical compositions of alloys are listed in Table 1
(all in wt%). The 40 g buttons obtained were forged at 950 C
to 10 mm diameter cylinders. These cylinders were encapsuled
in evaluated quartz tubes with pressure of 102 Pa and were
solution-treated at 850 C for 1 h before quenching into water
by breaking the capsules. Two buttons with different compositions were analysed by wet chemical analysis to characterize
the differences between nominal and actual compositions, and
the results are shown in Table 2. Interstitial contents of N, H
and O of both alloys were also listed in Table 2. The nominal
compositions shall be used to denote the alloys hereafter.
Tensile testing was conducted at room temperature (21 C) by
cyclic loading at initial strain rate of 1 103 s1 using specimens with a gauge section of 3 mm in diameter and 15 mm
long by MTS 810 Material Test System. In order to improve
the accuracy of measurement, tensile Youngs modulus and
recovered strains were determined from the stressstrain curves
recorded by using a strain gauge. The Vickers hardness was
measured under a load of 10 kg applied for 15 s along longitudinal direction of mechanically ground and polished specimens.
Transformation temperature was measured by differential scanning calorimetry (DSC) at heating or cooling rate of 10 C/min
Table 1
Nominal chemical compositions (wt%) and corresponding phase constitutions
of as quenched TiNbZrSn alloys determined by X-ray diffraction analysis










Table 2
Chemical analysis of TiNbZrSn alloys (wt%)















using Perkin-Elmer Pyris Diamond Type calorimeter. Phase constitutions and their lattice parameters in as-quenched specimens
were determined by 2/ coupling method of X-ray diffraction
analysis along the longitudinal direction of specimens using
D/max 2500PC Rigaku diffractometer. In order to avoid artifact of stress-induced martensitic transformation, the specimens
were heavily etched in a water solution with 8 vol.% of HF to
remove surface layer with internal stress introduced by grinding
and polishing. In order to increase accuracy of lattice parameter measurement, a low scanning speed of 1 /min was adopted
in this study. Specimens for optical microscope observation
were etched at the boiling temperature of a water solution with
40 vol.% HCl. Transmission electron microscopy (TEM) specimens were prepared from mechanically-thinned plates by electropolishing in a solution of 21% perchloric acid, 50% methanol
and 29% n-butyl alcohol at about 40 C. The thin foils were
examined on a Philips EM420 transmission electron microscope
operating at 100 kV.
3. Results and discussions
3.1. Microstructures and phase constitutions of
TiNbZrSn alloys
Fig. 1 shows three typical microstructures (optical
micrographs) of as-quenched quaternary alloys, represented
by Ti24Nb4Zr7.5Sn, Ti24Nb4Zr3.5Sn and Ti20Nb
4Zr7.5Sn alloys. They appear to have single microstructure
(Fig. 1(a)), or matrix with high and low amount of the 
martensite (Fig. 1(b and c)). The small dark spots in Fig. 1(a) are
often observed on metallographic samples of heavily deformed
-phase titanium alloys and are probably dislocation etch pits.
These metallographs also show that the average grain size of the
phase is about 80 m.
Systematic X-ray diffraction analyses revealed that alloys of
the studied range of composition have + ,  + , +  ,
 , or microstructures (Table 1). It is clear from Table 1 that,
for identical Zr and Sn contents, the  martensite is depressed
with the increase of Nb content. This is consistent with experimental results for binary TiNb alloys [21]. A similar trend
was also observed in the effects of Zr and Sn on the martensitic
transformation, as demonstrated by X-ray diffraction profiles of
Ti24Nb-based alloys presented in Fig. 2: under the condition
of 7.5 Sn addition, the  martensite forms in the alloy with 2%
Zr (Fig. 2(e)) but is suppressed in the alloys with 4 and 8% Zr
(Fig. 2(c and d)). For 4Zr addition, the  martensite appears in
alloy with low Sn addition (Fig. 2(b)) but disappears with the
increase of Sn contents (Fig. 2(a and d)). Clearly, the addition
of Nb, Zr and Sn decreases the stability of the  martensite, as
confirmed by the variation of lattice parameters with chemical
compositions to be described in the next section.
The effects of Zr and Sn on phase formation are complicated. Data presented in Table 1 and Fig. 2 show that, for
Ti24Nb7.5Sn base composition, the phase appears if
Zr addition is 8% but disappears for lower Zr contents (2%
and 4%); for Ti24Nb4Zr base composition, the phase is
suppressed for 3.5% and 7.5% Sn addition but forms if Sn


Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112118

Fig. 2. X-ray diffraction profiles of alloys based on Ti24Nb with: (a)

