Materials and Manufacturing Processes

ISSN: 1042-6914 (Print) 1532-2475 (Online) Journal homepage: http://www.tandfonline.com/loi/lmmp20

Electrical Discharge Machining of Ti6Al4V in

Hydroxyapatite Powder Mixed Dielectric Liquid

Nihal Ekmekci & Blent Ekmekci

To cite this article: Nihal Ekmekci & Blent Ekmekci (2015): Electrical Discharge Machining
of Ti6Al4V in Hydroxyapatite Powder Mixed Dielectric Liquid, Materials and Manufacturing
Processes, DOI: 10.1080/10426914.2015.1090591

To link to this article: http://dx.doi.org/10.1080/10426914.2015.1090591

Accepted author version posted online: 23

Sep 2015.

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 Electrical Discharge Machining of Ti6Al4V in Hydroxyapatite Powder Mixed
Dielectric Liquid

Nihal Ekmekci1, Blent Ekmekci1

1
Blent Ecevit University, Department of Mechanical Engineering, Zonguldak, Turkey

Address Correpondence to Blent Ekmekci, E-mail: bekmekci@hotmail.com,

bekmekci@beun.edu.tr

Abstract
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Hydroxyapatite (HA) powder suspension in deionized water was used as a dielectric

liquid during Electrical Discharge Machining of Ti6Al4V work material. The machined

surfaces were evaluated by scanning electron microscopy, energy dispersive

spectroscopy, and optical microscopy. The powder particles in the dielectric liquid

extensively migrated and formed an HA rich layer on the work material surface under

specific machining conditions. The result was attributed to the generation of secondary

discharges due to altered discharge conditions. The particles divided the primary

discharge channel into many secondary ones. When the main discharge channel

subdivided into several sub-discharges with comparable energy densities, the particles in

the discharge region got stuck among them. Then, moved toward the melted cavities and

penetrated to the surface at the end of the discharge duration. The results suggest the

process as a practical alternative for producing biocompatible interfaces or coatings for

medical applications.

KEYWORDS: Electrical discharge machining; Material migration; Hydroxyapatite

Deposition; Surface topography.

1
 INTRODUCTION

A small dielectric liquid gap separates both of the electrodes designated as work material

and tool electrode. Application of successive sparks among the electrodes result in high

local temperature increase and subsequent removal of material in Electrical Discharge

Machining (EDM) process. The temperature increase in spark incident regions is much

more than the melting and boiling points of the electrode materials. Therefore, when a

spark ceases, the melted cavities blowup aggressively into the dielectric liquid, generate a
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cavity in about semi-spherical shapes and solidify rapidly on both of the electrode

surfaces. The blowed out material also quickly solidifies in the form of small droplets and

alters the discharge conditions for the next cycle. Therefore, the dielectric circulation

takes away the products from the discharge region. The net result is the removal of a

small portion of material due to the application of electrical discharge. Use of many

sparks in high frequencies under proper dielectric circulation conditions and appropriate

movements of the tool electrode lead the matching geometry in the work material. The

tool electrode can be rotated and moved on three fundamental axes which further

improves the ability of sophisticated shape generation and dimensional accuracy on the

machined parts. The thermal characteristic of the removal mechanism makes possible to

machine hard materials. The mechanical properties of the work material such as hardness

is not a concern for machinability and machining forces are minuscule.

Different physical properties of the materials during machining result in their various

influences and cause differences in material removal rates [1]. Fine powder addition into

the dielectric liquid usually results in increased machining performance [2] and assures

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 higher precision and surface quality [3]. For example, addition of Wolfram (W) powder

lead approximately 50% increase in material removal rate during machining of SiC

composite [4]. Electrode polarity is also active in modifications of the surfaces as well as

the pulse time and pulse current [5]. Microhardness of re-solidified layer increases with

the use of Si, W, graphite [6] and TaC [7] powders. The conductive powder is usually

more useful in microhardness increase [8]. However, graphite powder is more suitable for

improving the microhardness when compared to Al [9]. Increasing Ti powder

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concentration results in a crack-free surface [10]. Nevertheless, the addition of fine

graphite particles leads to accumulation in the dielectric and cause unstable machining

conditions [11]. Moreover, Cu powder migrates easier than the graphite to the surface

when machining metal matrix composites [12]. SiC particles penetrate on interstitial free

steel surfaces [13] where the migration temperatures rely on the applied pulse energy

[14]. A Ti-rich layer forms over the surface of WC by the use of Ti powder in the

kerosene dielectric [15]. Similarly, W powder addition substantially increases the content

of W in the re-solidified layer [16]. The results indicate the potential for surface alloying

and functional surface generation by the process. The discharge transitivity in the inter-

electrode gap is altered due to the suspended powders in the dielectric liquid. The

probability of main discharge channel separation and the number of breakdown regions

are increased due to the discontinuities created in the gap. In some instances, suspended

powders in dielectric liquid migrate to the work material surface during machining.

