Materials and Manufacturing Processes

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Surface integrity analysis of Nitinol-60 shape

memory alloy in WEDM

Biplab Kumar Roy & Amitava Mandal

To cite this article: Biplab Kumar Roy & Amitava Mandal (2019) Surface integrity analysis
of Nitinol-60 shape memory alloy in WEDM, Materials and Manufacturing Processes, 34:10,
1091-1102, DOI: 10.1080/10426914.2019.1628256

To link to this article: https://doi.org/10.1080/10426914.2019.1628256

Published online: 17 Jun 2019.

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MATERIALS AND MANUFACTURING PROCESSES
2019, VOL. 34, NO. 10, 1091–1102
https://doi.org/10.1080/10426914.2019.1628256

Surface integrity analysis of Nitinol-60 shape memory alloy in WEDM

Biplab Kumar Roy and Amitava Mandal
Mechanical Engineering, Indian Institute of Technology (ISM), Dhanbad, India

ABSTRACT ARTICLE HISTORY

Nitinol-60, which belongs to the group of Nickel-Titanium based Shape Memory Alloys, offers remark- Received 13 November 2018
able properties like high wear resistance, high strength, shape memory, and super-elasticity; thereby Accepted 29 May 2019
making it convenient for use in aircraft and biomedical applications. However, these properties make KEYWORDS
Nitinol a ‘difficult-to-machine’ material during the traditional machining processes. Hence an experiment WEDM; Nitinol; SCD; RLT;
based study on Wire Electrical Discharge Machining of Nitinol-60 has been executed based on the Monte-Carlo
parametric effects. This study attempts to provide the quantitative details of the machined surfaces in
terms of maximum peak to valley height, the average peak to valley height, recast layer thickness, and
surface crack density. In addition, Response Surface Methodological models of these surface parameters
along with the cutting rate have been developed. Monte Carlo simulation of the generated regression
equations is carried out to study the behavior of the models using randomly generated data. The results
show that the developed models are in agreement with the experimental data; which further indicates
that the optimal parameters are suitable for mass production.

Introduction Material removal in EDM is based on a controlled spark

erosion process in which an electrical spark is used to melt
Shape Memory Effect (SME) in Nickel-Titanium based alloys
and evaporate the work material. Analysis and modeling of
were first discovered by Buehler et al.[1] in 1965 and the alloy
EDM parameters using Cu tool and Deionized (DI) water as
was termed as NITINOL (for ‘Nickel-Titanium- Naval-
the dielectric fluid was performed by varying voltage, current,
Ordnance-Laboratory’). Although SME was discovered earlier
pulse on time (Ton), and pulse off time (Toff) and it was
in some alloys like Au- 47.5% Cd and in In-Tl,[2] they did not
concluded that peak current had a larger influence on
get much popularity as Ni-Ti based alloys get. Nitinol is
Material Removal Rate (MRR), tool corrosion, and SR.[6]
a binary, near equal-atomic alloy of Ni and Ti. Due to its
Wire Electrical Discharge Machining (WEDM) is a type of
outstanding properties like high wear resistance, high
EDM process and uses a moving wire which serves as the tool
strength, super-elasticity; it is used in many fields like aero-
electrode. This wire is fed continuously from a spool at feed rates
space, biomedical, nuclear, micro-electro-mechanical systems
ranging from 1 m/min to 20 m/min. The material is removed by
(MEMS) etc.[3] But conventional machining of this alloy is
a series of repetitive sparks between the wire electrode and the
very difficult due to its low thermal conductivity which results
electrically conductive workpiece. As there is no contact between
in high strain hardening and high tool wear.[4] Therefore,
the work-piece and the wire electrode; mechanical stresses, vibra-
non-conventional machining processes like Laser Beam
tions and chatter problems are absent. Also, the mechanical
Machining (LBM), Abrasive Water Jet Machining (AWJM),
properties of the work-piece do not affect the machinability of
and Electrical Discharge Machining (EDM) are getting atten-
the machine as long as the work-piece is electrically conductive.
tion for machining of nitinol.[3] However, the surfaces pro-
Further, WEDM is best suited for precise machining. Guo et al.[7]
duced by AWJM are generally rough due to the effect of jet
conducted a study on the WEDM of insulating zirconia ceramics
drag. Also, the dimensional accuracy of surfaces produced by
using a conductive lacquer and a Cu tape and reported that
AWJM is inferior as compared to the surfaces produced by
optimal machining characteristics were obtained at Ton = 20µs.
EDM. The surfaces produced by laser machining consist of
The cutting speed increased initially and then decreased with
heat affected zones. Moreover, tapering is also a common
respect to the pulse on time. Experimental analysis of surface
problem encountered while laser machining with high aspect
finish of meso bevel and helical gears fabricated by WEDM was
ratios. Comparative study of the recast layer formed by EDM
performed and it was reported that roughness value increases with
and laser machining shows that the white layer formed with
an increment in peak current, pulse on time, servo gap voltage,
the laser machining is relatively more uniform than that
wire feed, wire tension and cutting speed.[8] Optimization on
formed with EDM, and the surface roughness (SR) of the
WEDM process parameters was studied individually by Dhobe
laser machined surfaces is poorer than that of EDMed
et al.[9] in AISI D2 steel, Mandal et al.[10] in Nimonic C-263, Nain
surfaces.[5]
et al.[11] in Udimet L-605, and Thankachan et al.[12] in Cu-BN

