fatigue behavior studies of niti shape memory alloys using bulge test_swapnil dhakate_10311017
TRANSCRIPT
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FATIGUE BEHAVIOR STUDIES OF
Ni-Ti SHAPE MEMORY ALLOYS USING BULGE TEST
Masters Degree Dissertation
Submitted in Partial Fulfilment of Requirements for the Degree of
Master of Technology
In
Metallurgical Engineering and Materials Science
by
Swapnil N Dhakate
Roll No: 10311017
Under the supervision of
Prof. Prita Pant
Dept. of Metallurgical Engineering and Materials Science
Indian Institute of Technology Bombay
June, 2012
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Acknowledgement
Foremost, I would like to express my sincere gratitude to my guide, Prof. Prita Pant, for
the opportunity provided to work on such an interesting topic. It has been a memorable learning
experience because of the freedom she allowed for doing work.
I would also like to acknowledge Dr. Madangopal K. for his extended support and
guidance. I would also like to thank OIM National Facility and Metal Forming Lab for allowing
use of their facilities.
I extend special thanks to Nishant Shelkar for helping me with all electronics related
queries. I am very grateful to Jaiveer Singh for his timely help with the EBSD and SEM
instruments. A very special thanks to my peers and fellow MEMS M.Tech students, andespecially my group members for their friendship, particularly, the distractions they provided. I
would also like to thank all those who directly or indirectly helped me during duration of my
project and made possible whatever I was able to do.
Yours Truly
Swapnil Dhakate
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Abstract
An experimental investigation in martensitic transformation behaviour during fatigue of
NiTi shape memory alloys using bulge test was undertaken. In order to carry out the fatigue, we
have designed a set-up that allows us to carry out Bulge tests on miniature samples so that a
marked region of the sample can be studied after repeated loading. The set-up was automated so
that the precise and accurate strains can be provided and large number of fatigue cycles can be
carried out. This set-up was then used to bring out the microstructural changes that occur during
fatigue in NiTiCuCr. EBSD results show that material can withstand large number of cycles (50)
at lower strain of ~10% whereas at higher strain of ~25% the material starts deteriorating at very
low cylces (5). The martensite retained after 50 cycles at 10% and 25% strains is 3% and 37%
respectively, which is large variation with strain. At higher strain, the orientation (001) shows
higher retained martensite as compared to (111) and (101) orientations. XRD showed that after
same number of cycles of fatigue on NiTi and NiTiCuCr, there was not much difference in the
amount of martensite formed but the orientations at which the martensites appear were different.
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Table of Contents
Abstract.....i
Table of Contents ..ii
List of Figures..iii
List of Tables..v
1. Introduction12. Literature survey
2.1. Introduction to SMA..32.2. Martensitic transformation..52.3. Pseudoelasticity and Superelasticity....92.4. Mechanical fatigue in NiTi and NiTiCu alloys.112.5. Factors affecting stress-strain response..132.6. Microstructure during fatigue.172.7. Characterization techniques and testing methods
2.7.1.DSC..192.7.2.Bulge Testing.192.7.3.EBSD212.7.4.Aramis21
3. Experimental Work3.1. Sample Fabrication..233.2. Bulge Fatigue Testing 25
3.2.1.Device Design253.2.2.Test Procedure.263.2.3.Automatization of set-up.263.2.4.Microprocessor coding..30
4. Bulge Fatigue Results4.1. Microstructual Correlation using EBSD.334.2. XRD Analysis.394.3. Strain Measurements Using GOM41
5. Conclusions and Future Work.446. Bilblography.467. Appendix.50
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List of figures
Fig 2.1 Crystal structure of (a) cubic austenite phase (b) monoclinic martensite phase..3
Fig 2.2 Schematic illustration of shape memory effect4
Fig 2.3 Bain Distortion.5
Fig 2.4 Lattice invariant deformations (b) Slip (c) Twin6
Fig.2.5 Schematic representation of the interface, habit plane7
Fig 2.6 Crystallographic steps for the B2 to Bl9 transformation in NiTi...7
Fig 2.7 Phase Transformation paths of NiTi alloys.8
Fig 2.8 (a) 3 possible lattice correspondences in the reverse transformation. 9
Fig.2.9 Different stress-strain path followed by superelasticity and pseudoelasticity...10
Fig 2.10 Stress-strain curves (hysteresis curves) during cyclic loading with number of cycles11
Fig 2.11 Stress-strain curve for same no. of cycles of loading but at different stress amplitudes.12
Fig 2.12 Accumulated plastic strain with increasing no. of cycles for different stresses..13
Fig 2.13 TTT diagram describing aging effect on alloy Ni52Ti48..16
Fig 2.14 Quasi-static Stress-Strain Curve for NiTi....17
Fig 2.15 Accumulation of localized plastic deformation within the grains upon cyclic load18
Fig 2.16 Microscope images at strain levels 0%, 2%, 4%, 10% showing full transformation...18
Fig 2.17 A typical DSC scan on a sample of Nitinol 19
Fig 2.18 Schematic representation of the bulge occurring during bulge testing.. 20
Fig 3.1 Assembled, dissembled, cross-sectional view of the bulge testing device25
Fig 3.2 Bulge Fatigue testing arrangement components27
Fig 3.3 Circuit diagram for the microcontroller circuit for controlling the stepper motor28
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Fig 3.4 Control pins on the circuit board29
Fig 3.5 Screenshot of the Wiz-C while setting up pin controls of the microcontroller..30
Fig 4.1 IPF images & Phase maps for NiTiCuCr for: 0, 5, 10, 30 & 50 cycles @ ~10% strain35
Fig 4.2 IPF maps for B19 in NiTiCuCr for 0, 5, 10, 30, 50 cycles resp. @ ~10% strain.36
Fig 4.3 IPF images & Phase maps for NiTiCuCr for 0, 5, 10, 30 & 50 cycles @ ~25% strain.37
Fig 4.4 IPF maps for B19 in NiTiCuCr for 0, 5, 10, 30, 50 cycles resp. @ ~25% strain.38
Fig 4.5 IPF maps for B2 in NiTiCuCr for 0, 5, 10, 30, 50 cycles resp. @ ~25% strain39
Fig 4.6 Grey Scale maps for NiTiCuCr for 0, 5, 10cycles resp.@ ~25% strain39
Fig 4.7 Variation in fraction of martensite for different strains.40
Fig 4.8 X-ray graphs at ~10% strain for various cycles & at ~25% strain for 20 cycles ...41
Fig 4.9 Screenshot of the interface while using GOM...43
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List of Tables
Table 3.1 Compositions of the alloys being used...24
Table 3.2 Specification of the device.27
Table 4.1 Deformation data obtained from ARAMIS44
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Chapter 1
Introduction
The development of new materials is critical for applications that need properties, or
combinations of properties not available in existing materials. Shape memory alloys (SMA)
are a good example of such novel materials, where the functional characteristics, such as
shape memory effect and superelasticity, are exploited through the interplay of structure and
properties. Shape memory alloys represent one subset of a class of materials called
smart/active materials, where, their functional capabilities arise due to distinctive
combination of various physical parameters, such as mechanical, thermal, optical, electro-
magnetic, and are usually accompanied by a change in crystal structure.
The three major types of shape memory alloys are the copper-zinc-aluminum-nickel,
copper-aluminium-nickel, and nickel-titanium (NiTi) alloys but Shape-memory alloys
(SMAs) can also be created by alloying zinc, copper, gold, and iron. They have the ability to
return to a previously defined shape when heated past a set transformation temperature
following deformation. Many SMAs also display superelastic or pseudoelastic behavior
where large deformation can be recovered on unloading. The NiTi alloys have greater shape
memory strain (up to 8 % versus 45% for the copperbased alloys), tend to be much more
thermally stable, have excellent corrosion resistance and also higher ductility. These
properties make SMAs, and in particular nickeltitanium (Nitinol), attractive for a variety of
applications. Important amongst these are actuators, stents, guidewires and other biomedical
applications in which fine and intricate design structures are subjected to rather complex
deformations[1].
