Acta mater. Vol. 44, No. 6, pp.

2295-2307, 1996
Elsevier Science Ltd
Pergamon Copyright 0 1996 Acta Metallurgica Inc.
0956-7151(95)00343-6 Printed in Great Britain. All rights reserved
1359-6454/96 $15.00 + 0.00

THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

D. S. FORD and S. R. WHITE
Composites Manufacturing Labs, Department of Aeronautical and Astronautical Engineering,
University of Illinois at Urbana-Champaign, Urbana, IL 61801, U.S.A.

(Received 27 June 1995; in revised form 7 September 1995)

Abstract-Extensive and full range mechanical testing of 55Ni45Ti nitinol alloy wire up to failure over
a wide range of testing temperatures is reported. Thermomechanical properties are obtained including:
initial modulus, secondary modulus, critical martensitic start and finish stresses, plastic flow stress,
recovery strain limit, failure stress and plastic modulus. The data is correlated with the Brinson constitutive
model modified to account for full range loading. The ratio of austenite to martensite moduli was found
to be 5.8 and the secondary modulus (stress-induced martensite) was found to be smaller by a factor of
two when compared to the modulus of (stress-free) thermally induced martensite. The influence of the
initial temperature treatment of the nitinol was shown to be pronounced within the transformation range.
Reasonably accurate correlation is obtained with the modified Brinson constitutive model although there
is some discrepancy in critical stress predictions which is partially attributed to experimental scatter.

1. INTRODUCTION common shape memory alloys its existence is limited

and it occurs over a very small temperature range
Shape memory alloys (SMA) undergo a solid state and with relatively small recoverable strains ( < 1%)
allotropic transformation between a low temperature [l, 6, 71. In nitinol, the R-phase structure only occurs
martensitic phase and a high temperature austenitic for specific compositions and annealing temperatures
parent phase. This transformation occurs under the [3,61.
influence of thermomechanical load. The parent to From an engineering perspective, nitinol represents
martensite transformation (p-m) is known as the one of the most useful shape memory alloy materials.
forward or martensitic transformation. The marten- It has low thermal conductivity, high resistivity, good
site to parent transformation (m-p) is called the fatigue resistance and is corrosion resistant [ 1, 81. One
reverse transformation. What makes SMA unique is of the most important aspects of nitinol is its ability
that most of the deformation caused by the trans- to experience large, reproducible shape recovery after
formation can be fully recovered by appropriate temperature cycling. Although a hysteresis results, it
stress and temperature histories. Alloys such as InTl, can be widened or narrowed as desired. For example,
CuAIZn, CuAlNi, CuSn, AuCd, NiTi and others a wide hysteresis and low recovery loads are required
have been shown to exhibit this shape memory for orthodontic applications where patient comfort
behavior. Of these, NiTi has received considerable and gradual loading is important [9]. For structural
attention in research and industry. actuators, large loads and small hysteresis are
NiTi, nitinol, was discovered in 1958 by William J. required. The properties of nitinol can be changed
Buehler at the Naval Ordinance Laboratory [l]. In considerably by changing the nickel composition of
NiTi alloys, austenite has a body centered cubic B2 the alloy, adding other alloying elements (Pd and
structure and is highly ordered [2]. Martensite is Pt [lo], Cu [l, 6, II], and others), or by altering
generally considered to be a monoclinic distortion of processing conditions such as annealing temperature
the B19 cell and can exist in many variants [3]. The [3, 121, amount of cold work [12-141, and aging
martensite transformations are first order [2,4] and [lo, 121.
heat is liberated when martensite is formed. There is Considerable attention has been devoted recently
a hysteresis associated with the transformation and to using nitinol in hybrid composite materials that
there is a temperature range over which both phases are capable of adapting to their environment or
co-exist. A third phase, called the R-phase, can also being actively controlled. Most of this work has
form. The R-phase has a rhombohedral structure focused on the development of SMA composites.
and its transformation is a displacive first-order SMA composites are materials in which SMA is
transformation that precedes the martensitic trans- embedded and used as an actuator. SMA composites
formation [3, 51. The R-phase can transform could be used for adaptive airfoils in which the
reversibly without hysteresis and has proven very performance of the aircraft is actively controlled by
promising for use in cyclic operations. However, for SMA actuation. Nitinol is particularly suited for