CONTACT Amitava Mandal amitava03@gmail.com Mechanical Engineering, Indian Institute of Technology (ISM), Dhanbad 826004, India
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/lmmp.
© 2019 Taylor & Francis
1092 B. K. ROY AND A. MANDAL
MMC’s; and it was concluded that the MRR was mainly affected
by Ton whereas the SR was affected by both Ton and Toff. Mussada
et al.[13] studied the hardenability of the surfaces machined by
WEDM. The experiments were performed on die steel and it was
reported that the wire speed and the servo feed greatly influenced
the recast layer and heat affected zone, and the hardness values
gradually decreased from the recast layer to the base metal. The
main factors that affect the roughness values are the formation of
recast layer, heat affected zone, irregular craters, wire vibrations
and non-uniform distribution of sparks.[8]
Experimental studies on WEDM of NiTi shape mem-
ory alloy reported that an increment in the pulse-on-time
lead to an increment in the cutting rate but resulted in
poor surface roughness.[14] Also, the shape recovery effect
of WEDMed TiNiX alloys diminished slightly due to the
formation of the white layer and its thickness was found
to be inversely proportional to the pulse duration.[15] Liu
et al.[16] investigated the composition, crystallography,
and properties of the white layer (WL) formed by
WEDM of NiTi SMA and found that the WL is
a crystalline structure which consisted of two different
layers: the top layer consisted of Cu, Ni and Zn solid
solution and had FCC structure while the bottom layer
consisted of nitinol austenite phase and Ti2O3. The grain
structure of the white layer was found to be in random
order. The interrelation between the fatigue life and sur-
face integrity of Ni-Ti samples machined by WEDM
showed that the fatigue cracks tend to initiate from the
micro-voids present in the recast layer which in turn
caused a lower fatigue life.[17] Sharma et al.[18] reported
that the un-machined surface area and recast layer devel-
oped in WEDM lead to the reduction in properties like
pseudo-elasticity and shape memory of porous Ni-Ti
alloy. Changes in shape recovery ability and micro-
hardness of WEDMed surface of Nitinol-60 SMA revealed
that the white layer generated on the surface comprised of
Ti2Ni, CuZn, Cu2O, NiO metal oxides. The micro-
hardness of the recast layer and the micro-hardness
taken at a depth of 250 µm were several times more
than that of the base alloy.[19] Mwangi et al.[20] studied
the suitability of micro-EDM in machining nitinol with
respect to steel and tungsten carbide. It was observed that
nitinol was machinable by µ-EDM, but the Tool Wear
Rate (TWR) was high and the process was the slowest
as compared to steel and WC. In the study of machining
characteristics of Ti50Ni45Co5 alloy in the WEDM process,
the presence of hard surface below the recast layer and
the presence of compressive residual stresses on the
machined surface were observed.[21]
From the past literature, it can be concluded that
WEDM is suitable for precision machining of nitinol,
but the machined surfaces contain defects such as pores
and micro-cracks due to the high temperature generated
during the machining operation. The development of the
recast layer and the heat affected zone can influence the
mechanical properties and the shape recovery properties
of nitinol. Since nitinol has applications in highly sensi-
tive components like morphing wings in the aerospace
industry, stents, and implants in bio-medical; it is of
utmost importance to check the surface integrity of the
machined surfaces prior to further usage. Therefore, the
present work is focussed on the modeling and optimiza-
tion of the WEDM on nitinol with respect to surface
crack density (SCD) and recast layer thickness (RLT). In
this study, the objective is to minimize the average peak
to valley height (Rz), maximum peak to valley height (Rt),
SCD, and RLT at the optimal cutting rate. Regression
models have been developed based on the response sur-
face methodology (RSM) and Monte-Carlo simulation of
the generated model has been carried out to study the
behavior of the models.
Materials and methods
Material background
The crystallography and metallurgical characteristics of NiTi
alloy are discussed in this section. Laves and Wallbaum
assumed that the structure of the equiatomic alloy Ni-Ti was
CsCl (B2) type.[22] However, subsequent research works in the
phase equilibrium area of Ni-Ti system proved that the struc-
ture is a large cubic cell consisting of 27 sub-cells of CsCl
structure and is stable at moderately elevated temperatures
only. Nitinol exhibits austenite (parent phase) at higher tem-
peratures and martensite (product phase) at a lower tempera-
ture. While the austenite phase (B2) is highly symmetric and
has a bcc crystal structure, the martensite phase (B19ʹ) has low
symmetry and exists as a monoclinic crystal. The conversion
of the austenite phase to the martensite phase is based on
diffusionless solid phase transformation which results in
shape memory effect.[23] During the conversion from auste-
nite to martensite, an intermediate phase may be observed
which is termed as the R-phase. The crystal structure of this
phase is reported to be rhombohedral distortion. The various
temperatures that define this transformation are As, Af, Ms,
and Mf. As or austenite start temperature is the temperature
where martensite initiates to convert to austenite on heating
and Af or austenite finish temperature is the temperature
where the conversion to austenite is 100% complete.
Similarly, Ms is the temperature where austenite begins to
convert to martensite on cooling and Mf is the temperature
where the formation of martensite is 100% complete. Apart
from these temperatures, there is another temperature Md,
which is the highest temperature where martensite cannot be
activated by stress and above this temperature, the alloy is
permanently deformed.[24] One-way shape memory effect
(OWSME) is an important characteristic of Ni-Ti based
SMA. In OWSME, Nitinol is in martensite form at lower
temperatures, and due to martensitic shear, it can be
deformed quite easily.[25] It retains its shape even after the
removal of the load due to residual strain and can revert back
to its original form by heating above its transformation
temperature.[26]
Experimental details
The work material selected for this study was Nitinol-60,
which was in the form of cylindrical rods (ø = 8mm,

