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DEVELOPMEMT OF METAL MEMBRANE USING

ELECTRIC DISCHARGE MACHINING AND ITS


ANALYSIS

Dissertation submitted to
Visvesvaraya National Institute of Technology
in partial fulfillment of the requirements for the award of the degree of

MASTER OF TECHNOLOGY
IN
INDUSTRIAL ENGINEERING

Submitted by
VIVEK R. SHARMA
13MT07IND012

Under the guidance of


Dr. Y. M. PURI
Associate Professor

Department of Mechanical Engineering


Visvesvaraya National Institute of Technology, Nagpur-440010
2013-2015
© Visvesvaraya National Institute of Technology (VNIT) 2015
DECLARATION

I, Vivek R. Sharma, hereby declare that the dissertation entitled


"Development of Metal Membrane Using Electric Discharge
Machining and Its Analysis" submitted therein has been carried out
by me in the Department of Mechanical Engineering of Visvesvaraya
National Institute of Technology. This work is original and has not
been submitted earlier either as a whole or in part for the award of any
degree/certificate at this or any other Institution/University.

Date: Vivek R. Sharma


Place: Nagpur (13MT07IND012)
Department of Mechanical Engineering
Visvesvaraya National Institute of Technology, Nagpur-440010

CERTIFICATE

This is to certify that the dissertation entitled "Development Of


Metal Membrane Using Electric Discharge Machining And Its
Analysis" is a bona fide work carried out by Vivek R. Sharma in the
Department of Mechanical Engineering of Visvesvaraya National
Institute of Technology, Nagpur and is submitted in partial fulfillment
of the requirements for the award of the degree of Master of
Technology in Industrial Engineering.

Project Guide Dr. S. B. Thombre


Dr. Y. M. Puri Head of Department
Associate Professor
CONTENTS

ACKNOWLEDGEMENTS ............................................................................................ i

ABSTRACT ...................................................................................................................ii

LIST OF FIGURES ..................................................................................................... iii

LIST OF TABLES ......................................................................................................... v

NOMENCLATURE ..................................................................................................... vi

1. INTRODUCTION ................................................................................................. 1

1.1. OVERVIEW OF MEMBRANE TECHNOLOGY ......................................... 1

1.2. TYPES OF MEMBRANE .............................................................................. 3

1.3. MEMBRANE STRUCTURE AND MATERIAL .......................................... 5

1.4. ADVANTAGES AND DISADVANTAGES OF MEMBRANE


TECHNOLOGY ........................................................................................................ 6

2. LITERATURE REVIEW ...................................................................................... 8

2.1. REVIEW OF LITERATURE.......................................................................... 8

2.2. PROBLEM IDENTIFICAION ..................................................................... 12

2.3. OBJECTIVE OF PROJECT ......................................................................... 13

2.4. METHEDOLOGY OF PROJECT ................................................................ 13

3. WIRE-CUT EDM ................................................................................................ 15

3.1. INTRODUCTION ......................................................................................... 15

3.2. PRINCIPLE OF OPERATION OF WIRE-CUT EDM ................................ 16

3.3. MECHANISM OF MATERIAL REMOVAL IN WEDM PROCESS......... 18

3.4. VARIOUS INPUT PARAMETERS OF WEDM ......................................... 19

3.5. VARIOUS OUTPUT PARAMETERS OF WEDM ..................................... 20

3.6. PROCESS PARAMETERS OF WEDM AND ITS INFLUENCE ON


WEDM ..................................................................................................................... 20