2295
2296 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

embedding because of its unusually high resistivity;

resistive heating can be used to induce the transform-
ation. In addition, up to 10% recovery strain upon
unloading can be achieved with nitinol [4].
In order to construct and design SMA composite
structures, an effective medium theory for SMA
composites is necessary. Composite constitutive
models and micromechanical theories are well known
and effectively describe composite material behavior
in most cases. SMA constitutive models have only
recently received attention. The constitutive models
fall into two categories: phenomenological and
micromechanical/thermodynamic. Phenomenological i
models generally require extensive empirical data and
they ignore the detailed microstructural mechanisms. Fig. 1. Typical stress-strain curve for nitinol showing four
Recent work in this area has sought to combine a regions of behavior. Region I is the linear elastic response
of the initial structure. Region II is the transformation of the
continuum thermodynamics approach with a micro-
initial structure to a single variant of stress-induced marten-
mechanical modeling of martensite-austenite volume site (SIM). Region III is the linear elastic response of SIM.
averaging. No single constitutive model has been Region IV is the plastic deformation and final failure.
found that adequately describes the entire range
of mechanical behavior up to failure. In addition,
although many studies exist on mechanical testing martensitic product in which a small amount of slip
of different nitinol systems. most are focused on and dislocation motion is apparent [6, 7, 161. The
examining the pseudoelastic and shape memory measured modulus in this region is defined as the
effects. Data on the full range of loading up to failure secondary modulus E,. Further deformation causes
are lacking. a second yield plateau associated with slip and dis-
In this paper, a comprehensive study of the location motion, resulting in plastic deformation
thermomechanical behavior of 55Ni45Ti nitinol wire (region IV). The stress at which this occurs is defined
is reported. The stress-strain behavior of nitinol up as the plastic flow stress, op.
to failure in tension is examined at several tempera- If the tensile test is reversed in region II or III. the
tures throughout the transformation range. From the material exhibits unique behavior. If the temperature
data several important material properties are deter- is above A,, a hysteresis loop occurs and the material
mined. These include the critical transformation returns to its original dimenions. This is known as
stress, phase moduli, stress influence coefficients and
failure stress, all as a function of testing temperature.
In addition, the effect of previous temperature treat- T>A, T-+
ment on mechanical behavior is examined. The
test results are then correlated with a phenomenolog-

lz
(5
ical constitutive model developed by Brinson [15]
p-m
which is modified to account for full range loading
effects.

heating above A, E
2. MECHANICAL BEHAVIOR OF NITINOL
(4 (b)
2.1. Constitutive response of nitinol
The constitutive respone of nitinol is dependent Ms>T>Mf T<M,
upon the applied load and temperature. Figure 1 is a
typical tensile stress-strain curve for nitinol. In region
I, linear elastic deformation of the initial structure
with initial modulus Ei occurs. Upon further deform-
ation into region II, the martensite start critical stress,
eM,, is reached which gives rise to stress-induced
martensite (SIM) for temperatures in the range
A, < T < Md or martensite reorientation for T < M,. &

Either of these processes produces a martensitic yield

plateau within which the stress remains approxi- (4
mately constant until the martensite finish transform- Fig. 2. Types of SMA constitutive response: (a) PE by
ation stress, oMy, is reached. Region III consists of transformation; (b) SME; (c) FE: and (d) PE by reorienta-
the elastic deformation of the self-accommodated tion
 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL 2291