4Zr11.5Sn, (b) 4Zr3.5Sn, (c) 8Zr7.5Sn, (d) 4Zr7.5Sn and (e) 2Zr7.5Sn

Fig. 1. Typical optical microstructures of water quenched quaternary

TiNbZrSn alloys: (a) Ti24Nb4Zr7.5Sn, (b) Ti24Nb4Zr3.5Sn and (c)
Ti20Nb4Zr7.5Sn alloys.

content is increased to 11.5%. By contrast, in Ti20Nb4Zr and

Ti22Nb4Zr base compositions, the phase appears for Sn
additions of 3.5% and 11.5% but disappears for intermediate
amount of Sn (e.g., 7.5%). Clearly, the effects of Zr and/or
Sn on the to transformation is complex compared to their
monotonic influence on the to  transformation.
Competition between the phase and the  martensite
during quenching has been investigated in metastable type

titanium alloys. Moffat and Larbalestier [21] conducted transmission electron microscopy (TEM) analysis of alloys with
different Nb contents and concluded that the modes of
phase decomposition to both the phase and the  martensite are mutually exclusive. The phase forms generally in
metastable type titanium alloys if the formation of the 
martensite is suppressed during water quenching from above
the transus [24]. In the present investigation, TEM analysis
(Fig. 3) did not find characteristic diffraction spots due to the
phase in Ti24Nb4Zr7.5Sn alloy that features single phase
microstructure (Figs. 1(a) and 2(d)). This suggests that appropriate amounts of Zr and Sn have the advantage of suppressing
the formation of both the martensite and the phase when the
alloy is cooled to room temperature.
The absence of (1 1 1) and (0 1 2) superlattice diffraction
peaks of the phase in X-ray diffraction profiles of all
studied alloys suggests that the phase is disordered. This
is consistent with the results for Ti29Nb13Ta4.6Zr and
Ti39Nb13Ta4.6Zr alloys examined by TEM [24]. By contrast, Banerjee et al. [25] recently reported that the metastable
phase in Ti34Nb9Zr8Ta alloy is ordered.
3.2. Effects of Zr and Sn on lattice parameters of the and

Lattice parameters of both the phase and the  martensite determined by X-ray diffraction analysis are listed in

Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112118


Table 5
Lattice strains of to  transformation in TiNbZrSn alloys


1 1 1 /
0 0 1 (%)

0 0 1 /
0 1 0 (%)

1 1 0 /
1 0 0 (%)




a The lattice parameters of the  martensite of this alloy are extrapolated

from Ti(20, 22)Nb4Zr7.5Sn alloys.

Fig. 3. Bright field TEM micrograph (a) and {1 1 0} selected area diffraction
pattern (b) of Ti24Nb4Zr7.5Sn alloy.

3.3. Transformation temperatures of TiNbZrSn alloys

Table 3
of phase in TiNbZrSn alloys
Lattice parameter (A)










Tables 3 and 4, respectively. In agreement with the binary TiNb

alloys [21], the addition of Nb increases the lattice parameter of
the phase. The data in Table 3 also show that the lattice parameter increases with Zr up to 8% content, whereas its increase with
Table 4
of the orthorhombic  martensite in TiNbZrSn alloys
Lattice parameters (A)


Sn is obvious up to 7.5% but then remains almost constant with

further increase up to 11.5%.
As to the  martensite, Table 4 shows that Nb tends to
increase the a but decrease b and c of the orthorhombic lattice; the lattice parameter ratios of b/a and c/a decrease with
the increase of Nb content as a result. Similar tendency is also
observed for Zr and Sn from Table 4. For binary TiNb alloys,
previous investigations showed that phase transformation start
temperature of the  martensite decreases with the decrease
of lattice parameter ratios of b/a and c/a, as reviewed in [21].
Thus, the depressing effects of Zr and Sn on the  martensite
formation can be related to their effects on lattice parameter
Lattice strains accompanying the to  phase transformation in quaternary TiNbZrSn alloys are estimated and
presented in Table 5. A dependence on chemical composition
is clearly seen and the minimum lattice strains occur at chemical compositions close to Ti24Nb4Zr7.5Sn. This quaternary
alloy has much reduced lattice strains compared with ternary
TiNbSn alloys reported in [25].








The temperatures for the to  and reverse phase transformations in quaternary alloys were measured by DSC method
between 150 C at cooling and heating rates of 10 C/min. In
sharp contrast with NiTi shape memory alloy, phase transformation peaks of the studied alloys are quite weak; only those
in several compositions can be distinguished and the results are
shown in Table 6. The peak heights of the phase transformation
in the alloys listed in Table 6 are generally lower than 0.02 W/g
and even difficult to distinguish. Fig. 4 gives an example of DSC
measurement of Ti24Nb4Zr7.5Sn alloy. The peak heights of
the studied alloys are also lower than those reported for ternary
TiNbSn alloys [13].
In order to examine the origin of weak phase transformation peaks of DSC measurements, polished Ti24Nb4Zr7.5Sn
Table 6
Temperatures of  phase transformation in TiNbZrSn alloys