The deformation is recovered in SMAs because it is accommodated by martensitic
phase transformation and transformation twinning/detwinning instead of crystallographic
slip. They undergo a martensitic phase transformation from a high-temperature, high-
symmetry austenite state (cubic) to a low-temperature, low symmetry martensite
(monoclinic) state. The change of symmetry gives rise to multiple variants of martensite in
order to maintain zero distortion of the habit plane and formation of transformation twins
during the process. Superelastic behavior arises when the material is deformed at a
temperature sufficiently above the martensite to austenite transformation temperature. The
applied stress causes a shift in martensite start temperature, and deformation is caused by
stress-induced austenite to martensite transformation. However, martensite is unstable at this
temperature and transforms back to austenite on unloading, hence recovering the
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deformation. This mechanism of transformation is reasonably well understood in single
crystals but is poorly understood in polycrystals.
Though extensive research has been carried out on fatigue behavior of SMAs, only
few studies have made an attempt to find the exact microstructural changes and the phases
accumulating as a result of irreversible processes during the process of transformation duringmechanical fatigue. Keeping this in view, mechanical fatigue experiments on a NiTi alloy
were conducted so as to obtain the microstructural evolution in fatigue of NiTi alloys.
Though austenite to martensite transformation during loading is expected to get completely
reversed during unloading, accumulation of defects in the lattice hampers reversible phase
transformation thus leading to deteriorating superelastic or shape memory response [2]. Our
objective was to monitor changes in microstructure that occur with increasing cycles, and
correlate them with residual martensite content in unloaded samples. This would help us
understand the effect of microstructure on fatigue behaviour of shape memory alloys.
The experimental work was carried out in three different stages. Firstly, the miniature
bulge fatigue testing device, developed earlier by Edul Patel [3], was automated so as to
provide control over the strain applied, and to make it feasible to subject samples to a large
number of loading-unloading cycles. Secondly, bulge fatigue testing and microstructural
evolution studies, using EBSD and XRD, were done by obtaining microstructure with
increasing cyclic loading at constant strain. Thirdly, strain measurements were calculated for
the varying applied strains and number of cycles of fatigue using GOM (ARAMIS) software.
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Chapter 2
Literature Survey
2.1 Introduction to Ni-Ti SMAs
The NiTi shape memory alloy (SMA), Nitinol, is widely used in biomedical,
structural, aerospace engineering etc due to its superior performance relative to other SMAs.
There are two characteristic effects exhibited by SMAs viz. shape memory effect (SME) and
superelasticity (SE) or pseudoelasticity (PE). Because of its shape memory properties,
Nitinol has been used for applications such as pipe couplings, actuators, dental & medical
applications like stents, surgical instruments, orthopedic components, etc. All these
applications involve repetitive loading, hence it becomes important to have knowledge
regarding Nitinol fatigue, factors affecting it, and ways to improve fatigue-life of the
material.
Shape memory effect and superelasticity are unique properties of certain alloys
systems that arise from a (reversible) thermo-elastic behavior of the alloy that has its basis in
temperature-induced diffusionless, solid-solid, first-order transformation (high-temperature
austenite low-temperature martensite) involving a change in crystalline symmetry
Fig 2.1 Crystal structure of (a) cubic parent austenite phase (after the British scientist Sir W.
C. Roberts-Austen, 1898) and (b) monoclinic low temperature martensite phase (after the
German Scientist Adolf Martens, 1890) [4]
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Fig 2.2 Schematic illustration of SME. Af & Mf are austenite & martensite finish temps. [5]
Above the austenite finish temperature (Af), the parent material is called austenite
and has a cubic structure. Upon cooling below the martensite start temperature (Ms), the
crystal structure changes to a low-symmetry, monoclinic martensite structure; this
martensitic transformation is reversible upon heating. Below the martensite finish
temperature (Mf), the alloy is completely martensitic and is termed as thermally-induced
martensite (TIM). TIM is also called self-accomodating martensite because it has a twinned
structure so as to have zero macroscopic strains on average. When the TIM is deformed by
an external stress, the shape change is accomplished by detwinning i.e. by the
transformation of twinned variants to a common variant favoured by the applied stress. Upon
heating above the austenite finish temperature, Af, martensite transforms back to the
austenite phase, in the process reverting to the original (undeformed) shape as shown in
schematically in Fig 2.2. Thus the material exhibits shape memory effect. In contrast, when
the austenite phase is deformed by external stress within the temperature range Af < T < Md,
the austenite undergoes a stress-induced martensite (SIM) transformation. Upon removal of
the load, however, the martensite structure reverts back to the austenite phase, since austenite
is the more stable phase within this temperature window. This is termed as the
superelasticity if the specimen recovers all of the loading strains; partial recovery of strain is
termed pseudoelasticity [5].
In principle superelastic SMAs would be ideal for repetitive loading-unloading
applications, provided the strain is small enough so that martensite does not undergo plastic
deformation. But in practice, Nitinol devices suffer from several forms of fatigue damage
that range from component shape change to catastrophic fractures. It has been found that
mechanical working and heat treatment significantly affect the behavior of Ni-Ti SMAs
implying that there exists a correlation between the microstructure and shape memory effect
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exhibited. Hence, microstructure studies for enhanced commercial applications remains a
good motivation for understanding the deformation mechanism in these materials during
fatigue.
2.2 Martensitic Transformation
Martensitic transformations are displacive, diffusionless transformations during
which the atoms execute a small, well-defined movement, resulting in a change in lattice
structure and a shape change. The lattice structure of the resulting martensite has orientation
relationship to the lattice structure of the parent phase. The austenite martensite interface
plane has been shown to be an undistorted plane, called the habit plane.
2.2.1 Diffusionless nature of the transformation
In a martensitic transformation, individual atoms execute well-defined and correlated
movements, where the displacement of each atom is less than one interatomic distance. The
martensitic structure is the result of a lattice transformation entirely without atomic diffusion.
This is completely different from some diffusion-controlled solid state transformations in
which atoms undergo random diffusion movements of a relatively long range nature [6].
It has been well established by Bain in 1924 that upon biaxial expansion of the lattice
constant in the (100) plane, a FCC solid may transform very rapidly into a BCC or BCT
phase through relaxation of the interlayer spacing along the perpendicular axis c, as shown in
figure 2.3. This is known as Bain distortion.
Fig 2.3 Bain Distortion in FCC to form BCT structure [6]
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(T) orientations are opposite in sense thus resulting in an undistorted plane in an average
sense. In BCC SMAs, 24 variants are possible.
Fig.2.5 Schematic representation of the interface. The microscopic strains in the lamellae
(M) and (T) are in opposite senses[6]
Fig 2.6 Crystallographic steps for the B2 to Bl9 transformation in NiTi. (a) B2 cells; (b) B2
BCT cell; (c) Orthorombic distortion; (d) (100)B2-[011]B2 shear to monoclinic;
(e) (011)B2[011]B2 planar shuffle. [8]
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The Austenite to Martensite transformation in Ni-Ti occurs in 3 ways as shown in the figure:
Fig 2.7 Phase Transformation paths of NiTi alloys for different alloy conditions [6]
The one step transition from B2 to B19 has been reported as first order thermo -
elastic one. The R-phase transformation occurs in binary TiNi alloys, if they are cold-
worked followed by annealing at proper temperatures, so that high densities of rearranged
dislocations are left in specimens. The conditions, under which the R-phase transformation
occurs i.e two step transformation, are to suppress B19 transformation relative to R-phase
transformation by introducing precipitates or dislocations, etc. The third type of
transformation is obtained when Ni is substituted by Cu in a binary TiNi alloy. The
martensite upon the first transformation is called B19 (orthorhombic), and the second
transformation represents the one from B19 to B19.
2.2.3 Reorientation and reverse transformation
During transformation various variants are formed depending on the stress applied
however it is commonly found that these variants eventually converge to one single most
stable dominant variant. During the elimination of variants little macroscopic strain is
generated. The positions of the martensite interfaces change under the influence of stress,
creating a balance of variants whose shears best accommodate the direction of applied strain.