pseudoelastic (PE) behavior [Fig. 2(a)]. At tempera- two possible transitions due to phase equilibrium
tures between Mr and A, a large permanent set and thermodynamic considerations. The two tran-
remains after unloading. Upon heating above A,, sitions are defined as T, = (M, + A,)/2 and T, =
however, the material will again return to its original (W + 4)P.
dimensions [Fig. 2(b)]. This is known as the shape Melton and co-workers [6, 191 examined the
memory effect (SME). If the material returns to its stress-strain behavior of many different types of
original dimensions by opposite stressing [Fig. 2(c)] nitinol such as ternary [19] 40Ni40TilOCu, binary [6]
then the phenomena is called ferroelastic (FE) behav- (54.5Ni45.5Ti, 54.8Ni45.2Ti, 55.5Ni44.5Ti) and
ior [17]. At temperatures less than Mr the martensite quaternary alloys [6] (49N44Ti5Cu2Fe). Isothermal
changes structure via reorientation processes. This tests were conducted in all temperature ranges within
reorientation occurs pseudoelastically upon loading a cryostat chamber containing alcohol, cooled with
and unloading as shown in Fig. 2(d). liquid nitrogen (T < O’C), in a water bath (0 d
T < lOO’C), or an oil bath (T > 1OOC). Melton and
co-workers examined the effect of nickel composition
2.2. Literature review
on critical stress/temperature behavior [19] as well as
The first extensive tension testing of nitinol wires the effect of alloy composition on the entire
was done by Cross et al. [18] as part of a case study stress-strain response [6]. The equilibrium tempera-
for Goodyear and NASA. The specimens used in the ture, martensite critical stress, austenite yield stress
experiment were 3.94 mm long by 0.79 mm diameter and martensite stress influence coefficient were shown
55Ni44.93Ti0.07C wires tested in a temperature to decrease with increasing nickel content. In
controlled environment. The stress-strain response addition, the plastic flow stress and the stress to
at various temperatures from well below Mr to induce SIM had similar stress influence coefficients
well above A, was examined and several material for T < Ms. This result showed that the plastic flow
parameters were determined from the tests including stress and the martensite critical stress occur by
modulus and martensite critical stress values. Cross similar twinning processes. In addition, the modulus
and co-workers found that the initial modulus was shown to decrease during cooling through
increased with increasing temperature above A4,. For the martensitic phase as in the earlier work by
temperatures between A, and Ar, the modulus in- Cross.
creased asymptotically to 82.7 GPa. At temperatures Other works on the entire stress-strain response up
less than M,, the modulus increased from 20.7 GPa to failure have been reported by Ford et al. [5], Dye
at M, to 28.3 GPa at Mr. Upon heating from [20], and Ditman [23]. The first two papers include
temperatures below Mr, the modulus essentially correlations with available constitutive models as well
remains constant (27.6 GPa) until reaching A,. The as an examination of the effect of thermal treatment
austenite to martensite modulus ratio was found to on the stress-strain response of 55Ni45Ti. The model
be about 2.9. Other researchers have found this correlations were restricted to stress-strain behavior
ratio to vary from as low as 2.3 to as much as 6 over the transformation range only. Little work exists
[5, 13, 19,201. that attempts to characterize the overall stress-strain
In addition, Cross and co-workers found that the behavior of nitinol. Most research on mechanical
martensite critical stress remains constant outside the testing has been relegated to the pseudoelastic or
transformation range (620 MPa for austenite and shape memory effects.
103 MPa for martensite). The austenite/martensite Researchers have found that compression, torsion
critical stress ratio in their case was found to be 6.2. and flexural loading of nitinol result in similar con-
Others have found typical critical stress ratios to be stitutive behavior to that observed in tension but
between 8 [19] and 10 [l]. with marked differences in mechanical properties,
Cross’ results showed that the martensite critical [4,9, 19,21,24-301. The compression response is
stress and initial modulus change drastically in the characterized by larger critical stresses and smaller
vicinity of the nitinol equilibrium temperature, (T,,); recoverable strains than those observed in tension.
the temperature of the minimum of the critical stress However, the critical stresses in torsion are much
versus temperature curve. The slope of the critical smaller than those observed in tension or com-
stress versus temperature curve around the equi- pression, while the recovery strains and are much
librium temperature is defined as the martensite stress greater [19]. Flexural response has been shown to be
influence coefficient (C,). The location of this comparable to that in tension [28-301.
transition varies widely as reported in the literature.
In Cross’ analysis, the transition was found to be A,
during heating and M, during cooling. Brinson [15] 2.3. Constitutive modeling
and Alder et al. [21] have also shown this transition The different constitutive responses are the result
to occur at M,. Furthermore, Sun and Hwang [ 171 of two types of thermoelastic martensitic structural
and Melton et al. [6, 191 have stated that this tran- changes: oriented growth and shrinkage of stress-
sition occurs at an equilibrium temperature defined as induced martensite variants (transformation) and
Teq = T, = (MS + A,)/2. Hedayat et al. [22] suggested reversible motion of the interface between the
2298 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