L = 100mm). The chemical composition of Nitinol-60 is
Ni 60%, and Ti 40% (wt. %). The experiments were
performed on “ELECTRA MAXICUT e 734” and Zn
coated brass of dia 250 µm was used as wire electrode.
In this study, deionized water was used as a dielectric
fluid.
Based on the trial experiments and machine limita-
tions, three process parameters at three levels were con-
sidered for the study: duty factor (DF) at 0.575% (Ton
= 1.10 µs, Toff = 190 µs), 0.701% (Ton = 1.20 µs, Toff
= 170 µs), 0.892% (Ton = 1.35 µs, Toff = 150 µs); gap
voltage (GV) at 40, 50, 60 volts and deionised water
dielectric flow rate (FR) at 2, 4, 6 Litres per minute
(LPM). The constant variables considered are wire feed:
1 mm/min and wire tension: 600 kgf. Each experimental
run was performed twice to find the mean values of the
responses. In each experiment run, the machining time
was noted using a stop-watch. The cutting rate was cal-
culated using Eq. (1). Surface roughness was measured
with a roughness tester (Mitutoyo SJ-210). The sampling
length was kept at 0.3 mm and cut-off length was kept at
2.5 µm. Five readings were taken at different locations for
each specimen and the arithmetic average was taken for
further analysis. The surface microstructure was studied
from images taken by FESEM (SUPRA 55). Prior to the
FESEM test, the machined surfaces were etched.
A solution of 2ml HF, 6ml HNO3, and 92ml H2O was
used as the etchant (Kroll’s Reagent) to etch the speci-
mens for 140–150 seconds and were cleaned with acetone.
For Surface Crack density (SCD), the FESEM images were
analyzed with the help of PDF-XChange Viewer software.
SCD is defined as the ratio of total crack length and the
image area (Eq. (2)).[27] Three images of each specimen
were taken and the average SCD was calculated. It should
be noted that all the images should be taken at the same
magnification for SCD calculation as it is a relative mea-
surement. A demonstration of calculation of SCD is
shown in Fig. 1. Here, the total crack length sums to
3245.18 nm and the image area is (14655
9885.66)
nm2. The corresponding SCD obtained is 2.24
10−5 nm/
nm2 or 0.0224 µm/µm2 (Run no. 9 with DF = 0.892%,
GV = 30V, FR = 4 LPM). For the recast layer study, the
Figure 1. Demonstration for the calculation of SCD: a) original FESEM image and b) SCD calculated FESEM image.
MATERIALS AND MANUFACTURING PROCESSES 1093
transverse section of the specimen was diamond polished
so as to obtain a mirror finish. The image obtained was
viewed with Image-J software (Fig. 2) at three distinct
positions and the mean was calculated. Recast layer thick-
ness can be calculated by dividing the image area with the
image length (Eq. (3)).
Cutting Distance
Cutting Rate ðCRÞ ¼ (1)
Cutting Time
Total Crack Length
Surface Crack Density ðSCDÞ ¼ (2)
Image Area
Image Area
Recast layer thickness ðRLTÞ ¼ (3)
Image Length
Results and discussion
The data from the experiments are presented in Table 1
and the ANOVA tables of the output parameters are
shown in Table 2. All the analyses were performed on
Minitab 17 software. From the ANOVA table, it can be
stated that all of the selected control parameters are sig-
nificant as their p-values are below 0.05. The values of
R-sq, R-sq (adj), and R-sq (pred) were tending to 100%,
which is required for the fitness of the model. Higher p-
values of lack of fit verified that the regression models
generated were significant.
Response surface outcomes
To determine the cause and effect with respect to the input
variables and output responses, Response Surface
Methodology (RSM) is employed, which is a collection of
statistical and mathematical techniques. RSM with Box-
Behnken design was used for the design of experiments
which contained a total of 15 experiments out of which
eight were corner points, one central point, and six were
star points. Box-Behnken designs are based on three- level
incomplete factorials and are second order designs which
1094 B. K. ROY AND A. MANDAL

Figure 2. Demonstration of calculation of RLT: a) original FESEM image with Recast Layer, Heat Affected Zone, and Base alloy b) area of the recast layer and c) length
of the recast layer.