Ti and itshos alloys are used in various medical applications like implant materials for

failed hard tissues and dental applications for about 40 years. However, released ions

3
 from metallic implants to the body cause adverse effects on organs, allergy, and

carcinoma [17]. Thus, implants have been coated to offer faster bone adaptation and

improve implant integration, according to essential characteristics such as desired phase

and crystalline, good coating integrity and suitable porosity [18]. Calcium phosphate-

based ceramic materials, such as hydroxyapatite, tricalcium phosphate are the preferred

coating materials due to the bio-activity characteristics. So, coating techniques and the

possible influences on the content become a significant concern for the researchers. There
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are some coating techniques for calcium phosphate deposition on titanium substrates.

Plasma spray method [19] is the most extensively used one. Shot peening, abrasive

blasting [20], aqueous spray method [21], electrochemical coating [22], pulsed laser

deposition [23], biomimetic apatite coatings [24] are the possible alternatives.

Previous studies suggested the possibility of suspended particle migration on to the work

material surface during Powder Mixed Electrical Discharge Machining (PMEDM).

Therefore, we examined the process feasibility as an alternative HA deposition technique

for producing biocompatible interfaces. Ti6Al4V samples are machined using different

pulse currents, pulse time and polarity in HA powder mixed water dielectric liquid. Then,

the resultant surface modifications are studied by using Scanning Electron Microscopy

(SEM), Energy Dispersive Spectrometry (EDS), and optical microscopy.

MATERIALS AND METHODS

A 3 l plastic liquid container was mounted on the machining table of AJANEDM

CNC983 brand die sinking type EDM via a specially designed stainless steel sample

4
 holder. The dielectric liquid was continuously mixed to avoid powder settlement and

accumulation (Figure 1). A Ti6Al4V rod of 10 mm diameter was cut at 8 mm intervals

and the sample surfaces were polished. Pure titanium was used as tool electrode during

EDM. Three different experimental group were tested to characterize the influence of

electrical parameters. The first group included six different pulse time setting with five

different current level using the positive tool electrode polarity (Table 1). The second

group of experiments includes the cases of using negative tool electrode polarity (Table
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2). The HA concentration in deionized water was 15 g/l for the both cases. Finally, the

last group was the analysis of samples machined by different concentrations (5, 10, 20

g/l) of HA powder in deionized water. The machining condition was selected from the

previous experimentations as 12 s pulse on duration and 22 A pulse current that reveal

the most plausible choice for the HA deposition. The SEM analysis of HA powder prior

to mixing shown a structure of interconnected globular forms (Figure 2a) with

characteristic Ca and P peaks using EDS analysis (Figure 2b). The particle size

distribution of the powder varied between 10 to 40 m (Figure 2c) which was analyzed

by using Malvern brand laser diffraction particle size analyzer in the wet dispersion. FEI

Quanta 450 brand and Jeol JSM 6060 brand SEM, which are both furnished with EDS

attachments, were used for topographical and compositional examinations. The spectrum

area was the all SEM picture area given on the left side of the EDS plots. Cross sections

of the samples were analyzed after application of conventional metallographic sample

preparation techniques (cutting, sanding and polishing). Sections were etched by Krolls

Solution (2 ml Hydrofluoric acid + 6 ml Nitric acid + 98 ml water) to show the features

of the microstructure.

5
 RESULTS AND DISCUSSION

The surface was found to be conveying its usual topographical structure when the pulse

time was 100 s, and the pulse current was 12A. The surface was covered with craters

due to the primary sparks during machining. There were only random occasions of

migrated particles and a dense microcrack formation. Decreasing the pulse time to 50 s

increased the rate of HA particle migration usually around the crater rims (Figure 3a).
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Migrated particles could be distinguished more easily with its darker appearance on the

backscattered image (Figure 3b). Therefore, reflecting a non-uniform region on its cross-

section (Figure 3c) and indicating the development of an additional layer over the

surface. The re-solidified and overlapped structure was beneath the layer and indicated

several occasion of micro cracks in the structure. The cracks perpendicularly penetrated

from the surface and usually terminated at the interface that is separating the recast

structure and the heat affected zone in the solid state. When and electrical discharge

ceases, the volume occupied by the discharge channel filled rapidly with the flow back

the dielectric liquid. The surface of the melted cavity cools quickly and, therefore, shrink

faster than the parent material. Moreover, high transformational stresses were developed

during the solidification process. Thus, if stresses exceed the materials ultimate strength,

cracks initiated on the surface and penetrated into the re-solidified layer.