self-accommodating variants (reorientation). To

describe the various types of behavior mentioned, Hruring
constitutive models have been developed. The
constitutive models which attempt to describe these
‘0° t -r----l
behaviors can be categorized into two groups: sa
phenomenological and thermodynamic/micromech-
0
anical.
Phenomenological models try to capture the
overall mechanical response while ignoring the micro-
structural mechanisms associated with the marten- b
sitic transformation. The constitutive equation is Mt M, .A\ 4
obtained from thermodynamic considerations [31] Temperature
dX = C(c, s’, T) dt + Q(t, 5, T) di’ + H(t, 5, T) dT Fig. 3. Martensite fraction versus temperature hysteresis
curve.
(1)
where 5 is the martensite volume fraction, C is the dependence is of primary importance for constitutive
Piola-Kirchoff stress, t is the Green strain, C is the modeling. Researchers have approached this problem
stiffness tensor, a is the transformation tensor, 0 is with a variety of techniques. Tanaka [31] uses a
the thermoelastic tensor and T is the temperature. thermodynamic approach based on nucleation con-
Integrating equation (1) while assuming material siderations. It yields an exponential dependence of
properties do not change during the transformation martensitic fraction on both stress and temperature
gives the I-D constitutive equation for the forward and reverse transformation to
account for both stress free thermal and SIM trans-
D - u,, = E(t - tO) + Q(c - 5”) + O(T - TO). (2)
formation. Zhang et al. [32] developed a similar
Equation (2) can be written in the following form exponential dependence. Liang and Rogers showed
that a simpler representation is obtained with a
0 -gTo=E[(t -co)+8(5 -5o)+~(T-T,,)1 (3) cosine dependence [30]. Lagoudas and Boyd [33] have
where E is the Young’s modulus, fl is the transform- shown that either approach is a special case of their
ation recovery coefficient, and c( is the thermal generalized continuum thermodynamic formulation.
expansion coefficient. The zero subscript is used to The above models are developed for use in model-
indicate the initial value at the start of transform- ing the PE and SME constitutive response. The
ation. For isothermal testing, the last term in martensite critical stress/temperature behavior for
equation (3) vanishes (i.e. T = TO) and equation (3) temperatures less than the equilibrium temperature is
reduces to not taken into account. As a result, the constitutive
behavior over the entire transformation temperature
c - go = -We - to)+B(5 - 5011. (4) range cannot be effectively determined. The phe-
nomenological model of Brinson [15] attempts to
The Young’s modulus is assumed to be constant
characterize the nitinol constitutive response over the
throughout transformation in the derivation of
entire transformation range. Experimental testing has
equation (2). However, the Young’s modulus has
shown the Brinson model to correctly represent the
been observed to exhibit a strong dependence on
constitutive behavior for all temperatures within the
martensite fraction. Most researchers have used a
transformation temperature range [5]. The Brinson
rule of mixtures relation for Young’s modulus
model is described next and is modified to account for
[equation (S)]
full range loading of nitinol.
E(5)=E,+5(E,u-EA) (5)
where E, and EM are the austenite and martensite 2.4. ModiJied Brinson model
moduli. Furthermore, the transformation recovery Brinson [15] assumes that the martensite fraction
coefficient is just can be written as the sum of the fraction of the
material that has been transformed by stress to a
fi= -I$ (6)
single variant, <‘, and the fraction that is pure
where t,_ is the recovery strain limit. temperature induced with multiple variants. 5’
The martensite volume fraction is the chosen state
variable that governs 5 =ts+cT. (7)
material transformation.
Figure 3 represents a schematic of a martensite In this case, for isothermal testing the one dimen-
fraction versus temperature plot for nitinol. As the sional constitutive equation (1) reduces to
temperature is increased from A, to A,, nitinol under-
goes the m-+p reverse transformation. On cooling fJ - oo= E(5)Kt -to) + !m+~L&5; (8)
from M, to M, the p+m forward transformation where the modulus varies with martensite volume
occurs. Accurate modeling of the martensite fraction fraction by equation (5). The martensite volume
 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL 2299

fraction for the forward p+m transformation is

determined by equations (9) for T > T,, and by
equations (1Oj and (11) for T < Teq.

T > Teq:

(9)

T < Teq:
Fig. 4. Critical stress versus temperature plot for nitinol
showing characteristic V-shaped response.

x(a
-@) 1+5;
f2
I>
The martensite volume fraction for the reverse
m+p transformation is found from equations (14)

P=++63+aT~ 0
(10)
where C, is the average austenite stress influence
coefficient given by equation (15)

where, 5 =;bos[&(T-As-;)]+1

(11)
(14)
If amin < 0 < ai; and Mf < T < Teq then equation
(11) Mhblds, otherwise A,, = 0 for T < Mf. For cases
c.4$+G
where the transformation stresses do not fall within CA =f
(15)
2
the minimum critical stress range given by the stress
inequality above, gw, and cMt can be used in place of where,

I)
G+,~ and o g: in equation (10). The values l,” and li
are the initial martensite components where [g is &P-A,) +1 (16)
determined from equation (12) f 5

I>
The stress ranges over which transformation occurs
&(T-M,) +1 . (12) are given by
eq f
forward, p--+m 0;; + C,(T - T,,)
In equations (9)-(12) GE: is the minimum critical
stress at Teq at the onset of martensitic transform- < ap-m d C,(T - Tey)+crmlnMt
ation, o’$ is the minimum critical stress at Tes at
reverse, m-+p C,(T - A,) < crm-p
the completion of the martensitic transformation,
o is the applied stress, T is the test temperature, < C,(T - A,). (17)
and C, is the average martensite stress influence
coefficient For stresses outside these ranges the material is
assumed to be linear elastic up to the yield point. At
c,= CMs+ CM‘ (13)
the completion of transformation, 5 = 5’ = 5: = I,
2 and the constitutive equation reduces to
The stress coefficients C,,,, and CM, are slopes of the
a=E,(t-t”)+a,, M,<T<A, (18)
martensite start critical stress and martensite finish
critical stress versus temperature curves about Tcg, where 6” is the strain at transformation completion.
respectively (Fig. 4). Brinson assumes that the two In the present work, Brinson’s model is modified to
are approximately equal and that Teq occurs at MS. allow prediction of mechanical behavior into region
The martensite stress influence coefficients are IV in Fig. 1. To accomplish this it is assumed that
positive for T > Teq and negative for T < Teq. Thus, after yielding nitinol behaves as a linear work-
in the present model the V-shape behavior of the hardening material. Thus, region IV can be modeled
critical stress versus temperature curve is taken into using a linear stress-strain law with a plastic
account. modulus, EP, as shown in equation (19). The current
2300 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