Table 1. Experimental data. are rotatable or nearly rotatable.[28] Final regression models
CR SCD obtained using RSM is presented in Eqs. (4)–(8).
Run DF GV FR (mm/ Rz (µm/ RLT
Order (%) (Volts) (LPM) min) (µm) Rt (µm) µm2) (µm)
CR ¼ 5:483 þ 20:06DF  0:02211GV þ 0:1603FR
1 0.701 50 4 2.354 9.458 12.3540 0.0134 9.102
2 0.892 50 6 2.454 10.384 13.1962 0.0205 11.762  12:49DF2  0:000018GV2  0:01119FR2
3 0.701 30 6 2.405 9.803 12.6360 0.0154 9.801
4 0.701 50 4 2.288 9.566 12.3510 0.0137 8.913 þ 0:02225DF
GV  0:0935DF
FR
5 0.575 70 4 1.478 8.295 11.5991 0.0116 8.623 þ 0:000244GV
FR (4)
6 0.701 30 2 2.395 9.794 12.4635 0.0146 9.381
7 0.701 70 6 2.157 9.337 12.2610 0.0128 8.872
8 0.892 50 2 2.424 10.126 12.9236 0.0179 10.673
9 0.892 30 4 2.557 9.859 13.3912 0.0224 12.306
10 0.892 70 4 2.416 10.006 12.8420 0.0169 10.364 Rz ¼ 5:01 þ 13:86DF  0:0417GV  0:362FR
11 0.575 50 2 1.584 8.813 11.6321 0.0115 8.304
12 0.575 50 6 1.749 8.882 11.7030 0.0116 8.366  9:72DF2  0:000275GV2 þ 0:0302FR2
13 0.575 30 4 1.911 9.122 11.8116 0.0121 8.432
14 0.701 50 4 2.312 9.565 12.3620 0.0136 8.978 þ 0:078DF
GV þ 0:162DF
FR
15 0.701 70 2 2.108 9.227 12.1540 0.0126 8.675 þ 0:000631GV
FR (5)
 MATERIALS AND MANUFACTURING PROCESSES 1095

Table 2. ANOVA table.

CR Rz Rt SCD RLT
Model: F 128.27 76.55 7581.22 350.76 257.51
Model: P 0.000 0.000 0.000 0.000 0.000
Linear: F 98.94 18.03 785.99 14.10 15.72
Linear: P 0.000 0.004 0.000 0.007 0.006
Square: F 79.82 16.62 332.71 29.56 31.32
Square: P 0.000 0.005 0.000 0.001 0.001
2-Way Interaction: F 5.87 14.19 216.28 55.97 50.87
2-Way Interaction: P 0.043 0.007 0.000 0.000 0.000
Lack of Fit: F 1.39 2.01 2.57 2.87 1.02
Lack of Fit: P 0.444 0.349 0.292 0.269 0.529
S= 0.0371456 0.0786437 0.0040320 0.0022258 0.0966462
R-sq = 99.57% 99.28% 99.99% 99.84% 99.78%
R-sq(adj) = 98.79% 97.98% 99.98% 99.56% 99.40%
R-sq(pred) = 95.05% 90.31% 99.90% 97.89% 97.72%

Rt ¼ 5:607 þ 14:985DF  0:00963GV þ 0:1097FR
 6:79DF2 þ 0:000115GV2  0:00580FR2
 0:01288DF
GV  0:0140DF
FR
 0:000409GV
FR
SCD ¼ 0:01537  0:02878DF þ 0:000151GV
 0:000971FR þ 0:04414DF2  0:000001GV2
 0:000011FR2  0:000397DF
GV
þ 0:002066DF
FR þ 0:000004GV
FR
RLT ¼ 11:15  14:86DF þ 0:608GV  0:449FR
þ 19:62DF2 þ 0:000424GV2 þ 0:0037FR2
 0:1657DF
GV þ 0:836DF
FR
 0:00139GV
FR
Monte – Carlo analysis
An advantage of the Box- Behnken designs is that it
requires a fewer number of experiment runs to be per-
formed. As a result, it is impossible to predict whether
the generated model will perform adequately when large
numbers of samples are to be considered as in the case of
the manufacturing sector. For this, it is important to use
a Monte- Carlo Simulation (MCS) which is based on ran-
dom data.
To analyze the behavior of the regression model generated,
MCS was performed. MCS involves the generation of a large
number of random data (X1, X2 … Xn) according to their
distribution and performing the experiments on the compu-
ter. The characteristics of the output model (Y = f(X)) are
analyzed and conclusions are made based on statistics. In this
study 100,000 random data of duty factor, gap voltage and
flow rate were generated according to a normal distribution.
These values were put into the regression equations and the
output values of cutting rate, Rz, Rt, SCD, and RLT were
generated. These generated output values were compared
with the experimental output values based on Anderson –
Darling normality tests. Anderson – Darling normality test
checks whether a sample of data comes from a population
with a specific distribution. If the p-value is less than 0.05 in
a normality test, it can be concluded with 95% confidence that
the data does not follow the normal distribution. Figure 3
(6) shows the comparison of normality tests done for experimen-
tal values and Monte – Carlo simulation of experimental
generated values.
It can be observed from Fig. 3 that the output of both
the experimental values and Monte – Carlo simulated (M.
C.S) values of any of the responses do not follow a normal
distribution. From Fig. 3a, it can be observed that the
(7)
maximum cutting rates obtained were 2.5570 and
2.7559 mm/min for experimental values and M.C.S respec-
tively. The mean and standard deviations were 2.1728 and
0.3380 for experimental values and 2.1589 and 0.4448
for M.C.S. The values of maximum cutting rate, mean,
and the standard deviations of the experimental data and
(8) the M.C.S data were close enough to claim that the regres-
sion models would predict precisely for any number of
samples. Similarly, the values of the experimental data and
the M.C.S data of other responses were also close enough to
conclude that the regression models would fit in case of
a large number of samples.
Effect of process parameters on cutting rate
3D plots of cutting rate vs. input parameters (Fig. 4) show that
with an increment in duty factor and a decrement in gap
voltage, the cutting rate increases. As the duty factor increases,
the energy of the spark per pulse increases and also, the
frequency of the pulse increases which, in turn, removes
more material from the sparking zone in a particular time
interval, resulting in an increment in the cutting rate.
Mathematically,
Ton Ton
Duty Factor ¼ ¼
Ton þ Toff Total Time of acycle
¼ Ton
f (9)
[Where, f = frequency = (Total time of a cycle)−1]
The cutting rate increases initially, reaches a maximum at
0.80% duty factor and then decreases with increasing duty
factor. Gap voltage can be defined as the voltage between the
1096 B. K. ROY AND A. MANDAL

