Nitinol Af Determination: Opportunities in Active Af Testing

Todd Dickson, Lumenous Device Technologies, Inc.

December 2014
Nitinol is well-known for its special properties that are governed by the transformation between
two solid phases of the material, the martensite phase and the austenite phase. Just as water transitions
between solid, liquid, and gas phases at specific temperatures, nitinol transitions between martensite
and austenite at particular temperatures. As with water, where its transition temperatures can vary
with impurity levels, atmospheric pressure, etc., nitinol is also a bit more complex; we cannot simply
name a constant transition temperature for all nitinol. The transition temperatures vary dramatically
based on a range of factors: the composition of the material, the thermomechanical history of the
material, the direction of temperature change (associated with the topic of hysteresis), and the stress
state of the material.
The Af temperature of nitinol refers to the boundary between the martensite-to-austenite
transformation temperature zone and the higher-temperature zone characterized by austenite. Since
most nitinol devices exploit the superelastic behavior of the austenite phase to recover or maintain a
particular configuration or shape, the Af temperature boundary point is of critical interest for most
nitinol users, since it defines the point at which shape recovery is considered complete. By controlling
Af well, component performance can be more reliably assured. In some cases, placing tighter limits on
Af can even enable further design optimization.
The Benefits of Better Repeatability
Af strongly influences the performance of a nitinol device. If we can control Af better (and test
it more reliably), we can obviously achieve more reliable performance. Moreover, if we improve
measurement reliability, we may exploit the material properties to achieve better and more consistent
performance. Some of the properties in play include:

Superelasticity: optimal at a working temperature 10-20C above Af (T)

Stiffness: greater at higher T
Fatigue resistance: higher at lower T

As we see, some desirable properties are in tension with each other. In some environments,
such as within the human body, there is a narrow range of working temperature. Therefore, for a
given component, based on its desired attributes for superelasticity, stiffness, and fatigue resistance,
there may be an optimal Af temperature. In this case, if we improve the measurement capability, then
we may improve the design itself -- and the performance of the component.
Methods for Determining Af
The two most common methods for determining the transition temperatures are known as
differential scanning calorimetry (DSC) and bend and free recovery (BFR). Note that the Af
temperatures determined by these two methods do not always correlate for reasons that will be
discussed further below.

DSC is the standard method for ingot characterization and measurement. It is also used in
bulk semi-finished materials and sometimes for component characterization. Fundamentally, DSC
identifies the temperature at which the phase change is occurring by measuring either the endothermic
or exothermic heat flow in the material associated with the phase change.
BFR is used in materials that can be deflected significantly including wires, tubes, sheets,
strip, thin film, and components of many shapes. Because BFR testing characterizes the components
mechanical behavior as a function of temperature, the Af determined by this method is often referred
to as the Active Af.
In typical Active Af testing, the component is
cooled well into the low temperature martensitic phase,
deformed, and then slowly heated. The shape recovery
is recorded with frequent sensor readings, typically with
either a mechanical sensor (e.g., an LVDT) or an optical
sensor. The ASTM F2082 standard provides guidance
on conducting this test. After the recovery has passed
well into the austenite region, the plot is processed by
drawing line fits to a) the martensite region, b) the
transition region, and c) the austenite region. The
intersections of these line fits are identified as the As
(austenite start) and the Af (austenite finish) transition
temperatures. This is sometimes referred to as the
tangent method of the ASTM F2082 standard.
Some of the important topics that arise in active Af testing are introduced below:
Strain and Load
Strain and Load can affect Af test results. The effect of strain and load during BFR is one
reason behind the difference between DSC and BFR results. (During DSC testing, the
specimen is not under any load.)
Strain is a real part of actual component performance. In that sense, the effect of strain and
load is not necessarily a disadvantage of BFR testing. When mechanical response to
temperature change is the key interest, BFR is often preferred -- even more so when
deflection and load are inherent in the component performance requirements. In this
case, the Af determined by BFR is often more reflective of real-world performance.
Further, although DSC gives very specific information about the temperature of the
phase transition itself from a fundamental metallurgical standpoint, it requires
specialized equipment, more time per test, and is destructive. Thus, while both methods
have their advantages, the most capable BFR processes are more suitable than DSC for
Af verification of most finished device components.
ASTM F2082 calls for deforming the test specimen so that its maximum bending strain (outer
fiber strain) lies between 2-2.5%. The recommended strain limit of 2.5% was determined