mechanical test data appears to support this of the martensite variants are taken into account.
assumption The models of Boyd and Lagoudas [33] and Sun and
Hwang [17] use the Mori-Tanaka averaging scheme
ff = EP(t - t”‘)+a,. (19)
to describe the martensitic volume fraction depen-
Plastic deformation begins when the plastic stress dence within an austenite matrix during austenitic
is reached. Since the plastic flow stress and transform- transformation, and the reoriented martensite volume
ation stresses occur by similar mechanisms [6], both fraction dependence within a stable martensite
exhibiting V-shaped stress/temperature response, matrix during transformation by reorientation of
similar types of relations can be used to obtain the martensite variants. Although the thermodynamic:
plastic flow stress as a function of temperature micromechanical models provide detailed analyses
of the microstructural behavior of the SMA during
transformation and reorientation. they require
q,=a~+C,(T-T,,) MfQT,<T,, (20) characterization parameters that are difficult to
determine by conventional means.
where a? represents the minimum plastic flow stress
determined at the equilibrium temperature, Teq, and
C’; and Cc are the plastic stress influence coefficients 3. MATERIALS
determined from the slope of the plastic stress/
temperature curve for T < T,, and T > Teq, respect- The material used in this experiment was a NiTi
ively. The plastic modulus is assumed to change alloy composed of 55% nickel and 45% titanium,
linearly with temperature over the transformation 55Ni45Ti. It was supplied by U.S. Nitinol, having
range varying from the plastic modulus of austenite, been annealed using a heat treatment process
Es, to the plastic modulus of martensite. EL. (# B175). The austenitic start temperature was quoted
as A, = 27’C with an austenite finish temperature of
EP= E&+ M,8T<Ar. A, = 3I3:c.

4. MECHANICAL TESTING OF NITINOL WIRES

A summary of the constitutive equations for all
regions over the temperature range M, < T < Af is The objective of mechanical testing was to acquire
given in Table 1. The table provides the initial stress uniaxial stress-strain data for nitinol wires up to
and strain and the martensite volume fraction within failure. The data are then used to assess the validity
each region. For region I. E, is the modulus of the of the modified Brinson model and the influence of
initial structure with martensite fraction, lT. During previous temperature history.
transformation (region II) equation (8) is used with
the initial values as shown in Table 1. The term G,~, 4.1. Experimental procedure
and the sum -(E(t,)ci + flE(t,)ls) are initial values Nitinol wire specimens were loaded in uniaxial
which balance each other. These terms may then tension to failure. The specimens were 0.66mm in
be dropped to yield a simpler representation, i.e. diameter and 381 mm in length. The wires were tested
0 = E(t)t -begs. At the start of region III the using an MTS-880 test frame with an environmental
material has fully transformed to martensite and chamber. The specimens were loaded at a rate of
the constitutive reponse is linear elastic above the 0.1 mm/s and data were collected every 200 ms.
martensite finish critical stress. Finally, in region IV Three sets of tests were used to examine the effect
a linear work hardening relationship is used above of previous temperature history. The first set of
the plastic flow stress. The plastic flow stress and specimens were resistively heated well above A, then
plastic modulus are determined from equations (20) allowed to cool to room temperature. The second set
and (21) respectively. of specimens were cooled well below Mf in liquid
nitrogen and allowed to warm up to room tempera-
ture. The last set of specimens was untreated and
2.5. Thermodynamic~micromechanical models
tested in the as-received condition.
Micromechanical models examine the effect of In each set, five groups of tests were conducted,
microstructural mechanisms on SMA transformation designated Tl-5. The first group was tested at tem-
behavior. Unlike the phenomenological models peratures below Mf and the fifth group at tempera-
described previously, the mechanism of reorientation tures above A,. The other three groups were tested

Table 1. Constitutive relations for regions I-IV

R&on c 8” 6, Constitutive equation Strain
 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL 2301

Table 2. Experimental test matrix

Temperature

Temperature Initial Tl T2 T3 T4 T5
history condition A,< T A, < T < A, M,<T<A, M,dT<M, T<M,
Heated (HT) 50 = 0 7” 6 8 9 2
Cooled (CT) l$=5;= I 4 7 6 7 4
Untreated (UT) to = ? 7 7 6 5 5
“Indicates number of specimens tested.

at intermediate temperatures. Table 2 shows the by this method. Instead, knowing A, and having
complete test matrix for the experiments. found Teq from the data as shown in Fig. 4, MS is
The temperature was controlled in the environ- calculated using the equilibrium temperature, i.e.
mental chamber by circulating cryogenic CO, gas for M, = 2Teg - A, [6, 16, 171.
groups T3-5. For elevated temperature testing, The stress influence coefficients were determined by
groups Tl and T2, the chamber was heated with measuring the critical stress and plastic flow stress as
resistive heaters. Wires were gripped using conven- a function of temperature. Plots of uM,, gMr and 0.p
tional flat grips, incorporating a small loop and hook versus temperature were constructed and a linear
arrangement for alignment purposes. For reproduci- least squares fit to the data was used.
bility of the data, a flat grip set-up was used in favor The recovery strain limit, tL, was determined from
of the drum grips used for wires in previous testing the isothermal tensile test results by extrapolating
PI. from the second linear elastic region (fully trans-
formed) to the strain axis. The point of intersection
4.2. Data reduction is t,_ (Fig. 1).
The material constants Young’s modulus of aus-
tentic (EA) and martensite (EM), the plastic moduli of
austenite and martensite (E: and E$,J, the transform- 5. EXPERIMENTAL RESULTS