3.7. ADVANTAGES OF WEDM PROCESS ..................................................... 24


3.8. DISADVANTAGES OF WEDM PROCESS ............................................... 24

3.9. APPLICATIONS OF WEDM PROCESS .................................................... 24

4. MACHINING OF MEMBRANE ON WEDM.................................................... 25

4.1. WIRE-CUT EDM ......................................................................................... 25

4.2. INPUT PARAMETER .................................................................................. 29

4.3. MACHINING TECHNIQUE FOR DEVELOPMENT OF MEMBRANE .. 29

5. MEMBRANE CHARACTERISATION ............................................................. 34

5.1. CONTACT ANGLE MEASUREMENTS .................................................... 34

5.2. SURFACE MORPHOLOGY ........................................................................ 38

5.3. POROSITY OF MEMBRANE ..................................................................... 42

5.4. PORE SIZE AND PORE SIZE DISTRIBUTION ........................................ 45

5.5. PERMEABILITY OF MEMBRANE ........................................................... 52

6. RESULT AND DISCUSSION ............................................................................ 56

6.1. CONTACT ANGLE ..................................................................................... 56

6.2. SURFACE MORPHOLOGY ........................................................................ 56

6.3. POROSITY OF MEMBRANE ..................................................................... 57

6.4. PORE SIZE AND PORE SIZE DISTRIBUTION ........................................ 57

6.5. PERMEABILITY AND FLUX .................................................................... 58

6.6. APPLICATION OF MEMBRANE .............................................................. 60

7. CONCLUSIONS.................................................................................................. 63

7.1. CONCLUSIONS ........................................................................................... 63

7.2. FUTURE SCOPE .......................................................................................... 64

REFERENCES ............................................................................................................ 65

APPENDIX A
APPENDIX B
i

ACKNOWLEDGEMENTS
I would like to express my deep sense of respect and heartfelt gratitude to my guide
Dr. Y. M. Puri, who not only guided my project work, but also stood as a mentor in realizing
my potential. I thank him for introducing me to the field of electric discharge machining and
for providing the facilities in his laboratory for carrying out experimental analysis on wire
EDM. His invaluable advice, unwavering trust and unconditional support helped immensely
in timely and successful completion of the project.

I thank Dr. S. B. Thombre, Professor and Head, Department of Mechanical


Engineering, for extending the departmental facilities for my research work.

I am thankful to Prof. A. J. Rathod, Assistant Professor, Department of Chemical


Engineering, for providing valuable feedback and suggestions at various stages of the project.
I like to express my deepest gratitude to Gangadhar Navnage, Technician in Mechanical
Engineering Department, Vikas Gohil (Ph.D. research scholar) and Mohsin Dalvi (M.tech
student) for their valuable suggestions and help in carrying out project work. I am extremely
thankful to all the faculty members and staff of the department of Mechanical Engineering for
providing me unwavering guidance and support for the entire two years of my master’s
degree course.

Lastly, I owe a special debt and gratitude to my parents for supporting me in my


endeavours.

Vivek R. Sharma
(13MT07IND012)
ii

ABSTRACT

The separation, concentration, and purification of molecular mixtures are the


major problems in the chemical industries. Efficient separation processes are also
needed to obtain high-grade products in the food and pharmaceutical industries to
supply communities and industry with high-quality water, and to remove or recover
toxic or valuable components from industrial effluents. The membrane technology is
recently used for the filtration of such toxic or recovering of valuable components in
chemical industries. The membranes available for the filtration are made up of
polymers or ceramics having their own disadvantages like higher fouling rate, sealing
problem, heavier and bulky in nature and lower flux. So there is needed to develop
newer type of membrane especially membrane made up of metal.

In this work a novel method for the development of metal membrane is


discussed. The metal membrane is developed through machining of aluminium metal
on WEDM. The aluminium metal is sliced in cross sectional direction to develop an
aluminium wafers of thickness about 100-180 µm. These wafers are porous in nature
due to the formation of minor craters and cracks on the wafers during machining and
these wafers can act as a membrane. The various membrane characteristics like
porosity, permeability, surface morphology, pore size, etc. is discussed in this work.
Some applications of metal membrane developed through this process are also
discussed in this work.
iii

LIST OF FIGURES

Figure 1.1 Schematic diagrams of isotropic membranes ............................................... 4

Figure 1.2 Schematic diagrams of anisotropic membranes ........................................... 5

Figure 2.1 Flow Chart of Methodology ....................................................................... 14

Figure 3.1 Schematic diagram of the basic principle of WEDM process .................... 17

Figure 3.2 Block diagram of WEDM .......................................................................... 17

Figure 3.3 Detail of WEDM cutting gap ..................................................................... 19

Figure 3.4 Series of electrical pulses at the inter electrode gap ................................... 21

Figure 4.1 Ezee Cut Plus Wire EDM ........................................................................... 26

Figure 4.2 Control Panel of WDEM ............................................................................ 28

Figure 4.3 Reference machining of workpiece ............................................................ 29

Figure 4.4 Schematic diagram of three kinds of layers on an WEDM machined


surface .......................................................................................................................... 30

Figure 4.5 Schematic representation of the slicing of workpiece ................................ 31

Figure 4.6 Schematic diagram of cross section of machined membrane ..................... 31

Figure 4.7 Slicing of the aluminium work piece on WEDM ....................................... 32

Figure 4.8 Control panel window ................................................................................ 33

Figure 4.9 Membrane samples ..................................................................................... 33