Figure 3. Analysis of Experimental data and Monte – Carlo Simulated data for a) Cutting Rate; b) Rz; c) Rt; d) SCD; e) RLT.

work-piece and the wire electrode. When the gap voltage
increases, the voltage between the electrodes also increases,
and hence, the sparking starts from a higher stand-off dis-
tance, which reduces the spark intensity and results in lower
cutting rate. The cutting rate varies with the gap voltage in an
inversely-linear manner. The cutting rate improves marginally
as the flow rate increases, as an increment in flow rate leads to
rapid flushing of debris formed after the melting of the work-
piece and hence, the increment in cutting rate. By performing
single parameter optimization, the maximum cutting rate was
found to be 2.6177 mm/min at a duty factor of 0.815%, gap
voltage of 30 V and a flow rate of 4.101 LPM.
 MATERIALS AND MANUFACTURING PROCESSES 1097

Figure 4. Effect of process parameters on CR.

Effect of process parameters on surface roughness (Rz and affects the desired accuracy of the geometry. Hence, the
and Rt) flow rate should be kept at the optimal value. Using single
parameter optimization, it is found that the optimal condi-
In this study, Rz and Rt are preferred over Ra as Ra cannot
tions for Rz are DF = 0.575%, GV = 70 V, and FR = 3.6970
differentiate between peaks and valleys. Moreover, Rz and Rt
LPM and the optimal value was found to be 8.224 µm. Rt is
together can determine the quality of any surface. If the values
defined as the maximum peak to valley height and is very
of Rz and Rt are close to each other, then it can be concluded
sensitive to large irregularities from the reference line. The
that the surface is uniform. 3D plots of roughness Rz are
optimal conditions for Rt were DF = 0.575%, GV = 70 V, and
shown in Fig. 5a-b. Rz or average peak to valley height
FR = 2.0 LPM and the optimal value was 11.474 µm. The 3D
equalizes large irregularities that are not a part of the surface
plot of Rt is shown in Fig. 5c-d. From this analysis of different
finish. Roughness increases with an increment in duty factor
surface characteristics, it can be concluded that the flow rate
and flow rate, and a decrement in gap voltage. As the duty
plays an important role in determining the roughness of the
factor increases, the intensity of the spark increases which
surface as per the requirement (Rz or Rt).
leads to larger craters and deeper cracks resulting in higher
roughness. As the gap voltage increases, the stand-off distance
increases resulting in a reduction in spark intensity and hence
Effect of process parameters on SCD and RLT
improved surface finish. The flow rate plays a decisive role in
deducing the roughness of the surface. If the flow rate is too During the WEDM process, the temperatures generated are very
low, the dielectric fluid gets contaminated due to insufficient much higher than the melting point of the work-piece and is
flushing, leading to unfavorable spark conditions and result- followed by rapid quenching. As a result, large thermal stresses
ing in a rougher finish. At very high flow rates, the flushing are developed which exceed the fracture strength and thus,
conditions lead to large wire vibrations resulting in non- cracks are developed. Both the dimension and the severity
uniform sparking which in turn results in a rougher surface of the cracks are determined by the thermal properties of the
1098 B. K. ROY AND A. MANDAL
Figure 5. Effect of process parameters on (a, b) Rz and (c, d) Rt.
work-piece as well as the discharge energy input. 3D plots of
SCD are shown in Fig. 6a-b. The curve of DF vs. SCD shows an
increasing trend. From the fig., it can be observed that as DF
increases from 0.6 to 0.9%, SCD increases from 0.012 to
0.018 µm/µm2. This is due to the fact that an increment in DF
leads to an increment in discharge energy. This discharge energy
causes thermal residual stress in the work-piece which leads to
the formation of cracks. The graph of FR vs. SCD also shows an
increasing trend. As the FR increases from 2 to 6 LPM, the SCD
also increases from 0.015 to 0.021 µm/µm2. An increment in the
FR leads to faster quenching rates which tend to make the work-
piece brittle in nature. The graph of GV vs. SCD shows
a decreasing trend. The value of SCD decreases from 0.0145 to
0.0125 µm/µm2 when GV is increased from 30 to 75 V. An
increment in the GV increases the voltage between the electrodes
but the spark intensity is reduced due to increment in stand-off
distance. This leads to lower thermal residual stresses and hence
lower cracks on the machined surface. From the single para-
meter optimization, it is observed that the optimal value of SCD
is 0.0113 µm/µm2 at DF = 0.575%, GV = 60.303 V and FR = 6
LPM. 3D plots of RLT are shown in Fig. 6c-d. It can be observed
that the graphs of SCD and RLT almost follow a similar trend.
The graph of DF vs. RLT shows an increasing trend. As the value
of DF increases from 0.5 to 0.9%, the value of RLT increases
from 8.5 to 10 µm. An increment in DF leads to an increment in
energy per spark which leads to an increment in melting and
evaporation rates. During this, the FR is not sufficient to flush
away the debris from the machined zone. As a result, some of the
debris gets solidified in the machined zone itself due to quench-
ing, thereby leading to the formation of recast layer. The graph of
GV vs. RLT shows a decreasing trend. As the GV is increased
from 30 to 75 V, the RLT shows a reduction from 9.3 to 8.7 µm.
An increment in GV leads to a decrement in the spark intensity
which further leads to lower melting and evaporation rates at the
same FR and hence, the RLT decreases. Ideally, the graph of FR
vs. RLT should be showing a decreasing trend. However, data
from the experiment shows that the graph is of increasing
nature. This can be attributed to the fact that even at a FR of 6
LPM, the flushing is not sufficient to remove the debris from the
machined zone. However, due to faster quenching rates at higher
FR, the molten material gets solidified faster, thereby leading to
the formation of recast layer. The optimal value of RLT is found
to be 8.3337 µm at DF = 0.575%, GV = 48.585 V, and
FR = 4.868 LPM.
 MATERIALS AND MANUFACTURING PROCESSES 1099