ation temperatures (MS, M,, A,, and A,), the stress 5.1. Stress-strain behavior
influence coefficients (C,, CM,, C;), and the recov-
ery strain limit (t,) were determined from the exper- In this section the test results and discussion is
imental data. The moduli E, and EM were determined restricted to the HT set of data only. In subsequent
from the linear elastic regions of the stress-strain sections a discussion of the effect of previous tem-
curves for testing at T > Al. In this case the initial perature history is addressed. Figures 6(a)-(e) show
material is all austenite (5 = 0). After stress-induced the results for groups Tl-T5. In all plots there is an
transformation is complete the material is all marten- initial linear elastic deformation up to a critical stress
site (5 = 1) at which stress-induced martensite begins to form. A
plateau region occurs during transformation, after
CT= EAc (5 = 0) (22) which the detwinned martensitic structure is elasti-
cally deformed up to the plastic flow stress. Further
a = E,t (5 = 1). (23)
straining induces plastic flow until final failure.
The transformation temperatures M,, A, and A, for At T > A, [Fig. 6(a)] the critical stress increases as
all sets of tests and MS for the HT case are determined temperature increases. In addition, region III behav-
by the method shown in Fig. 5. Linear fits to the data ior is short-lived and plastic flow occurs quickly after
are drawn on the modulus versus temperature curve. transformation is complete. Figure 6(b) shows the
The intersections define the transition temperatures. mechanical behavior at test temperatures between A,
However, the CT and UT A4, cannot be determined and A,. The critical stress decreases with temperature
and a definite martensitic plateau is observed. The
plastic flow stress is relatively constant within this
temperature range.
The behavior for test temperatures between MS and
A, is shown in Fig. 6(c). Again, the critical stress
decreases with decreasing test temperature and the
plastic flow stress is relatively constant. After trans-
formation is complete, the curves tend to overlay
each other all the way to failure. Figure 6(d) shows
the results for testing between M, and M,. There is
s~ : ’
little effect of temperature within this region. How-
b ever, in contrast to Tl-T3 groups, the critical stresses
Mf M, As 4 T for group T4 increase with decreasing temperature
Fig. 5. Method used to determine transformation tempera- from 100 MPa at 7°C to 110 MPa at 1°C. The mar-
tures. tensitic plateau is also more pronounced. Finally, the
2302 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

1 Ot)o--~-- ~~

0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80
Strain (%) Strain (%)

0 ~““;“~‘,~“‘t”“I”‘,t”“t_-l’~~‘l -a~-++J-t ~--f--+-k

0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80
Strain (%) Strain (%)

0 /N / I p I I / ‘yLpu,

0 10 20 30 40 50 60 70 80
Strain (%)

Fig. 6. Mechanical behavior of 55Ni45Ti nitinol wires (HT Case): (a) Tl [T > A,]; (b) T2 [A, < T < A,]:
(c) T3 [MS G T < A,]; (d) T4 [Mr < T C MS]; and (e) T5 [T < M,].

stress-strain behavior at test temperatures less than
Mr is shown in Fig. 6(e). In this case the curves
overlay each other throughout the entire loading
range.
5.2. Effect of previous temperature treatment
Figures 7(a)-(e) give the stress-strain curves for set
HT, CT and UT at several different temperatures.
The largest differences observed were between the HT
and CT treated specimens, although the discrepancies
were quite small in an absolute sense. The CT and UT
sets gave nearly identical behavior within all tempera-
ture ranges. If differences were apparent amongst the
sets, it occurred within the transformation range and
in the fracture stress. The plastic flow stress for
all wire treatment cases was relatively consistent
suggesting that the plastic processes are not greatly
affected by initial wire treatment.
At T > A, [Fig. 7(a)] there is little difference in
mechanical behavior between the sets. The HT spec-
imens have a slightly higher failure strain than the CT
and UT specimens. However, noticeable differences in
behavior during transformation are apparent at lower
temperatures [enlarged views in Fig. 7(b) and (c)l,
Here the critical stress and initial modulus is largest
for the HT specimens. This effect is easily explained
by referring to Fig. 5. The HT specimens follow the
left branch of the hysteresis loop during cooling.
 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL 2303