Ms ( C)

Mf ( C)



As ( C)

Af ( C)




Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112118

Fig. 4. DSC curves of water quenched Ti24Nb4Zr7.5Sn alloy.

specimens were subjected to in situ optical microstructure observation during cooling and heating between 20 and 150 C.
The results show that the transformation from the matrix to
 martensite is quite limited when the specimen is cooled
to 80 C (Fig. 5), 30 C lower than the martensitic finish temperature measured by DSC (Table 6). This suggests
that the martensitic transformation is not fully thermoelastic

Fig. 5. In situ optical microstructure observation of Ti24Nb4Zr7.5Sn alloy

water quenched to 20 C (a) and 80 C (b).

in the studied TiNbZrSn quaternary alloys, in contrast with

fully thermoelastic transformations during cooling and heating
observed in TiNbSn ternary alloys [13]. The in situ optical
microstructure observation also shows that the transformation
start temperature is about 10 C, higher than the DSC measured value of about 50 C, suggesting internal stress induced
by surface polishing has significantly increased the martensitic
transformation temperature.
Comparing the data of Ms temperature shown in Table 6,
it can be estimated that 1 wt% of Nb, Zr or Sn decreases
Ms temperature by about 17.6, 41.2 or 40.9 C, respectively.
The estimation was made using actual chemical compositions
obtained by chemical analysis instead of nominal ones listed
in Table 1. It also should be noted that the influence of interstitial elements such as oxygen was assumed constant in the
above calculations. Based on these data, Ms temperatures of the
alloys not listed in Table 6 can be roughly estimated: the phase
transformation temperatures of Ti(2026)Nb4Zr11.5Sn and
Ti24Nb8Zr7.5Sn alloys are lower than 150 C, while those
of Ti(20, 22)Nb4Zr3.5Sn alloys are higher than +150 C.
They are all out of the temperature range we set for DSC study.
The effects of Nb and Sn on martensitic start (Ms ) temperature have been investigated in ternary TiNbSn alloys by
Hanada and coworkers [13,26]. Inconsistent results, with 1% Sn
decreasing Ms by about 78 C [13] or 52 C [26], were reported.
Both reported data were much higher than the estimation of the
present study (40.9 C). In addition, the Ms decrease due to Nb
in ternary alloys [26] is about twice that in the studied quaternary
alloys. One possible reason of the above quantitative difference
is related to chemical composition. The following experimental results tend to support such speculation: Sn was reported to
have quite weak effect on martensitic transformation in binary
TiSn but the effect is strong in ternary TiNbSn alloys [26];
additional evidence is provided by small addition of Pd in TiNb
alloys that weakens the effect of Nb on martensitic transformation and results in trivial change of transformation temperature
even when Nb content is increased from 30 to 40 wt% [19]. How
the interaction of these alloying elements influences the martensitic transformation temperature is open for further theoretical
Table 6 shows that the differences of Ms and Mf as well as
As and Af are just about 2 C, much lower than those for ternary
TiNbSn alloys [13,26]. Furthermore, the difference between
Af and Ms is about 7.7 C in Ti24Nb4Zr7.5Sn alloy, much
lower than TiNbSn ternary alloys. Takahashi et al. [13] and
Nitta et al. [26] reported that the corresponding difference is
about 25 and 90 C in Ti25.4Nb9.9Sn and Ti27Nb8.1Sn
alloys, respectively. This small difference in transformation temperatures in Ti24Nb4Zr7.5Sn alloy can be attributed to the
low lattice strains of to  phase transformation, as mentioned in Section 3.2. It was noted earlier that the martensitic
and reversible transformations are difficult to complete in the
quaternary alloys during cooling and heating (see Fig. 5). This is
consistent with the small differences of start and finish transformation temperatures, Ms and Mf as well as As and Af . However,
it cannot explain the small difference between both start temperatures, As and Ms .

Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112118


ent phase did not fully transform to the  martensite before

testing. This is evidenced by the double yielding phenomenon
in the stressstrain curve (Fig. 7(a)) due to the stress-assisted
martensitic transformation. X-ray analysis (Table 1) that reveals
+  microstructure of Ti24Nb2Zr7.5Sn supports above
argument. As mentioned in Section 3.3, the martensitic transformation in the studied quaternary alloys appears much more
sluggish than is usual for thermoelastic martensite and does
not go to completion. The double yielding phenomenon is also
observed for Ti24Nb4Zr7.5Sn alloy (Fig. 7(b)) but not for
Ti24Nb4Zr11.5Sn alloy (Fig. 7(c)). In this case, the phase
is fully stabilised with respect to the martensitic transformation

Fig. 6. Tensile Youngs modulus (a) and Vickers hardness (b) of water quenched
TiNbZrSn alloys.