The interfaces between variants move to grow the most favourably oriented variants and
shrink the least favourably oriented. Some variants become dominant in the configuration.
This process creates a macroscopic strain, which is recoverable as the crystal structure
reverts to austenite during reverse transformation [8]. Figure 2.8 illustrates how the
crystallographic reversibility is automatically guaranteed by superlattice structures.
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Fig 2.8 (a) Three possible lattice correspondences in the reverse transformation of the B2 to
B19 transformation; (b) parent phase crystal structure resulting from lattice correspondence
A: a B2 superlattice the same as the pretransformation structure; (c) parent phase crystal
structure resulting from lattice correspondence B: completely different from a B2
structure[8].
Generally, the crystal structure of martensite is relatively less symmetric compared to
that of the parent phase. For this reason, the kinds of lattice correspondences between the
phases involved in the reverse transformation are restricted. In figure there are, if we ignore
the ordered arrangement of the atoms, three equivalent lattice correspondences, represented
by the rectangles marked A, B and C. Since the changes in crystal structure shown in (c)
would raise the free energy, reverse transformations along path B or C are impossible. Thus
the orientation of the parent phase crystal is automatically preserved by its ordered structure.
2.3 Pseudoelasticity and Superslasticity
Superelasticity typically occurs when a material is deformed above As, where
external applied stress causes the transformation of the parent austenite phase to a
martensitic phase. Normally, austenite is the stable phase under stress-free conditions.
However, upon the application of a critical stress, austenite starts transforming to martensite
at a constant stress, thus producing a stress plateau. The plateau (points B to C in Fig 2.9) is
a consequence of the martensite phase variants formation during transformation. The
selection of the variants depends on the loading direction and the crystal orientation in case
of a polycrystalline specimen. At a certain strain value, the stress plateau terminates, and the
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new martensitic phase now elastically deforms. However, this martensite becomes unstable
upon the removal of the stress; hence during unloading, the martensite phase reverse
transforms to the austenite phase and at zero loads the material should be entirely austenitic
with the specimen recovering its original undeformed form [9,10]. Superelasticity typically
occurs if the specimen temperature is between Af < T < Md, where Md is the highest
temperature at which stress induced martensite forms for particular value of stress. If the
temperature is above Md, the stress level needed to induce martensite is greater than the
stress required to introduce slip in austenite and hence SIM does not occur.
Fig.2.9 Different stress-strain path followed by superelasticity and pseudoelasticity
Any incomplete recovery during unloading in the stress-strain curve is termed
pseudoelasticity. In some materials, deformation of the austenite phase well above Md
(where SIM is not possible) leads to the formation of twins that are unstable and hence there
is a driving force to return to the original condition by the shrinking or disappearance of the
twins during unloading. This type of mechanical twinning disturbs the lattice ordering and is
therefore different from conventional twinning; it is termed pseudotwinning. Upon
unloading, the material attempts to return to the preferred lattice ordering by shrinking of the
twins [11,12]. This is depicted by the non-linear unloading of the stress-strain curve in
Figure. Few other materials that are in their martensitic state also exhibit twinning
pseudoelasticity (martensitic pseudoelasticity), where the deformation occurs by the motion
of the martensite twin boundaries.
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2.4 Mechanical Fatigue of NiTi Alloy
The mechanical fatigue behavior of Ti-Ni and Ti-Ni Cu shape memory alloys can largely be
said to depend on the stability of their pseudoelasticity (PE) curves during mechanical
cycling. The stability of PE can be evaluated or characterized by the residual elongation
remaining after the specimen is unloaded, the critical stress needed for martensite to start
forming, and the hysteresis curve which is a measure of the energy dissipated in one cycle
[13]. The stability of these characteristics is affected by the test temperature, the nickel
content and the previous heat treatment of the alloy. If the test temperature is chosen close to
Af, stability of PE stress-strain diagram is achieved easily because the residual deformation
after unloading is lowest. Also, if the critical stress for slip is high and the alloy readily
undergoes cyclic strain hardening, then residual elongation after unloading decreases as the
number of cycles increase, and hence the cyclic stress-strain diagram is more rapidlystabilized. For increasing the critical stress for slip, higher nickel content and suitable heat
treatment can induce dislocations and precipitation hardening can be done resulting in
reduced residual deformation during fatigue.
Fig 2.10 Stress-strain curves (hysteresis curves) during cyclic loading with number of cycles
The hysteresis loop observed in stress-strain diagram has been said to be result of
dissipation of the non-chemical irreversible energy that arises due to the interfacial friction
between adjacent martensite variants during their reorientation process [14]. When stress is
applied, there are certain martensitic variants that are favored for growth whereas others are
reoriented, leading to gradual dislocation accumulation at the interface between different
martensite colonies. The hardening observed during cyclic loading is related to this
accumulation. With increasing cycles the width of the hysteresis loop decreases, indicating
decrease in ability of material to undergo reversible transformations. The narrowing of loops
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represents decrease in the area inside the loop which is the energy dissipated in each cycle
[15]. The reason stated for this is that with increase in stress range the volume fraction of
detwinned martensite increases and the proportional energy loss of the detwinned martensite
is only half of the twinned martensite, as was observed by Huang and Lim.
Fig 2.11 Stress-strain curve for same no. of cycles of loading but at different stresses [15]
For comparison of effect of stress amplitude, Fig 2.11 shows the stabilized stress
strain hysteresis loops generated at various stress amplitudes, all at the 100th fatigue cycle. At
all the stress ranges, the loops have relatively narrow width with near-linear loading andunloading response. With increasing stress amplitude, the hysteresis loops move to the right
on the strain axis thus indicating higher amounts of strains accumulated in the SMA [10].
This shows that with increasing the stress amplitude the amount of irreversible martensite
also increases leading to strain accumulations.
Fig 2.12 Accumulated plastic strain with increasing no. of cycles for different stresses[15]
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Consider Fig 2.12 where the effect of stress amplitude on the accumulated plastic
strain, as a function of the number of fatigue cycles is shown. It can be clearly seen that the
strains are much higher for same number of cycles for higher stress amplitude as has been
discussed earlier. It can be seen that plastic strain increases rapidly between 10th and 20th
cycles before reaching a plateau value that is maintained until failure. The initial strain
results from a combination of stress-induced growth of one martensite variant at the expense
of an adjacent, unfavorably oriented one, as well as stress-induced reorientation of
martensite and twin boundary migration within a martensite variant. Due to such
adjustments, dislocation density increases during cyclic deformation. It is believed that
internal plastic deformation is necessary for martensite reorientation in polycrystalline
matrices because orientation mismatch exists among the preferential variants of martensite in
neighboring grains [16]. Therefore, the interface between any two martensite variants
becomes highly strained, which in turn makes dislocation based deformation difficult. This is
possible reason stated for the observed stabilization at higher N.
It has been observed that the energy dissipated i.e. area under the hysteresis loop
goes on decreasing with number of cycles which implies that the damping capacity of the
material goes on decreasing with progressive cycling. Also, decrease in recoverable energy
i.e. the area within the reverse transformation curve decreases with increase in the number of
cycles.
2.5 Factors Affecting Mechanical Fatigue Behavior
2.5.1 Composition Effect
As the nickel content increases, Ms decreases and the transition from shape memory
effect to pseudoelasticity shifts towards the lower temperature region. Also, the critical stress
for slip, for inducing martensite in austenite, rises with increasing Ni content and results in
reducing the growth rate of residual deformation due to retained martensite as the number of
cycles increases and support stabilization of the cyclic stress-strain diagram. This increase is
attributed to solid solution hardening and to some extent also to the precipitation of fine
Ti3Ni4 particles [18]. The greater deformations in lower nickel alloys i.e. less hardened
alloys are ascribed to the fact that that their dislocations offers only slight resistance againstthe growth of preferentially oriented martensite variants.