Figure 6. Effect of process parameters on (a, b) SCD and (c, d) RLT.

Multi-objective optimization of process parameters

In single parameter optimization, only one parameter can be
optimized at a time. Hence, a multi-objective optimization is
done to optimize all the responses at the same time. This was
done by using desirability approach. In the desirability
approach, the value 0 is assigned to a completely undesirable
characteristic, and a value of 1 is assigned to a completely
desirable characteristic. The composite desirability is calcu-
lated by taking the geometric mean of all the individual
desirability values. In this study, the cutting rate was max-
imized and all the other responses were simultaneously
minimized. The optimal values of CR, Rz, Rt, SCD, and RLT
were found to be 1.7498 mm/min, 8.5799 µm, 11.7812 µm,
0.0118 µm/µm2, and 8.5493 µm respectively at DF = 0.6106%,
GV = 69.1919 V, and FR = 4.6667 LPM. Multi-objective
optimization is also performed by not considering the cutting
rate and minimizing the other responses to study the surface
characteristics. The optimal values of Rz, Rt, SCD, and RLT in
this case were 8.2938 µm, 11.5747 µm, 0.0115 µm/µm2, and
8.5178 µm respectively at DF = 0.575%, GV = 70 V, and
FR = 5.2323 LPM. The optimal values of the responses
along with the parametric settings are presented in Table 3.

Table 3. Optimization table.

Multi-Objective Optimization
Response Single Parameter Optimization With CR Without CR
CR (mm/min) 2.6177 1.7498 Optimal Settings: - Optimal
(DF = 0.815%, GV = 30V, FR = 4.101 LPM) (d = 0.999) DF = 0.6106%, Settings: DF = 0.575%,
Rz 8.224 8.5799 GV = 69.1919V, 8.2938 GV = 70.00V,
(µm) (DF = 0.575%, GV = 70V, FR = 3.697 LPM) (d = 0.957) FR = 4.6667 LPM, (d = 1.000) FR = 5.2323 LPM,
Rt 11.474 11.7812 D = 0.9636 11.5747 D = 0.9802
(µm) (DF = 0.575%, GV = 70V, FR = 2.0 LPM) (d = 0.949) (d = 0.976)
SCD (µm/µm2) 0.0113 0.0118 0.0115
(DF = 0.575%, GV = 60.303 V, FR = 6 LPM) (d = 0.974) (d = 0.999)
RLT 8.3337 8.5493 8.5178
(µm) (DF = 0.575%, GV = 48.585V, FR = 4.868 LPM) (d = 0.938) (d = 0.946)
1100 B. K. ROY AND A. MANDAL
Microstructure and metallurgical characteristics
A surface microstructure is studied with the help of FESEM
images taken at different magnifications. Figure 7a shows the
FESEM micrograph of the surface with the highest cutting
rate (DF = 0.81%, GV = 30 V, FR = 4.1 LPM) under 500X
magnification and Fig. 7b shows the optimal surface
(DF = 0.57%, GV = 70 V, FR = 5.2 LPM) at the same
magnification. It can be observed that a lot of white particles
of non-uniform size have been accumulated in the first case.
The accumulation of these particles in the machined zone
may be due to the material deposition from the wire and the
dielectric. The same surfaces with higher magnification
(20,000X) are shown in Fig. 7c-d. It can be observed from
Fig. 7c that the surface exhibits both severe cracks and
micro-cracks. Some of these cracks are penetrating in nature.
Penetrating cracks initiate from the recast layer and termi-
nate either in heat affected zone or base metal. These defects
arise due to the higher discharge energy and improper flush-
ing conditions which results in severe thermal stresses and
hence, the cracks are formed. Large voids are also observed
in this parameter setting. The temperature during the
WEDM process rise approximately up to 12,000 ᵒC and
a part of the molten material and the dielectric fluid gets
evaporated and gets trapped in the work-piece in the form of
Figure 7. FESEM micrographs of surfaces of a) Max CR Surface (500X) b) Optimal surface (500X) c) Max CR Surface (20,000X)) d) Optimal surface (20000X).
vapors. These vapors have a tendency to come out resulting
in the formation of voids. From Fig. 7d it can be observed
that at optimal conditions, severe cracks are eliminated
completely. Also, the sizes of the voids are reduced consid-
erably. The micro-cracks are observed only on the solidifica-
tion layer and hence the presence of penetrating cracks is
eliminated.
Conclusions
The machining of Nitinol-60 has been performed success-
fully by WEDM. Quantitative analyses of the surface char-
acteristics have been performed by considering three input
parameters viz. pulse-on-time, gap voltage and flow rate;
and five output parameters viz. cutting rate, maximum
peak to valley height (Rt), the average peak to valley
height (Rz), recast layer thickness (RLT), and surface
crack density (SCD). The relationship between the input
factors and the responses were developed using RSM.
Monte-Carlo simulation was performed to verify the effec-
tiveness of these models for a large number of runs.
Surface integrity of the machined surface has been studied
with the help of FESEM images. The following conclusions
have been made from the present investigation.