Further, decreasing the pulse time to 12 s resulted in a denser and more homogenously

distributed HA layer over the surface. Only small portions of the work material could be

observed on the surface using SEM (Figure 3d,e). The covering and re-solidified layer

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 thicknesses, as well as the number of occasions of microcracks, decreased considerably

(Figure 3f). The discharge channel is not cylindrical when powder additives are used in

dielectric liquid [25]. The suspended particles alter the dielectric strength of the liquid by

increasing the number of equal breakdown regions. Moreover, HA particles around the

discharge channel are also affected by the electrostatic forces. According to Kunieda and

Yanatori, [26] many chains of particles lineup and link the gap in a very short period.

The primary discharge channel is interrupted and the chains are ruined due to the
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expansion of the discharge channel. The main discharge channel subdivided into several

secondary discharges and suspended particles stack among them. Additionally, the

particles are under the thermal effects of the discharge boundaries. At the end of the pulse

current, all the subdivided discharge channel boundaries suddenly collapse and produce a

negative pressure within the gap. Then, the stacked particles and surrounded dielectric

liquid flash suddenly to the melted cavities. The process is very fast and allows the

particles to penetrate into the cavities even in a molten state and builds-up a particle rich

layer over the surface due to the sequential collisions at high temperatures.

The formation of a crack network on the surface is usual during machining of Ti and its

alloys due to its low thermal conductivity. However, the number of cracks in the recast

layer considerably decrease when HA powders deposited on the surface. This result also

supports the conclusion of primary discharge channel subdivision. The decreased energy

in secondary discharges results in reduced thermal stress during solidification.

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 Increasing pulse current to 22A revealed similar trends of particle migration phenomena

with respect to pulse time. The regular features of non-additive electric discharge

machining were apparent when using 100 s pulse time. Decreased pulse-on duration to

50 s resulted in similar surface features with the previous case. The difference was the

decrease in crater sizes due to the reduced time for the discharge channel to expand. A

few number of HA particles were randomly distributed over the surfaces which could be

attributed to the stochastic nature of the process. Therefore, it is concluded that the
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particle migration phenomena was not initiated for the cases. Reducing the pulse time to

12 s resulted in a drastically altered surface texture (Figure 4a, b). It was impossible to

see the classical features of non-additive EDMed surfaces. Migrated particles fused and

formed a covering layer over the surface due to the sequential collisions of HA particles

at high temperatures at the end of each electrical pulse. The result is the characteristic Ca

and P peaks (Figure 4c) obtained from the EDS analysis. The sample cross-section was

gold-plated due to improper electrical connectivity in the HA layer for further SEM

analysis. The thickness of the layer was varying between 20 and 50 m, and features of

EDMed surfaces lay beneath the covering layer (Figure 5a). Enlarged SEM section

views (Figure 5b) and corresponding EDS peaks (Figure 5c) demonstrated the

agglomerated structure of the layer and its composition. The results pointed out the most

plausible choice for HA deposition among the analyzed samples. The results indicate that

the extent of differences is highly sensitive to the selected electrical parameters during

EDM. The discharge conditions drastically alter and particle migration commence under

specific machining conditions. The surface textures illustrate the controlled nature of the

process by adjusting the pulse time and current. The particle migration phenomenon

8
 initiates when using low pulse time settings and slightly increases while reducing the

pulse current. The results are also in accordance with the previous study [14].

When using a relatively high pulse time (25 s) and reduced pulse current (7A) during

machining, the layer also formed over the surface (Figure 6a). The size of the grains was

comparable to the previous case (Figure 6b) with characteristic EDS peaks (Figure 6c).

However, keeping the pulse time at 12 s but increasing pulse currents to 72A resulted in
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an evenly distributed HA layer over the surface. The base metal noticeable from the

deposited layer at some sections (Figure 6d). The enlarged SEM view indicated a slight

decrease in grain size (Figure 6e), and a considerable decrease in P peak intensity (Figure

6f). HA particles decompose over 1000 C and, therefore, the built-up temperature

become an important aspect. Using higher pulse currents also increases the energy level

of the subdivided discharge channels. Although the HA particles migrate to the surface

during machining, its composition alters due to the high build-up temperatures. The

stacked particles between relatively high energy discharges are heated above the

decomposition temperature just before pulse cessation. This conclusion also implies an

important aspect of process control by adjusting the machining parameters in a simple

way for different types of additives. Moreover, the switch from the deposition and

removal process is also possible by changing the electrical parameters. So, HA layer

thickness and the shape of the substrate could be structured during the process.