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It has been stated that Cu addition to NiTi alloy prevents Ti3Ni4 precipitation, and
results in a narrow transformation hysteresis, more constant Ms temperature and superelastic
plateau. The austenitic transformation (Af) of nickel/titanium alloys generally increases with
copper content. A disadvantage of most Ti-Ni-Cu alloys is that the transformation
temperatures do not decrease below room temperature. The Ms above room temperature
does not allow complete Austenite at room temperature. In order to decrease the austenitic
transformation temperature, without substantially affecting its superelasticity and SME, the
addition of Cr, W, Mn, Fe, Co and Al is done [17]. It is believed that the addition of 0.5 to
2% Fe and upto 1% Cr will reduce the Af temp of a NiTiCu alloy to below 30oC. Following
is the relationship for obtaining ternary alloys of NiTiCu while retaining superelastic
properties at temperatures below 35oC. The amount of the additional element X is not greater
than approximately 5%, preferably not greater than about 3%.
(Ti50-a/Ni50-b/Cua+b)100-c/Xc
where, a=0-10%, b=0-20%, c=0-5%, X= V, Cr, Mn, Fe, Co, W, Al
2.5.2 Effect of Thermo-mechanical Treatment and Temperature
Any solution annealed microstructure in cyclic loading does not exhibit fullyrecoverable superelastic strains, i.e. it exhibits irreversible strains that cannot be recovered
either by unloading or heating. This has been shown to be due to the ease of slip in the
austenite phase that leads to partial pseudoelasticity. Thus, in order to improve the SE
properties, the critical stress for slip has to be increased through any of the following
methods: 1. work hardening, 2. grain-refinement, 3. precipitation-hardening or a combination
of these. The grain-size effect on the pseudoelastic behavior of NiTi shows that refinement
of grain size improves pseudoelasticity. Following are the thermo-mechanical treatment used
for NiTi alloys:
Cold-work + Stress relieving Annealing:
It has been seen that samples cold worked and annealed at 400oC not only exhibit large
superelastic strains, but also the best SE and SM characteristics. The cold-worked alloy
exhibits large amount of tangled dislocation networks. The specimen annealed at 400oC
shows re-arranged dislocations, i.e., recovery takes place. However, the annealing treatment
at 400oC does not recrystallize the alloy. These heat treated samples exhibit a clean
martensitic transformation and also maintain sufficient strength due to the re-arranged
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dislocations. The specimens annealed at 400oC exhibited superior superelasticity than the
specimens annealed at 500oC, in which recrystallization takes place. The specimens annealed
at 600oC exhibits grain growth following recrystallization, and superelastic behavior is
inferior [18].
Precipitation hardening:
A solution-annealed alloy aged at about 600oC exhibits superelasticity, but in a very
narrow temperature range. In comparison, specimen aged at 500oC exhibits superior SM and
SE characteristics, with a large superelastic temperature range. This can be ascribed to a
high-density of precipitates, increasing the critical stress for slip.
Aging at 500oC produces high density of small sized Ti11Ni14 precipitates, whereas at
600oC, the precipitates are larger and density is lower. At 700oC, the precipitates are not
observed at all. is the transformation order for
precipitates, but since Ti11Ni14 phase is the only desired precipitate, because of its coherency
with the parent phase matrix, for increasing the pseudoelasticity, time of the transformation
must be taken care of [18].
Fig 2.13 TTT diagram describing aging effect on alloy Ni52Ti48 [18]
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Work-hardening + precipitation-hardening:
Both work-hardening and precipitation hardening has been shown to improve the SE and
SM characteristics. It has been further shown that combined usage of both types of hardening
mechanisms is more effective to improve the critical stress for slip. This treatment is
provided when SE is to be achieved at higher stress levels. The recovery temperature forcold-worked NiTi alloys is between 400oC and 500oC. Aging heat treatment of a cold
worked NiTi alloy is likely to produce a complex microstructure containing large densities of
dislocations and precipitates that are interwoven in such a way that precipitations act as
obstacles for dislocation movement and may hinder the recovery process [18].
2.5.3 Effect of Mean Strain
Mean stress and mean-strain determine the phase of the material in superelastic
specimens. Depending on the mean strain, a specimen may contain austenite (A), martensite
(M), or both phases and different deformation modes are associated with each of these cases.
Fig 2.14 Quasi-static Stress-Strain Curve for NiTi [22]
During loading of specimen, austenite phase exists at strains lower than f. As the
strain reaches upper plateau region transformation from austenite to martensite occurs. So a
mixture of austenite and martensite exists till strain reaches f+t. Further straining causes
complete transformation to martensite followed by elastic and plastic deformation. During
unloading, martensite remains stable till strain is reduced to r and then transformation to
austenite starts for strains in the lower plateau region. The difference in the mixture of
martensite and austenite in this region as compared to that in upper plateau is the volume
fraction of the phases present. Transformation to austenite occurs with some residual
martensite at strains lower than r-t. Now if a small value of strain is superimposed on a
fixed value of strain then it can either trigger forward or backward transformation.
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2.6 Microstructure during Fatigue
Limited work has been done on the evolution of microstructure during fatigue of
SMAs. Though some work has been reported on the microstructure, it has focused on the
study of growth of residual martensite phase during cyclic deformation.
From the microstructures shown in figure, it was concluded that some residual
variants of martensite occurs after cyclic loading in some grains but not in others. The reason
for such a behavior has not been mentioned. It was found that the same variants of martensite
get activated in each cycle but the spatial position varies from cycle to cycle. Different
variants of martensite may form in each cycle and it may form in different grains in
successive cycles.
(a)
(b)
Fig 2.15 (a) Accumulation of localized plastic deformation within the grains upon cyclic
load. Identical locations imaged on virgin specimen and after four different cycles, specimen
fully unloaded. (b) Micrographs of activated variants at 2% strain in one set of grains at
different cycle numbers (cycle 1, 6 and 10 from left to right) [14]
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Fig 2.16 Microscope images at strains 0%, 2%, 4%, 10% showing full transformation [14]
The above microstructure shows that even at 100% transformation it is not necessary
that there will be 100% martensite in the grain that are favourable for martensitic
transformation. (*The 100% transformation is said to be the point at which plateau of the
stress-strain curve cease to be flat and rises upwards due to plastic deformation of
martensites formed.) Also the grains that are unfavourably oriented never transform. As the
transformation begins in a grain martensite variants increase but at some higher stress, a
grain adjacent to the transformed grain gets activated due to local increase in stress and
hence instead of further transformation in the first grain, transformation to martensite begins
in adjacent grain. Due to this sequenced transformation behavior, variants are restricted in
each grain in turn and unable to transform fully, in contrast to what is seen typically in single
crystals.
2.7 Characterization techniques and testing methods
2.7.1 Differential Scanning Calorimetry
DSC is a thermal analysis technique in which the difference in the amount
ofheat required to increase the temperature of a sample and reference is measured as a
function of temperature. The basic principle underlying this technique is that when the
sample undergoes a physical transformation such as phase transitions, more or less heat will
need to flow to it than the reference to maintain both at the same temperature. By observing
the difference in heat flow between the sample and reference, differential
http://en.wikipedia.org/wiki/Heathttp://en.wikipedia.org/wiki/Temperaturehttp://en.wikipedia.org/wiki/Phase_transitionhttp://en.wikipedia.org/wiki/Phase_transitionhttp://en.wikipedia.org/wiki/Temperaturehttp://en.wikipedia.org/wiki/Heat -
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scanning calorimeters are able to identify transformations. The result of a DSC experiment is
a curve of heat flux versus temperature or versus time.