3.4. Youngs modulus and superelasticity of TiNbZrSn

Tensile Youngs moduli of the studied alloys are plotted in
Fig. 6(a). The Youngs modulus of as-quenched alloys varies
with chemical composition and a minimum of about 52 GPa is
obtained in Ti24Nb4Zr7.5Sn alloy. Examining phase constitutions of the alloys given in Table 1, it can be seen that the alloys
containing the phase generally have high Youngs modulus.
This is because the phase has higher Youngs modulus than
the and the  phases [46]. The data in Fig. 6(a) also show
that Youngs moduli of the alloys containing the phase are
only slightly higher than those without the phase. This suggests that the volume fractions of the phase are quite low in
these alloys. The measurements of Vickers hardness presented
in Fig. 6(b) also support this deduction.
Superelasticity of water quenched TiNbZrSn alloys
was evaluated by cyclic deformation at initial strain rate
of 1 103 s1 at room temperature (21 C). Three typical stressstrain curves, demonstrated by Ti24Nb-2Zr7.5Sn,
Ti24Nb4Zr7.5Sn and Ti24Nb4Zr11.5Sn alloys, are
shown in Fig. 7. The martensitic start (Ms ) temperature for
the above three alloys decreases in turn. Although the tensile
test temperature is about 9 C lower than the martensite finish
(Mf ) temperature of Ti24Nb2Zr7.5Sn (Table 6), the par-

Fig. 7. Stressstrain curves at 21 C of water quenched Ti24Nb2Zr7.5Sn

(a), Ti24Nb4Zr7.5Sn (b) and Ti24Nb4Zr11.5Sn (c).


Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112118

because its Ms temperature is too low as a result of its high Sn

Since elastic strain recorded by a tensile testing machine can
be twice as high as its true value [13], the stressstrain curves
shown in Fig. 7 were recorded by using a strain gauge to ensure
accurate measurement of elastic strain. It can be seen from
Fig. 7(b) that, for Ti24Nb4Zr7.5Sn alloy, elastic strains of
1%, 2% and 3% are totally, near totally and partially recovered,
respectively, after unloading. The superelasticity of this alloy is
slightly lower than ternary Ti25.4Nb9.9Sn alloy [13]. From
the view point of thermoelastic transformation, the above difference can be explained by the difference between the testing
temperature and the austenitic finish (Af ) temperature. For the
ternary alloy, the testing temperature is 30 C higher than the
Af temperature, a generally accepted temperature difference for
achieving significant superelasticity. On the other hand, the temperature difference for the quaternary alloy, about 63 C, is too
high to obtain good superelasticity. The above argument suggests
that increasing Af temperature by decreasing the contents of
Nb, Zr and/or Sn would improve superelasticity. However, additional experiments yield contrary results. Quaternary alloys with
increased Sn content were found to possess improved superelasticity and a maximum recoverable tensile strain of 3.3% was
obtained in an alloy with 7.9 wt% Sn (compared to 7.5 wt% Sn
in the studied alloy) [27]. Furthermore, stressstrain curve of
as hot-rolled 7.9Sn alloy exhibits non-linear elastic deformation
behaviour without double yielding, substantially different from
the curve shown in Fig. 7(b).
It should be noted that there exist several reports of superelasticity that are not related to the  martensitic transformation [19,22,23]. Further investigation to reveal other kinds of
mechanism is therefore of crucial importance for improving the
superelastic properties of titanium alloys (e.g., by combining
two or more mechanisms).
4. Conclusions
The effects of Zr and Sn contents on Youngs modulus
and superelasticity of water quenched quaternary TiNbZrSn
alloys were investigated in this study. The main results are summarized below:
(1) Both Zr and Sn tend to increase the lattice parameter of the
phase; they increase the lattice parameter a but decrease
b and c of the  martensite.
(2) The martensitic start temperature decreases by about 17.6,
41.2 and 40.9 C due to the addition of 1 wt% of Nb, Zr
and Sn, respectively. Zr and Sn are therefore effective in
suppressing the  martensitic transformation, as can be
explained by their effects on the lattice parameter ratios of
c/a and b/a.
(3) The lattice strains of forming the orthorhombic  martensite from the bcc phase are dependent on chemical composition. The minimum is obtained in Ti24Nb4Zr7.5Sn

among the studied alloys. A small temperature hysteresis,

Af Ms , of about 7.7 C, is detected in this alloy.
(4) The formation of the athermal is dependent on both Zr
and Sn contents in Ti(2026)Nb-based alloys.
(5) Ti24Nb4Zr7.5Sn alloy with single microstructure has
a minimum Youngs modulus of 52 GPa and recovered elastic strain larger than 2% after cyclic deformation at room
The work was partly supported by the NSFC (grants
50471074 and 30471754) and the Chinese MoST (grant



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