At intermediate temperatures (Mr < T < Af) the HT 5.3. Phase diagram
specimens retain their austenitic phase to lower The critical stress at the initiation and completion
temperatures which results in a higher modulus and of transformation is plotted versus temperature
elevated critical stresses. For completeness, Figs 7(d) for all treatment cases in Fig. 8. The critical stress
and (e) are provided. These show the stress-strain follows a V-shaped curve with the minimum
response for groups T4 and T5. There is little differ- occurring at the equilibrium temperature. The general
ence in behavior amongst the different treatments for trend is the same for all treatment cases. The HT
each group. While this lack of discrepancy for group case has much lower stress influence coefficients and
T5 is expected, group T4 should also follow the above equilibrium temperature. However, the completion
arguments. It is conjectured that the test temperature and initiation curves coincide approximately for
(13°C) is close enough to Mr ( x 5°C) that no all cases at temperatures below the equilibrium
discernible difference could be measured. temperature.

s 800 2 250

$ 600 8 200
150
3
; 100
v1 50

0 10 20 30 40 50 60 70 80 0 5 10 15 20
Strain (%) Strain (%)

(a > @I

~ UT Set
____ UT Set

0 5 10 15 20 0 10 20 30 40 50 60 70 80
Strain (%) Strain (%)

0-
0 10 20 30 40 50 60 70 80
Strain (%)

Fig. 7. Effect of wire treatment on mechanical behavior of 55Ni45Ti nitinol wires (HT Case): (a) ‘I’1
[T > A,]; (b) I2 [A, < T < A,]; (c) T3 [M, < T < A,]; (d) T4 [Mf < T < M,]; and (e) T5 [T < Mf].
2304 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

4(JoT__x-_E__
600 --~
- HT (initiation)
- HT (completmn)
i- UT & CT (initiatmnJ
- UT & CT (completmn)

50
D
0 -t_- , -~~, A_ ~~_~ _ ,_ ELI sso - -i - ~. .~_ ~~_~ 0.5

-10 0 IO 20 -iI) 40 50 60 0 5 IO I5 20 2s 30 35 40

Temperature ( “C) Temperature (“C)

Fig. 8. Critical versus temperature phase for 55Ni45Ti. Fig. 10. Plastic flow stress and modulus versus temperature
for 55Ni54Ti.

Table 3. Transformation and equilibrium temperatures for the three

treatment cases IZOO-

Specimen
test A,(_C) A,(‘C) M,(‘C) M,(“C) T,,(“C)

HT 38 27 17 0 21
CT 16” 5 21 J
UT 16” 5 27
K 600
co
“Determined from T,, = (M, + A,)/2
HT Set
~ UT Set
I;li /
CT Set
200 v
Table 4. Martensite stress influence coefficients for the three treat-
ment cases
O- ‘t-2 ~.~ __~ .~ ~. .~~ _.
T < Tcs T ’ T,, -10 0 IO 20 30 40 so 60

Specimen C.% C C c .MY Temperature ( “C)

test (MPal”C) (MPG’ CJ (MPa:j’C) (MPal’C)
Fig. Il. Failure stress versus temperature for 55Ni45Ti
HT ~ 1.0 -0.7 10.0 9.3 (0.66 mm diameter wire tested in uniaxial tension).
CT PO.6 - 0.7 13.2 13.9
IJT -0.6 --0.7 14.5 16.8

Table 3 shows the transformation temperatures

for stress-free conditions and the equilibrium
Table 5. Material mouerties used in modified Brinson model
temperatures for transformation initiation for all
Value
wire treatments. There is little difference between CT
Property T < T,, T > T,, and UT specimens and Tcq occurs near A,. For the
E, @Pa) 53 Same HT specimens, T,, is much lower and occurs near
&(GPa) 9.6 Same (MS + A,)/2 = 22S”C which is assumed by many
Es(GPa) 0.9 Same
EP,(GPa) 0.8 Same researchers [6, 16, 171.
C,s(MPa!“C) -0.9 13.2 Table 4 summarizes the results for the martensite
C,,(MPa/’ C) -0.7 13.9 start and finish stress influence coefficients (CMS and
C,(MPa/“C) -2.0 1.0
C,,) for each wire treatment case. For temperatures

70 I 10

60

htial Modulus

I , im-
3 CT Set
0 ,/ / LL.~ .._~~j_~~.-~
0 10 20 30 40 SO 60
I0 0 IO 20 Xl 40 SO ho
Temperature (“C) Temperature ( “C)
Fig. 9. Initial and secondary moduli versus temperature for Fig. 12. Recovery strain limit versus temperature for
55Ni45Ti. 55Ni45Ti (CT case only).
 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL 2305

greater than Teg, CMSz CM, for each treatment case,
although there is some variability between sets with
values between 9 and 17 MPa/“C. For temperatures
below Teq, the ratio of CM5to Cur ranges from 0.9 to
1.4. For all treatment cases CM3is nearly constant in
this temperature range.
The initial and secondary modulus versus tempera-
ture are shown in Fig. 9. The secondary modulus is
nearly constant (9.6 GPa) up to the equilibrium tem-
perature and then begins to decrease with increasing
temperature. There is no effect of previous tempera-
ture treatment on secondary modulus. This suggests
that the martensitic variant which is chosen for stress
accommodation is not influenced by previous wire
treatment.
The initial modulus shows a hysteretic response.
The HT case follows the left branch while the CT and
UT cases follow the right branch. Obviously, the HT
specimens are completely austenitic above MS,
whereas the CT and UT specimens are initially of
mixed (austenite/martensite) phases. All treatment
cases correspond in the extreme ends, at temperatures
above A, and below Mr. It is interesting to note that
the low temperature asymptote for initial modulus