Fig 2.17 Shows a typical DSC scan on a sample of Nitinol [24]
The data is analyzed to report the Austenite start, peak and finish (As, Ap, Af) plus
the Martensite start, peak and finish (Ms, Mp, Mf). Typical data in fig. show that the
transition is both reversible and hysteretic. The transformation temperature hysteresis in the
transition on heating and cooling depends on the exact percentages of nickel and titanium in
the alloy. Typically, the magnitude of the hysteresis is reported as the difference between Ap
and Mp and in this case is 30.14C. Typical values of the hysteresis for binary Nitinol
samples are between 25-50C [24]
2.7.2 Bulge Testing
Bulge test is a versatile characterization method capable of determining a complete
set of material properties of thin films under various stress conditions. It is based onmeasuring the deformation of a thin specimen under an applied pressure. The obtained
pressure-deformation behavior is then utilized to extract meachanical properties of thin film
samples. In this method, a thin specimen is deformed by means of pressure application
which can be done using various available methods like hydroforming using oil or water, by
means of punch or in case of miniature bulge testing using a spherical headed screw which
acts like a punch. This method can also be applied to SMAs in order to study the biaxial
stress-strain behavior as well as fatigue.
http://en.wikipedia.org/wiki/Calorimeterhttp://en.wikipedia.org/wiki/Calorimeter -
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Two major advantages associated with bulge test are the ease of specimen handling
and the capability of imposing various loading conditions. These cannot be obtained by other
thin film testing methods such as nanoindentation, substrate-curvature technique, and
microtensile testing.
Fig 2.18 Schematic representation of the bulge occurring during bulge testing and direction
in which pressure is exerted [27]
If we assume that the sample bulges spherically, the stress and strain in the thin specimen
may be considered uniform across the width, independent of whether the film deforms
elastically or plastically, and are given by
Elastic and plastic global stress:
Eq.1
Elastic and plastic global strain:
Eq.2
When the deflection is much smaller than the membrane width, i.e. h
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2.7.3 Electron backscatter diffraction (EBSD)
Electron backscattered diffraction (EBSD), also known as backscattered Kikuchi
diffraction (BKD) is a microstructural-crystallographic technique used to examine the
crystallographic orientation of many materials, which can be used to reveal texture or
preferred orientation of any crystalline or polycrystalline material.
Atomic layers in crystalline materials diffract the accelerated electrons from the
primary beam of scanning electron microscope. These diffracted electrons can be detected
when they impinge on a phosphor screen and generate visible lines, called Kikuchi band.
These band pattern are effectively projections of the geometry of the lattice planes in the
crystal and are capable of providing direct information about the crystalline structure and
crystallographic orientation of the grain from which they originate. This pattern is then
compared with the crystallographic information for phases of interest from the database.
Indexing of the lines then gives us the phases present and also allows us to perform analyses
on polycrystalline aggregates. It can also be applied to crystal orientation mapping, defect
studies, phase identification, grain boundary and morphology studies, regional heterogeneity
investigations, material discrimination, microstrain mapping, and physico-chemical
identification [28].
2.7.4 GOM (ARAMIS) Software:
Aramis is an optical measurement technique used for 3D deformation analysis.
ARAMIS is a non-contact and material independent measuring system providing for static or
dynamically loaded test objects, accurate 3D surface coordinates, 3D displacements and
velocities, surface strain values (major and minor strain, thickness reduction), etc.
In Aramis, CCD cameras are used for recording images of a sample undergoingdeformation. For each stage of load, this system calculates 3D coordinates of the object
surface on the basis of digital image processing and thus calculates 3D displacements and
strain.
In this 3D image correlation technology, two cameras catch the same image and by
the combination and correlation of these two images 3D strains are calculated. A random or
regular pattern with good contrast is applied to the surface of the test object, which deforms
along with the object. The deformation of this structure under different load conditions is
recorded by the CCD cameras and evaluated. The initial image processing defines unique
http://en.wikipedia.org/wiki/Crystallographyhttp://en.wikipedia.org/wiki/Crystallinehttp://en.wikipedia.org/wiki/Phase_(matter)http://en.wikipedia.org/wiki/Phase_(matter)http://en.wikipedia.org/wiki/Crystallinehttp://en.wikipedia.org/wiki/Crystallography -
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correlation areas known as macro-image facets, typically 5-20 pixels square, across entire
surface area [29]. The center of each facet is a measurement point that can be thought of as
an extensometer and strain start point. These facets are tracked in each successive image
with sub-pixel accuracy. Then the coordinates of the entire surface are precisely calculated
and compared with the undeformed image to get the 3D shape of the component, the 3D
displacements, and the plane strain. Also, in cases where images from the same region are
available with sufficient surface features to meet required conditions, there is a provision in
Aramis to upload image series in various stages so as to calculate displacements and strains
in the specimen.
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Chapter 3
Experimental work and Results
3.1 Material Preparation
Two NiTi alloys have been chosen for the study viz. NiTi and NiTiCuCr. It has already been
discussed that the replacement of Ni with Cu increases the pseudoelasticity of the material
and that of Cr decreases the austenite formation temperature, hence such a combination was
chosen for studies. The composition of these alloys is as shown below:
Table 3.1. Compositions of the alloys being used:
(in atomic %) Ni Ti Cu Cr
Alloy 1 50.8 49.2 - -
Alloy 2 45 49.7 5 0.3
Alloy Preparation: Alloys were prepared by mixing appropriate amounts of the
elements in their pure form and melting in vacuum arc furnace. Repeated melting i.e. about
6-7 times was carried out to ensure homogeneity of the alloys. The material obtained was in
the form of buttons of 50 gms, each of which was then hot rolled at 950o
C to form strips.
Rolling and Heat treatment: Reduction in thickness from 10 mm to 0.7 mm was carried out
in about 24 passes with approximately 9% reduction in each pass at a temperature of around
950oC. Solution annealing was then carried out in a muffle furnace at 950oC for 20 minutes
to obtain completely homogenized stress free alloys. The samples were water quenched after
annealing.
Further heat treatment, on an experimental basis, was carried out on Ni50.8Ti49.2 alloy in orderto precipitate Ni14Ti11 with smaller size and higher densities, as per the TTT diagram by
Nishida, Wayman and Honma [18]. The solution annealed alloy was aged at 550oC for 1hr
followed by water quenching. Since this treatment has been earlier tried and tested and has
worked as expected, it was carried out on half of the Ni50.8Ti49.2 material in inert gas
environment by encapsulating the material in quartz tube.
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Thus the samples used for studies are
(a) Ni50.8Ti49.2, solution annealed
(b) Ni50.8Ti49.2, solution annealed + precipitation hardened (aged, 550oC, 1Hr)
(c) Ni45Ti49.7Cu5Cr0.3, solution annealed
NiTiCuCr was not aged as there will be no changes in the phases present i.e. no precipitation
will be observed in alloy even after ageing because there is no excess of Ni available in the
alloy to form precipitates.
Specimen Preparation
From the rolled strips, 7 mm X 7 mm pieces were cut. For metallographic studies as
well as for mechanical fatigue experiments, the thickness was reduced from 0.7 mm to 0.25
mm by grinding and polishing. Polishing of samples was carried out using SiC emery papers
of different grits and diamond polish followed by electrochemical polishing in order to get a
highly polished mirror-like surface free from scratches and pits. These samples were
electropolished using Lectropol polishing machine at 16 Volt for 15 seconds at 0C in a 20%
perchloric acid solution in methanol.
Characterizarion Instruments used:
All Electron backscattered diffraction (EBSD) measurements were carried out on a
FEI Quanta-200 HV scanning electron microscope (SEM) equipped with a TSL OIM
analysis unit. The Kikuchi patterns were generated at an acceleration voltage of 20 kV, and
recorded by means of a camera. A crystallographic orientation map is produced by scanning
over a selected region of the sample by an electron beam. The resulting Kikuchi patterns are
indexed and analysed automatically. An image quality (IQ) parameter and a confidence
index (CI) is recorded for each Kikuchi pattern. All strain measurements were carried out
using ARAMIS, an online measurement technique from GOM software. The subset size and
subset step were carefully selected for the measurements. XRD patterns were obtained using
Pananalytical Xpert X-ray diffractometer. Analysing was done using Xpert Highscore and
Xpert Stress Viewer.