by extensive testing during the development of the standard to be the maximum strain at
which the resultant measured Af is not impacted by the applied test strain.
Load effects are an artifact of the test method. When a rotary or linear displacement
transducer (RVDT or LVDT) is used to measure the recovery (change in deflection as
temperature increases during the test), a load is exerted on the component. In some
cases (such as in shape memory actuators), this may be an important value to set
correctly. In most superelastic devices, it is desirable to minimize this load. The load
suppresses the recovery, leading to slightly higher values of Af. The degree of variation
is a function of the magnitude of the applied load.
In order to avoid the data shift and the measurement noise caused by load effects, a noncontact vision system can be useful as a replacement for the RVDT or LVDT. When
using a non-contact vision system, there is no load applied to the component.
Friction
Friction in the moving parts of an RVDT/LVDT system can produce noise in the data. By
careful design and process capability assessment, this can be controlled.
Friction of an RVDT/LVDT on the test sample can produce strain in very fine samples.
If a sample is fixture during the test, sample-to-fixture friction may be present in LVDT and
vision systems.
Frictional effects and other dynamic effects can be reduced when using a non-contact vision
system. Fixtures can be simplified or eliminated to further reduce noise in the system.
Heating rate
Repeatability of the test may degrade with higher ramp rates:
Thermal gradients. ASTM F2082 requires limiting the heating rate to 4C /min in order to
minimize thermal gradients in the bath, and to ensure that the full component crosssection has a homogeneous temperature.
Data sampling resolution. Higher rates of temperature increase also require more rapid
sampling rates of deflection and temperature. An insufficient data rate will degrade an
otherwise good line fit. Good line fits are crucial for repeatable Af determination.
Starting Temperature
It is important to first cool the sample and the fixture, then deform the sample (while keeping it
cold), and keeping both the sample and fixture cold until starting the recovery test.
The ASTM F2082 standard was written to include materials with a wide range of
transformation temperatures. The standard requires cooling the materials to -55C or
colder for materials that are superelastic at room temperature, and to 10C or colder for
materials that are martensitic at room temperature. Some practitioners adjust the
starting temperature when the expected transformation temperature is within a known

window -- as long as the chosen start point is a temperature at which the material is fully
martensitic.

Critical Considerations for Vision Systems

While non-contact vision systems eliminate various complicating factors of RVDT/LVDT
systems, there are certain factors that need careful attention in the design, setup, and
operation of a vision solution.
Resolution of imaging. Insufficient resolution can degrade the plot quality and reduce
repeatability.
Edge detection, algorithms and lighting. Edge detection algorithms, image processing,
and lighting have to be designed and managed to ensure consistency of edge detection
during a test and between tests.
Agitation. If the test employs agitation (e.g., stirring) to minimize thermal gradients in the bath,
visual artifacts need to be avoided, suppressed, or filtered.
Data Plotting
As previously mentioned, the sample rates of deflection and temperature are important for
ensuring a good line fit to the data.
Tangent method. The Af is determined by the intersection of the transition zone line fit and
the austenite region line fit. The ASTM F2082 standard calls for the transition zone line
fit to be tangent to the steepest portion of the transition zone plot. When the transition
zone slope contains local variation, engineering judgment and/or sophisticated statistical
line fit algorithms are employed to determine the best line fit to the region. When there
may be doubt about the best line fit, it is advisable to report the data plot with line fits as
well as the Af temperature finding itself.
Endpoint method. The endpoint method is not addressed in ASTM F2082. In tangent
method determination, we see that the material continues to recover slightly even after
reaching the Af point marked by the intersection of the tangent line fits. For some
components, it may be important to certify the actual final temperature of recovery. In
this case, the temperature may be referred to as the endpoint method Af.
Repeatability
As discussed above, a highly repeatable Af measurement process can promote significant
reliability or design improvements. Even for legacy product, understanding repeatability is essential
for tolerance-setting and process control. For customary measurement processes, measurement
capability analysis includes calibration and an evaluation of gauge, repeatability, and reproducibility
(GR&R). In GR&R studies, a test is repeated with multiple operators to evaluate the variation among
the results achieved in real-world use.

In the context of Af determination, there is no such thing as accuracy since there is no

reference standard for calibration. Instead, when evaluating the performance capability of the
measurement system, we focus on repeatability and reproducibility (R&R).
When validating a commonplace dimensional measurement device such as a caliper, we
measure a calibration standard a number of times. Calibration standards are known to be unchanged
by the measurement process, so this approach works fine. In the case of Af, we have to adjust this
approach. Cycling a component through the Af test may change the components thermomechanical
history and thus influence its Af temperature. As a result, in Af R&R studies, we do not measure a
component more than once. Instead, we make a single specimen, segment it into individual subspecimens, and test each sub-specimen only once.
It is useful to begin with an understanding of the current state of the art. In the preparation of
the ASTM F2082 standard, an R&R test was performed on nitinol wire using the techniques defined in
the standard. (The study details are published in the standard.) These results might represent the
generally accessible process capability in the industry. The repeatability result was 4.6C in one study
of 5 sub-specimens and 2.7C in another distinct study of 5 sub-specimens.
With careful and dedicated efforts to address the sources of measurement variation discussed
above, some laboratories have achieved repeatability in the range of 0.5C and below a reduction in
measurement error of 80% or better.
Throughput and Ease of Use
The factors described above have generally restricted Af testing to small sample sizes and
personnel with specialized training. The slow throughput of test methods intersects with these
constraints, and the resulting scarcity of data has placed limits on industrys ability to control Af. A
not-insignificant number of nitinol-related product recalls have to do with insufficient shape recovery
in superelastic use conditions. More robust test methods that are simpler to use and more repeatable
will open the testing bottleneck, offer improved safety, and enable more effective product design.