0)"'
0 10 20 30 40 50 60 70 80 0 10 20 30 40 50 60 70 80

Strain (%) Strain (%)

(a > @I
1000

s 800

“E 600

z 400

fr-li! ;
CA 2~

0 --t--t--t--t--t-P
0 10 20 30 40 50 60 70 3
0 5 10 15
Strain (%) Strain (%)

(C > (4

_s,,i,yy$iig
0 10 20 30 40 50 60 70 80
Strain (%)

(e)
Fig. 13. Experimental correlation with modified Brinson model (CT Case): (a) Tl [T zz A,]; (b) T2
[A, < T < A,]; (c) T3 [M, f T < A,]; (d) T4 [M, < T < M,]; and (e) T5 [T < Mf].
2306 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL

( z 16 GPa) does not correspond to the secondary For temperatures less than Tcqexcellent correlation to
modulus asymptote (9.6 GPa). This indicates that experimental results is obtained [Figs 13(c)-(e)].
there are significant differences in mechanical behav- When using Tes = M, in the modified Brinson model,
ior of the detwinned martensitic variant (secondary it is observed that the plastic flow stress and critical
modulus) and the twinned variants (low temperature stress at initiation are both underpredicted
initial modulus). This lends support to the approach [Fig. 13(c)]. The value of T_, chosen for use in
that Brinson [15] suggests for modeling martensitic modeling is of primary importance and no clear
fraction, in which both stress-induced martensite and distinction can be made from the current data. The
thermally induced martensite are distinct, although value of Tcq is somewhat dependent on previous
two separate values of martensite moduli may be temperature history (Table 3). However, in no case
necessary. was T.Lqz M,, a common assumption in previous
works [15. 18, 211.

5.4. Plastic jaw and ,failure stress

The plastic flow stress and modulus are plotted as 7. CONCLUSIONS
a function of temperature in Fig. 10. The plastic flow
stress versus temperature is similar to the V-shape The mechanical behavior of nitinol is extremely
critical stress curve previously observed. However, sensitive to temperature within the transformation
the plastic flow stress reaches an asymptote range between Mf and A,. Small variations in tem-
(568 MPa) for temperatures greater than A,. It is perature can yield large changes in such properties
interesting to note that the slopes (stress influence as initial modulus and critical stresses. The design of
coefficients) about the equilibrium temperature are SMA actuators and SMA composites must account
very similar. The plastic modulus asymptotically for these material characteristics. In such cases the
approaches 0.9 GPa for temperatures greater than operating temperature should be well controlled or
A,, and a value of 0.8 GPa for temperatures less placed well outside the transformation range.
than Teq. The asymptotes are taken as the austenite For 55Ni54Ti the ratio of austenite to martensite
plastic modulus (Es) and martensite plastic modulus moduli was found to be 5.8. This is near the upper
(E&X end of the reported range of values (2.3-6). In
Figure 11 shows the failure stress behavior as a addition, it has been shown that the secondary
function of temperature for all wire treatments. modulus (of SIM) is smaller by a factor of two when
Strength is nearly constant (z 1000 MPa) up to A, compared to the initial modulus at temperatures
and then begins to decrease with increasing tempera- below M, (stress-free thermally induced martensite).
ture. There is little effect of previous temperature The plastic flow stress follows a similar V-shaped
treatment on the failure stress. temperature curve and reaches an asymptote of
Finally. the recovery strain limit versus test tem- 586 MPa at high temperature.
perature is plotted in Fig. 12. The behavior is very The influence of the initial temperature treatment
similar to failure stress; the recovery strain is constant of the nitinol was shown to be pronounced within the
up to a critical temperature (A,) and then begins to transformation range. The effect is predictable con-
fall off. For 55Ni45Ti the recovery strain is limited to sidering the hysteretic behavior of the martensitic
about 8.5%. fraction versus temperature curve.
Finally. reasonably accurate correlation is ob-
tained with a modified Brinson constitutive model as
a whole. For temperatures less than the equilibrium
6. MODEL CORRELATION
temperature, the experimental correlation is excellent.
In this analysis, the CT experimental data was used
in the model correlation. Due to the CT wire treat-
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 FORD and WHITE: THERMOMECHANICAL BEHAVIOR OF 55Ni45Ti NITINOL 2307

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