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3.2 Bulge Fatigue Testing
3.2.1 Device Design
The bulge test, in which a thin specimen is pressurized and its out-of-plane deformation or
bulge is monitored, is a well-accepted methodology for obtaining the stress-strain behaviour
of thin samples subjected to biaxial loading. The main advantage of using bulge test to study
fatigue in shape memory alloys is that the setup that we have designed allows us to test a
sample that is small enough that microstructure of a pre-defined region of the sample can be
seen repeatedly after cyclic loading. This gave us direct observation of microstructure
evolution with fatigue cycles, and we could correlate it with the residual strain. Also, it is
possible to estimate the total strain from bulge height when loaded and residual strain from
the height of unloaded sample assuming spherical bulge, and thus we can even correlate the
recovery after desired number of cycles. The device used for the bulge fatigue testing was a
modification of the one designed and developed by Edul Patel [3].
(a) (b)
(c) (d)
Fig 3.1 (a) Assembled, (b) dissembled, (c) cross-sectional view
and (d) photograph of bulge testing device
As can be seen from the diagram, it consists of a nut, two washers, bolt having hole
with threading on the inside and screw. The sample with thickness around 0.25 mm is
clamped by means of two washers. We found that the tip of the screw, though relatively
blunt, was still sharp enough that after repeated loading cycles, the sample had undergone
severe plastic deformation at the point of contact instead of uniform bulging. So, it was
replaced by another screw having a steel ball at its tip, which ensured that bulging of the
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sample takes place. This kind of screw, with steel ball and without plunger inside, though is
available in market but is scarce.
Table 3.2: Specification of the device
Specifications
Original Earlier Modified
Max sample size 7 mm sq 7 mm sq
Screw pitch .6 mm .7 mm
Least bulge height
attainable .1 mm adjustable
Bulge Diameter 2 mm 2 mm
Screw Diameter 2 mm 3 mm
3.2.2 Procedure for the bulge test
1. Sample was first cut into a 7 mm x 7 mm piece, thinned to 0.3 mm and then electropolished.
2. Area of 300 x 400 microns was marked on the specimen using micro-indenter3. The marked area in the undeformed sample was scanned using the EBSD system4. Sample was fitted in the bulge device and desired strain applied for 5 cycles5. Sample was removed from the device and the same marked area was scanned using
EBSD to observe changes in microstructure
6. Steps 4 and 5 were repeated for 10, 30 and 50 cycles
3.2.3 Automation of the set-up
In the first design of the device, the bulging screw was rotated manually to impose
the desired strain. But this gave poor control over the amount of strain applied, and was not
suited for multiple cycling experiments. Hence the set up was automated so the magnitude
of strain could be kept constant over multiple cycles.
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In automated set-up, cyclic loading is effected by means of a screw driven by stepper motor.
Details of the setup are shown in fig 3.2. Coupling the motor with the screw was a major
concern while developing the set-up. The important considerations were: easy detachability
of the screw from the motor, efficient transfer of load from motor to screw and ease of
handling. This difficulty was overcome by developing a custom-made head that was attached
to the shaft of the motor which could be fixed in the notch provided at the tail-end of the
screw. Sufficient space is provided for the in and out movement of the shaft-head in the
notch. This arrangement works as coupling between the mechanical part of the setup and
electronically controlled part. The motor is in turn controlled by a microcontroller.
Fig 3.2 (a) Coupling arrangement between the stepper motor and mechnical arrangement,
(b) Bulge Fatigue testing arrangement components
The head of motor shafts induces forward and backward movements in the screw. Now in
order to control the strain and number of cycles during fatigue, the movement of the motor
shaft is controlled using a microcontroller. The microcontroller circuit, for controlling motor
rotations, consists of PIC 16F877A, custom made driver A3982 and pull up resistor
arrangements. PIC 16F877A is a 40 pin, CMOS FLASH-based 8-bit microcontroller and 8
channels 10-bit Analog-to-Digital (A/D) converter, which works on 14-bit instruction
programming language. Earlier another IC i.e. PIC 16F84 was tried but due to technical
difficulties like requirement of another circuitry for analog to digital conversions, etc.
designing was complex. The circuit diagram for microcontroller circuit and schematic design
for entire setup is as follows:
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Fig 3.3 Circuit diagram for the microcontroller circuit for controlling the stepper motor
In the present case, a program for controlling the number of rotations and number of
cycles (for both forward and backward direction) has been fed in the PIC by means of an IC
programmer. Since there are no standard drivers available for the stepper motor circuit, a
custom driver for providing actual control signals to the stepper motor is used, which was
developed by Nex-Robotics. This is of great importance in the working of the circuit as a
precisely controllable signal is to be provided. With the help of switch provided inputs for
number of rotations and number of cycles can be fed, in binary form. This can even be
converted into decimal digital input The stepper motor that has been used has specifications
of 200 steps per rotation i.e. 1.8 degree of turn per step and torque ratings of 1.3 kg. Thepower supply for the entire assembly is provided using 450 W SMPS.
Fig 3.4 Control pins on the circuit board
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Program used for controlling the microprocessor is written in Wiz-C. WIZ-C
Professional is a complete PIC microcontroller (MCU) development, compiler, assembler
and simulation package for the C language. In this we have to select the kind of
microprocessor we have to program. Each microprocessor has a number of components
within it that have to be connected to the other components of the circuit. When each
component is selected it can be connected to the MCU pins by clicking the picture of the
component pin and then clicking the MCU pin - they will be joined. Pins can be user named
as well, to make the code easier to understand. Some components can only be connected to
certain pins - they will connect themselves automatically.
Each component has a list of parameters. In the case of our serial element this includes the
bit rate. The bit rate is selected from a drop down list, now when the application is generated
it will automatically configure the serial element for this bit rate regardless of the MCU type
used or oscillator frequency. Finally according to the connections made, a program is
required for the entire assembly to operate.
Fig 3.5 Screenshot of the Wiz-C while setting up pin controls of the microcontroller
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3.2.4 Microcontroller Programs:
Program written to control all switches on the microcontroller is given in Appendix
as Stepper_main. Program written at user interface is as follows:
#include "C:\\Swapnil\\Wiz-C Projects\\Stepper\\stepper_Auto.h"
//****************************************************************************
// Interrupt handling code written here enables user to initiate and terminate the program whenever
desired by providing suitable inputs
// Note quick interrupts are used so code must be simple
// defining the variables for the program
int one_cycle; // one cycles is the degree of rotation fixed for input 1
int fr_cycle_number; // Desired no. of one cycle (i.e. 60 degrees in this case) rotations beforereversing
int fr_cycles; // Desired number of forward cycles
int revcount; // Number of reverse cycles completed
int fr_cycle_count; // Number of forward cycles completed
int cycle_count; // total of forward and reverse rotations completed
int stopflag; // Stop rotations
void UserInterrupt()
{
// Insert your code here
#asmline SETPCLATH UserIntReturn,-1 ; SETPCLATH for interrupt routine
#asmline goto UserIntReturn ; Assembler - go back to interrupt routine
}
//**************************************************************************
// Initialisation code here.