(1) All the process parameters viz. duty factor, gap voltage, and
flow rate were found to be significant for all the responses.
The cutting rate was found to increase with the duty factor
up to 0.8% and then decreased with the duty factor.
(2) Flow rate plays an important role in the type of sur-
face roughness values to be measured. The optimal
flow rate for Rz was found to be 3.697 LPM whereas
the optimal flow rate for Rt was found to be 2.0 LPM
at a duty factor of 0.575% and gap voltage of 70 V.
(3) Surface Crack Density was found to increase with an
increase in flow rate. An increment in the FR leads to
higher quenching rates which tend to make the work-
piece brittle in nature and the cracks form on the
surface due to thermal residual stresses.
(4) Recast Layer Thickness was also found to increase with the
flow rate which indicated that flushing was insufficient
even at a maximum flow rate of 6 LPM and the molten
material solidified time due to higher quenching rates.
(5) The models generated from the regression equations
were confirmed with Monte-Carlo analysis for 100,000
runs and it was observed that none of the responses
followed a normal distribution. However, the means
and standard deviations of Monte-Carlo simulated values
were close to the means and standard deviations of the
experimental values which indicated the model was accu-
rate and that the parametric settings may be used for mass
production.
(6) From the FESEM images, it was observed that at the
optimal settings, severe cracks and penetrating cracks
were eliminated significantly and the sizes of the
voids were also reduced.
Funding
This project was supported by the Science and Engineering Research
Board (SERB), Govt. of India [ECR/2017/000807];
References
[1] Buehler, W. J.; Wiley, R. C. Nickel - Base Alloys. U.S.
Patent3,174,851, March 23, 1965.
[2] Ren, X.; Otsuka, K. Origin of Rubber-Like Behaviour in Metal
Alloys. Nature. 1997, 389, 579–582. DOI: 10.1038/39277.
[3] Rasheed, M. S.; Abidi, M. H. Analysis of Influence of Micro-EDM
Parameters on MRR, TWR and Ra in Machining Ni-Ti Shape
Memory Alloy. Int. J. Recent Technol. Eng. 2012, 1, 32–37.
[4] Al-Ahmari, A. M. A.; Rasheed, M. S.; Mohammed, M. K.;
Saleh, T. A Hybrid Machining Process Combining Micro-EDM
and Laser Beam Machining of Nickel-Titanium-Based Shape
Memory Alloy. Mater. Manuf. Processes. 2016, 31, 447–455.
DOI: 10.1080/10426914.2015.1019102.
[5] Fu, C. H.; Liu, J. F.; Guo, Y. B.; Zhao, Q. Z. A Comparative
Study on White Layer Properties by Laser Cutting Vs.
Electrical Discharge Machining of Nitinol Shape Memory
Alloy. Procedia CIRP. 2016, 42, 246–251. DOI: 10.1016/j.
procir.2016.02.280.
[6] Abedi, E.; Daneshmand, S.; Neyestanak, A. A. L.;
Monfared, V. Analysis and Modeling of Electro Discharge
MATERIALS AND MANUFACTURING PROCESSES 1101
Machining Input Parameters of Nitinol Shape Memory Alloy
by De-Ionized Water and Copper Tools. Int. J. Electrochem.
Sci. 2014, 9, 2934–2943.
[7] Guo, Y.; Hou, P.; Shao, D.; Li, Z.; Wang, L.; Tang, L. High-
Speed Wire Electrical Discharge Machining of Insulating
Zirconia with a Novel Assisting Electrode. Mater. Manuf.
Processes. 2014, 29, 526–531. DOI: 10.1080/
10426914.2014.892983.
[8] Chaubey, S. K.; Jain, N. K. Investigations on Surface Quality
of WEDM- Manufactured Meso Bevel and Helical Gears.
Mater. Manuf. Process. 2018, 33, 1568–1577. DOI: 10.1080/
10426914.2017.1415440
[9] Dhobe, M. M.; Chopde, I. K.; Gogte, C. L. Optimization of
Wire Electro Discharge Machining Parameters for Improving
Surface Finish of Cryo-Treated Tool Steel Using DOE. Mater.
Manuf. Processes. 2014, 29, 1381–1386. DOI: 10.1080/
10426914.2014.930890.
[10] Mandal, A.; Dixit, A. R.; Das, A. K.; Mandal, N. Modeling
and Optimization of Machining Nimonic C-263 Superalloy
Using Multicut Strategy in WEDM. Mater. Manuf. Processes.
2016, 31, 860–868. DOI: 10.1080/10426914.2015.1048462.