All the results presented up to this point belong to the machining case using 15 g/l HA

suspended powder in water dielectric liquid. EDM of samples using 12 s pulse time and

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 22A pulse current in water dielectric liquid with 5 and 10 g/l HA suspended powder

respectively indicated a gradual rise in the number of secondary discharges. The result of

secondary discharges on the surface could be visualized as smaller cavities around the

central crater rims. During the pulse on period, the discharge channel expands and

confronts with the suspended particles in the dielectric liquid. Therefore, the primary

discharge channel branched in a few number of secondary discharges from its outer

boundaries when using a low concentration of HA powder in dielectric liquid (Figure 7).
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Increasing the HA powder concentration to15 g/l revealed the HA layered structure as

given previously. Further increase in HA powder concentration to 20 g/l also showed

such a layer without noticeable differences. Increasing the particle concentration in the

dielectric liquid increases the number of discontinuities in the gap and lead a complete

division of the primary discharge channel into many secondary ones. Therefore, the

deposition mechanism activates at the particular concentration that is between 10 to 15

g/l for the case.

Negative tool electrode polarity using 100 s pulse on time in 15 g/l HA suspended

powder in water dielectric liquid revealed the usual crater like topography (Figure 8a).

Reducing the pulse time to 50 s altered the topography with partly cracked structures in

some regions (Figure 8b). Further decrease in pulse time to 12 s resulted in a surface

completely covered with such structures (Figure 8c). The corresponding EDS analysis

results were impressive since P peak intensity was very high when compared to the Ca

peaks (Figure 8d). Further EDS analysis of surfaces EDMed using negative tool

electrode polarity also designated higher P peak intensities than Ca. A fraction of added

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 HA particles confronted with a discharge channel and completely decomposed into its

ions in the plasma channel. Then, P and Ca ions move to the negative pole for reduction

and positive pole for oxidation respectively.

CONCLUSIONS

Generation of several secondary discharges is the critical factor to initiate the migration

mechanism in HA powder mixed EDM. The suspended particles in the vicinity of

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discharging region interface with the main discharge channel and divide it into several

secondary ones. The stacked suspended particles among the secondary discharges are

heated and flushed back to the cavities produced at the end of a pulse time. The result is a

build-up process of a suspended particle rich layer, and it is in contrast to the material

removal mechanism caused by the primary sparks. Moreover, particle migration

mechanism could be activated for each pulse current level by adjusting the pulse time.

Using high pulse current over distinct levels and reduced pulse time result in a build-up

of a decomposed layer due to high temperatures attained during the process.

Using 22 A pulse current and 12 s pulse time led the most plausible choice for HA

deposition on the Ti6Al4V substrate. Besides, the tool electrode polarity is positive, and

HA suspended particle concentration in water dielectric liquid is 15 g/l or higher. The

results indicate the possibility of HA deposition on titanium alloy surfaces by the use of

the process. It is possible to switch between the deposition and removal process during

the machining and suggest an attractive method for arrangement the shape of the

substrate and the thickness of the covering HA layer for future applications.

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 ACKNOWLEDGEMENT

The authors acknowledge the sincere thanks to The Blent Ecevit University Research

Program for the grants given on the subject, which otherwise the work would not be

initiated.

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 Table 1. EDM process parameters using positive polarity

Pulse time (s)

3 6 12 25 50 100

Pulse current (A) Specimen number

7 1 () 2 3 () ()

12 4 5 6 7 8 9

22 10 () 11 () 12 13
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42 14 15 16 () 17 ()

72 18 () 19 () 20 ()

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 Table 2. EDM process parameters using negative polarity

Pulse time (s)

3 12 50 100

Pulse current (A) Specimen number

12 21 22 23 ()

22 24 25 26 27

42 28 29 30 ()
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 Figure 1. Experimental setup a) General appearance b) Schematic view c) A view during

machining
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 Figure 2. HA powder properties a) SEM micrograph b) EDS analysis c) Particle size

distribution
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 Figure 3. Ti6Al4V surface machined using positive electrode polarity tp=50 s I=12 A;

a) SEM secondary image b) SEM back scattered image c) Optical section view tp=50 s

I=12 A; d) SEM secondary image e) SEM back scattered image f) Optical section view

tp=12 s I=12 A
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 Figure 4. Ti6Al4V surface machined using positive polarity tp=12 s I=22 A; a) SEM

secondary image b) SEM back scattered image c) EDS peaks

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 Figure 5. Section SEM images of Ti6Al4V surface machined using positive polarity

tp=12 s I=22 A a) General appearance b) Grain structure c) EDS peaks

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 Figure 6. Ti6Al4V surfaces machined using positive polarity; a) Back scattered SEM

image b) HA grains; c) EDS peaks tp=25 s I=7 A; d) Back scattered SEM image e) HA

grains; f ) EDS peaks tp=12 s I=72 A

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 Figure 7. Ti6Al4V surfaces machined using positive polarity tp=12 s I=22 A; a) 5g/l b)

10g/l HA powder additive in water dielectric liquid

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 Figure 8. Ti6Al4V surfaces machined using negative tool electrode polarity I=22 A; a)

tp=100 s b) tp=50 s c) tp=12 d) Corresponding EDS peaks of tp=12

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