// Note that when this routine is called Interrupts will not be enabled - the
// User will enable them before the main loop
void UserInitialise()
{
//LCDClear();
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one_cycle=34; // Since motor used have unit rotation of 2 degrees hence 34 input means that
when
program is called with '1' as input it rotates by 2*34=68 degrees precisely!!!
fr_cycle_number=1; // sets the initial values as 1 to start the rotation in forward direction
fr_cycles=1;
revcount=0; // reverse rotation does not begin
fr_cycle_count=0;
cycle_count=0;
stopflag = 1; // stopflag = 1 means 'stop' command for motor
ST=0;
DI=0;
}
************************************************************************
// Insert your main loop code if required here. This routine will be called
// as part of the main loop code
void UserLoop()
{
if(stopflag==0)
{
ST=1; // command on the MCS to stop
Wait(10); // after stopping wait for 10 microseconds
ST=0; // command to enable start of motor in reverse direction than the
current one
revcount = revcount + 1;
if(revcount==one_cycle) // loop to keep increasing the number of forward cycle counts
{
revcount = 0;
fr_cycle_count = fr_cycle_count + 1;
}
if(fr_cycle_count==fr_cycle_number) // condition to terminate forward cycle rotation
{
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fr_cycle_count = 0;
cycle_count = cycle_count + 1;
DI = !DI;
}
if(cycle_count==2*fr_cycles) stopflag = 1; // condition to terminate entire program
Wait(10);
}
}
****************************************************************************
// User occurrence code is code to initiate the motor
void startmot()
{
revcount=0; // setting initial variable values
fr_cycle_count=0;
cycle_count=0;
stopflag = !(stopflag);
}
****************************************************************************
// Write values code to convert binary values and input in decimal form for no. of one cycle rotations
before reversing and no. of such sets of forward and reverse cycles
void writevalues()
{
if(fr_t)
fr_cycle_number= int(bit0+bit1*2+bit2*4+bit3*8+bit4*16+bit5*32+bit6*64+bit7*128);
else
fr_cycles=int(bit0+bit1*2+bit2*4+bit3*8+bit4*16+bit5*32+bit6*64+bit7*128);
}
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Chapter 4
Bulge Fatigue Testing Results
4.1 Microstructural Correlation During Fatigue Using EBSD
In order to study the effect of fatigue loading on the microstructure of NiTiCuCr, fatigue
tests were carried out using the set-up described in section 3.2.3. The microstructure was
obtained using EBSD in deformed conditions after varying number of cycles and was
compared with initial microstructure in undeformed condition. The study of these
microstructures was done to get an insight into accumulation of residual martensite after
cyclic loading.
The sample with thickness around 0.25 mm in electropolished condition was prepared for
the test. In order to mark a specific area for repeated observations, microindentation was
done. It was ensured that the area selected is not marred by any abnormality like dents, pits,
etc. By repeatedly scanning the same region of the sample, we expected to identify where
residual martensite forms during cyclic loading and how does the microstructure change
during fatigue cycles. Also we expected to identify whether martensite forms preferentially
in certain orientations of austenite, and whether the martensite formed has any preferred
orientations.
For performing fatigue tests on NiTiCuCr samples, constant strain and strain rate
condition was maintained. Experiments were carried out at two different strains of about
10% and 25% by controlling the amount of rotation on the screw driven by motor. The strain
rate was constant as it is defined by the speed of rotation of the motor, which was constant.
The samples were fatigued for certain number of cycles viz. 5, 10, 30, 50. Since two
different strains were used, every other condition remaining same, attempt has been made to
compare martensitic formation with increasing number of cycles of fatigue as well as for
different strains.
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(a) (b) (c)
(d) (e)
(f) (g) (h)
(i) (j)
Fig 4.1 Color coded IPFmaps (colours correspond to orientations as per the IPF shown)
(a)(b)(c)(d)(e) & Phase maps (f)(g)(h)(i)(j) for NiTiCuCr for: 0, 5, 10, 30 and 50 cycles
respectively @ ~10% strain
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Fig 4.1 shows the inverse pole figure and phase maps for the NiTiCuCr samples taken from
same area after increasing number of cycles of fatigue for strain of approx. 10%. It can be
seen that there is there is change in shape of grains gradually along with slight change in
orientation (observed by comparing color code for IPF). It can also be observed that
martensite phase formed in first few cycles was near grain boundary area but as the cycling
progressed, uniform distribution was observed throughout the area irrespective of grain
orientation or size.
(a) (b) (c)
(d) (e)
Fig 4.2 IPF maps for B19 in NiTiCuCr for 0, 5, 10, 30, 50 cycles resp. @ ~10% strain
Fig 4.2 shows the IPF of retained martensite. It appears that martensite in the
undeformed sample has orientations around (001) crystallographic axis. After 10th
cycle, a
random distribution of orientations is observed. If we compare this to the phase map in Fig
4.1, there is almost no new martensite formation after 5 cycles. After 10 cycles, martensiteis no longer present only along grain boundaries, but distributed all over the scanned region.
And this new retained martensite appears to have no preferred orien tation.
Main observation:
Amount of residual martensite formed is extremely less (1-3%) even after 50 cycles
of fatigue. This indicates that if any stress-induced martensite formation occurred
during loading, it was reverting to austenite during unloading and no significant
accumulation of defects had occurred after 50 cycles.
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(a) (b) (c)
(d) (e)
(a) (b) (c)
(d) (e)
Fig 4.3 Color coded IPF images (a)(b)(c)(d)(e) & Phase maps (f)(g)(h)(i)(j) for
NiTiCuCr for undeformed, 5, 10, 30 and 50 cycles respectively @ ~25% strain
For understanding the effect of strain on residual martensite, similar fatigue cycles
were done at a significantly higher strain, approx. 25%. The same area was observed for
grain orientation and phase changes occurring as a result of fatigue. Since there was a slight
shift in the marked area of observation and the centre of the bulge, the deformed region in
slightly shifted from the centre towards right. IPF maps in Fig 4.3 clearly show extensive
grain fragmentation after just 5 cycles. Looking at the phase maps for the same region, it is
clear that most of the fragmented grains consist of retained martensite. After 5 cycles of
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deformation, the percentage fraction of martensite is about 19% as compared to about 1% at
earlier strain (~10%). This fraction increases to 37% as the number of cycles increases to 50.
Another important observation is that some original austenite grains are still retained
after 50 cycles, and these grains have blue (111), green (101) or nearby colors (orientations).
Grains with red (001) or its nearby colors (orientations) are first ones to form retained
martensite after the first 5 cycles. The (111) and (101) orientations of the austenite have the
ability to accommodate more strain as compared to (001) orientation. Hence the martensite
variants formed in (111) and (101) orientations is able to reorient and grow but in (001) the
martensitic variants undergo plastic deformation for the same strain, thus, resulting in
retained martensite in (001) orientation whereas reversible martensitic transformation in
(111) and (101). It may be speculated that at high strains, martensite formed in (001)
oriented austenite grains is more likely to be heavily deformed and hence retained upon
unloading.
(a) (b) (c)
(d) (e)
Fig 4.4 IPF maps for B19 in NiTiCuCr for 0, 5, 10, 30, 50 cycles resp. @ ~25% strain
It can be seen that martensite has random texture, with a slight preference for (001)
orientation seen after 5 cycles. Austenite texture also appears to be more randomized after
deformation. It is speculated that the deformed region have grains of very small sizes which
are being considered while forming the IPFs. Therefore, it can be seen that the entire IPF is
covered even though only a few big grains can be seen in IPF maps.
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. (a) (b) (c)
(d) (e)
Fig 4.5 IPF maps for B2 in NiTiCuCr for 0, 5, 10, 30, 50 cycles resp. @ ~25% strain
(a) (b) (c)
(d) (e)
Fig 4.6 (a),(b)&(c) Grey Scale maps for NiTiCuCr for 0, 5, 10cycles resp.@ ~25%
strain; (d) & (e) are surface relief due to martensitic formation
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The grey scale maps for different cycles of fatigue are shown in Fig 4.6. With increasing
deformation, the bands of martensite are observed to be increasing, this is evident from the
surface relief cause on the sample surface after deformation. The density of the martensitic
needles can be seen to increase with increasing fatigue.
Fig 4.7 Variation in fraction of martensite for different strains
In current study, the amount of martensites formed during the two different strains
was a good indication of how the martensite transformation varies with varying strain. It was
found that at strain of ~10% the retained martensite in the material was very less and rate of
increase with subsequent cycling was also low (ranged in order of few percents). Whereas
when the strain increased to ~25%, the martensite percent showed a steep rise even at low
number of cycling. This suggests that upto 10% strain, samples can undergo repeated cycling
without much change in the microstructure. This is very desirable in actuators that have to
undergo many cycles. At higher strain (25%), however, even after 5 cycles there was almost
19% retained martensite indicating that reversibility of phase transformation had been
significantly impaired at higher strains.