[11] Nain, S. S.; Garg, D.; Kumar, S. Performance Evaluation of
the WEDM Process of Aeronautics Super Alloy. Mater.
Manuf. Process. 2018, 33, 1793–1808. DOI: 10.1080/
10426914.2018.1476761
[12] Thankachan, T.; Soorya Prakash, K.; Loganathan, M. WEDM
Process Parameter Optimization of FSPed Copper-BN
Composites. Mater. Manuf. Processes. 2018, 33, 350–358.
DOI: 10.1080/10426914.2017.1339311.
[13] Mussada, E. K.; Hua, C. C.; Rao, A. K. P. Surface
Hardenability Studies of the Die Steel Machined by WEDM.
Mater. Manuf. Process. 2018, 33, 1745–1750. DOI: 10.1080/
10426914.2018.1476695
[14] Bisaria, H.; Shandilya, P. Experimental Studies on Electrical
Discharge Wire Cutting of Ni-Rich Niti Shape Memory Alloy.
Mater. Manuf. Processes. 2018, 33(9), 977–985. DOI: 10.1080/
10426914.2017.1388518.
[15] Hsieh, S. F.; Chen, S. L.; Lin, H. C.; Lin, M. H.; Chiou, S. Y. The
Machining Characteristics and Shape Recovery Ability of Ti-Ni-X
(X=Zr, Cr) Ternary Shape Memory Alloys Using the Wire
Electro-Discharge Machining. Int. J. Mach. Tools Manuf. 2009,
49, 509–514. DOI: 10.1016/j.ijmachtools.2008.12.013.
[16] Liu, J. F.; Guo, Y. B.; Butler, T. M.; Weaver, M. L.
Crystallography, Compositions, and Properties of White
Layer by Wire Electrical Discharge Machining of Nitinol
Shape Memory Alloy. Mater. Des. 2016, 109, 1–9. DOI:
10.1016/j.matdes.2016.07.063.
[17] Liu, J. F.; Li, C.; Fang, X. Y.; Jordon, J. B.; Guo, Y. B. Effect
of Wire-EDM on Fatigue of Nitinol Shape Memory Alloy.
Mater. Manuf. Processes. 2018, 33, 1809–1814. DOI: 10.1080/
10426914.2018.1512125.
[18] Sharma, N.; Raj, T.; Jangra, K. K. Parameter Optimization and
Experimental Study on Wire Electrical Discharge Machining of
Porous Ni40Ti60 Alloy. Proc. Inst. Mech. Eng. B J. Eng. Manuf. 2017,
231, 956–970. DOI: 10.1177/0954405415577710.
[19] Lotfineyestanak, A.A.; Daneshmand, S. The Effect of
Operational Cutting Parameters on Nitinol-60 in Wire
Electrodischarge Machining. Adv. Mater. Sci. Eng.2013,
2013, Article ID 457186, 6 pages. DOI: 10.1155/2013/457186.
[20] Mwangi, J. W.; Zeidler, H.; Kühn, R.; Schubert, A. Suitability
Assessment of Micro-EDM in Machining Nitinol for Medical
Applications. Presented at theEuspen’s 16th International
Conference Exhibition, Nottingham, U.K, 2016.
[21] Soni, H.; Narendranath, S.; Ramesh, M. R. Experimental
Investigation on Effects of Wire Electro Discharge
Machining of Ti50 Ni45 Co5 Shape Memory Alloys. Silicon.
2018, 10, 2483–2490. DOI: 10.1007/s12633-018-9780-9.
1102 B. K. ROY AND A. MANDAL
[22] Laves, F.; Wallbaum, H. J. The Crystal Chemistry of Titanium
Alloys. Naturwissenschaften. 1939, 27, 674–675. DOI: 10.1007/
BF01494992.
[23] Sun, L.; Huang, W. M. Nature of the Multistage Transformation
in Shape Memory Alloys upon Heating. Met. Sci. Heat Treat.
2009, 51, 573–578. DOI: 10.1007/s11041-010-9213-x.
[24] Duerig, T.W.; Pelton, A.R. Ti-Ni Shape Memory Alloys. In: Materials
Properties Handbook: Titanium Alloys; 1994; pp. 1035–1048.
[25] Buehler, W. J.; Cross, W. B. Nitinol–Unique Wire Alloy with
a Memory. Wire J. 1969, 2, 55.
[26] Daneshmand, S.; Kahrizi, E. F.; Akbar, A.; Neyestanak, L.;
Mortazavi, M. Experimental Investigations into Electro Discharge
Machining of NiTi Shape Memory Alloys Using Rotational Tool. Int.
J. Electrochem. Sci. 2013, 8, 7484–7497.
[27] Rahul,; Datta, S.; Masanta, M. Surface Integrity and Metallurgical
Characteristics of the EDMed Work Surfaces of A2 Tool Steel (SAE
304SS), Inconel 601 and Ti-6Al-4V: A Comparative Analysis. Silicon.
2018, 10, 1557–1572. DOI: 10.1007/s12633-017-9640-z.
[28] Ferreira, S. L. C.; Bruns, R. E.; Ferreira, H. S.; Matos, G. D.;
David, J. M.; Brandão, G. C.; Da Silva, E. G. P.;
Portugal, L. A.; Dos Reis, P. S.; Souza, A. S.; et al. Box-
Behnken Design: An Alternative for the Optimization of
Analytical Methods. Anal. Chim. Acta. 2007, 597, 179–186.
DOI: 10.1016/j.aca.2007.07.011