4.2 X-Ray Analysis
While EBSD scans are a good way to see change in microstructure, there is still a
limitation on the area that can be scanned. So X-ray diffraction was used to get volume
averaged data regarding the crystal structures present in the NiTiCuCr and NiTi deformed to
10% strain. Fig 4.8 shows Intensity vs. 2 plot for samples after 0, 5, 10, 20 cycles. In Cycle
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0 (undeformed sample) only austenite peaks are seen. With increasing number of cycles,
intensity of all martensite peaks increases implying an increase in martensite content in the
sample. Other peaks such as the M peaks of (220) and (132) appear only after 10 cycles of
deformation. The martensite amount is very low even after 20 cycles in both the alloys. The
peak A(220) has decrease from undeformed to 10 cycles deformation and then further
increased suggesting martensite M(220) formation at the same orientation. Also, graphs
below suggest that more orientations of martensite form in NiTiCuCr as compared to NiTi at
lower strains but almost same at higher strains.
(a) (b)
(c)
Fig 4.8 (a)&(b) X-ray graphs for NiTi and NiTiCuCr at ~10% strain for various cycles
of fatigue; (c) X-ray graph for NiTi and NiTiCuCr at ~25% strain and 20 cycles
From the graphs, it can be seen that the martensite contents can also be seen to
increase as the amount of strain increases. When NiTi and NiTiCuCr are compared for the
amount of martensite formed seems similar but at different orientations. Thus, we can
conclude that martensite content increase with strain but the orientations of the retained
martensite varies with the alloy.
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4.3 Strain Measurements using GOM
For calculating the amount of strain caused during fatigue with varying number of
cycles, we used ARAMISa GOM software which is an image processing software capable
of optical measurements. In order to obtain strain, extremely good quality images of the
same region on the sample surface are required before and after subsequent cycles of fatigue
deformation. These images are required to have sufficient features on the surface like second
phase, precipitates, grain boundary or even scratches, etc. The contrast of these features must
stand out when compared to the parent phase or image background.
In NiTiCuCr as well as NiTi, we already had these features in the form of precipitates
randomly distributed throughout the specimen surface. In order to create the contrast, mild
etching was done using H2O:HNO3:HF:: 5:4:1 volume fraction. Microindentation was done
so as to mark the same area. Then SEM images of the undeformed sample were taken at
1200X. Care should be taken while taking the SEM images for the deformed samples atvarious cycles that the brightness and contrast of the sample should be adjusted to be as close
as possible to undeformed image. Failure to do this will mean that the software cannot detect
facet points on the image which are required for strain calculation. As a result the entire
surface of the image will not be considered for calculating strain, only the detected region
will be. Another important factor in using ARAMIS for strain calculations by SEM images is
that for the kind of surface features your sample shows, facet point and facet steps are to be
decided which can only be determined by trials. For the images used in current project, the
facet size used was 30 with step size 13 with accuracy of 67% at computation steps 3.
The steps to use ARAMIS for strain calculations are: 1) Start New project from
File on the Access Toolbar at the top of screen 2) Select 2D project; by default it is 3D
3) Enter the description of the project 4) Set the Facet Size, Facet Step, Accuracy ,
Computation Steps, etc as project parameters 5) Once the project is formed, go to Stage
in the Access toolbar on top of screen and select Input Images via Image Series 6) Press
the arrow sign to select and input image (this should be your undeformed image and should
get set as Stage0) 7) Similarly input other deformed images in order of fatigue cycle 8) Set
Stage0 as start point using Auto start point or Add Start point 9) Compute the project by
going to Project on Access toolbar and then Compute Project .
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Fig 4.9 (a) Screenshot of the interface while using GOM; (b)(c)&(d) Color maps
showing major, minor strain and thickness variation respectively. It should be noted
that software is unable to detect entire surface area. Hence calculations are from the
detected area only.
Strain calculations were done for both NiTi and NiTiCuCr at different strains viz.
0.11mm bulge height for 50cycles, 0.23mm bulge height for 10, 20 and 50 cycles.
Table 4.1: Deformation data obtained from ARAMIS
NT,
0.11, 50
NT,
0.22, 10
NT,
0.22, 20
NT,
0.22, 50
NTC,
0.11, 50
NTC,
0.22, 10
NTC,
0.22, 20
NTC,
0.22, 50
Major Strain 8.84 11.9 20.36 16.24 8.01 10.49 16.78 17.64
Minor Strain 6.01 7.47 18.45 17.041 5.78 11.04 18.45 16.76
Thickness
reduction
1.012 1.35 1.95 1.78 1.06% 1.18 1.69 1.65
(NTNiTi, NTCNiTiCuCr, 0.11&0.22 are bulge height; 10, 20, 50 are no. of cycles)
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From the table, it can be seen that the strain values obtained for both the alloys at
0.11 mm bulge, 50 cycles is lower than that at 0.22 mm bulge, 10 cycles. Therefore, it can be
interpreted that the residual martensite formed under latter conditions is higher, which was
also evident from earlier studies. Also, in general, there is an increase in strains as the
number of cycles increased for both the alloys when bulged to 0.22 mm, except for NiTi
when number of cycles is increased from 20 to 50. It is highly likely that this is because the
area chosen for studies in 50 cycles sample was away from the bulge. In the limited data that
is available, major and minor strains appear to be not too different, especially for the
NiTiCuCr samples. This sort of a spherical shape of bulge is what we had hoped to achieve
from the setup.
NiTi is showing higher percentage of deformation as compared to NiTiCuCr at
similar conditions. The irregularity in the rate of increase and decrease of strain can highly
be attributed to personal inability to decide exactly the area which is going to get bulge.
Also, the images used cannot contain the features distributed evenly throughout the surface;
hence the images used for two different deformations contains different fraction of area
detectable by the software. These are the hindrances to effective use of the method which
needs to be sorted out. But this method can be used to make the FLDs for the alloy precisely.
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Chapter 5
Conclusions and Future Scope
Conclusions
1. Automation of the bulge fatigue set-up has been successfully carried out. Now,fatigue can be carried out for desired number of cycles at desired strain with
precision and control over the deformation process.
2. The EBSD study of the NiTiCuCr alloys shows much higher amount of martensitefor higher strain when the two strains 10% and 25% are compared. Even for 5cycles
at 25% strain the amount of martensite formed is much more than for 50 cycles at
10% strain. This implies that material is safe at lower strain of 10% for 50 cycles
3. It was observed that at higher strain the grains that seem to resist deformation andresidual martensite formation are mostly 2 orientations (111) and (101). With low
confidence it can be said that the orientation (001) is the preferred orientation for
formation of martensite.
4. GOM, image processing software, has been successfully used for determination ofstrain. This method, though is showing some limitations in softwares ability to
detect entire surface area, can be effectively used for calculating strains from SEM
images when compared to strain calculations from bulge height.
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Future Scope
1. Comparative Bulge Fatigue BehaviorA comparative study on bulge fatigue microstructure can be done for better
understanding of evolution of microstructure esp. martensite accumulation in all the alloys
and effect of various factors like composition, heat treatment, etc.
2. Martensite Orientation StudyMartensitic variants formed during fatigue can be identified using SEM images by
comparing with those which have earlier been identified experimentally by Nishida et.al.[41,42]. Also this can then be further applied in identifying preferred orientation of
martensite formed; even the preferred grain orientation can be found through this analysis for
martensitic formation. If the same region after increasing cycle of deformation is observed
then reorientation, if any, can be observed.
3. Developing Forming Limit DiagramWith the use of GOM (Aramis), FLDs can be formed for different SMAs. Samples
with different dimensions are required to be made such that all strain paths can be achieved
(as is done for sheet metal forming).
4. Identifying the effect of Strain rateBy small modification in the program and circuit designed, it can effectively be used
at varying strain rates as well. Hence there is scope for carrying out all the Bulge Fatigue
Studies at different strain rate.
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3