Figure 5.1 Digital image of a liquid droplet on a dry surface in which the contact
angle (θ) is measured according to the sessile drop method. ....................................... 35

Figure 5.2 Water droplet on membrane surface........................................................... 36

Figure 5.3 MATLAB program window ....................................................................... 37

Figure 5.4 Surface Roughness Measurement Surftest SV - 3000 ................................ 39

Figure 5.5 Membrane tested for surface roughness ..................................................... 40

Figure 5.6 Graph of surface roughness of sample 1 .................................................... 40


iv

Figure 5.7 Graph of surface roughness of Sample 2 .................................................... 41

Figure 5.8 Fluid re-saturation method ......................................................................... 43

Figure 5.9 Membrane samples immersed in turpentine solution ................................. 44

Figure 5.10 Scanning Electron Microscope (SEM) ..................................................... 45

Figure 5.11 SEM image of membrane surface ............................................................ 46

Figure 5.12 Program window of MATLAB ................................................................ 47

Figure 5.13 Pore diameters of sample 1 (Side 1) ......................................................... 47

Figure 5.14 Pore diameters of sample 1 (Side 2) ......................................................... 48

Figure 5.15 Pore diameters of sample 2 (Side 1) ......................................................... 48

Figure 5.16 Pore diameters of sample 2 (Side 2) ......................................................... 49

Figure 5.17 Pore size distribution chart (Sample 1) .................................................... 50

Figure 5.18 Pore size distribution chart (Sample 2) .................................................... 51

Figure 5.19 Dead end filtration apparatus.................................................................... 52

Figure 5.20 Metallic membrane pasted on aluminium sheet ....................................... 53

Figure 5.21 Metallic membrane placed on apparatus .................................................. 53

Figure 5.22 Membrane samples tested for water flux.................................................. 55

Figure 6.1 Comparison of water flux ........................................................................... 59

Figure 6.2 Micro-filtration function ............................................................................. 60

Figure 6.3 Micro-filtration spectrum for water ............................................................ 61

Figure 6.4 Refractometer ............................................................................................. 61

Figure 6.5 Decolourization of contaminated water...................................................... 62


v

LIST OF TABLES

Table 4.1 Technical specification of WDEM .............................................................. 27

Table 4.2 Input parameters .......................................................................................... 33

Table 5.1 Pore volume and porosity ............................................................................ 44

Table 5.2 Pore size distribution (Sample 1) ................................................................. 50

Table 5.3 Pore size distribution (Sample 2) ................................................................. 51

Table 5.4 Summarized effective area and water flux .................................................. 55

Table 6.1 Average roughness of membrane ................................................................ 57

Table 6.2 Porosity of membrane .................................................................................. 57

Table 6.3 Average pore size......................................................................................... 58

Table 6.4 Comparison of water flux ............................................................................ 59

Table 6.5 Glucose rejection through different membrane ........................................... 62


vi

NOMENCLATURE

EDM Electric Discharge Machine

WEDM Wire-cut Electric Discharge Machine

Toff Pulse Off Time

Ton Pulse On Time

Ip Pulse Peak Current

Vp Pulse Peak Voltage

D Duty Factor

Wf Wire Feed

Fp Dielectric Flushing Pressure

Vs Supply Voltage

Sf Servo Feed

Wt Wire Tension

SR Surface Roughness

Ra Average Surface Roughness

MRR Material Removal Rate

HAZ Heat Affected Zone

SEM Scanning Electron Microscope

Vb Bulk Volume
vii

Vg Grain Volume

Vp Pore Volume

Ø Porosity

Wsat Weight of Saturated Sample

Wdry Weight of Dry Sample

ρ Density of Liquid
1. INTRODUCTION

1.1. OVERVIEW OF MEMBRANE TECHNOLOGY


The separation, concentration, and purification of molecular mixtures are
major problems in the chemical industries. Efficient separation processes are also
needed to obtain high-grade products in the food and pharmaceutical industries to
supply communities and industry with high-quality water, and to remove or recover
toxic or valuable components from industrial effluents. For this task a multitude of
separation techniques such as distillation, precipitation, crystallization, extraction,
adsorption, and ion-exchange are used today. More recently, these conventional
separation methods have been supplemented by a family of processes that utilize
semi-permeable membranes as separation barriers.

Membranes and membrane processes were first introduced as an analytical


tool in chemical and biomedical laboratories; they developed very rapidly into
industrial products and methods with significant technical and commercial impact
(Strathmann H., 2004). Today, membranes are used on a large scale to produce
potable water from sea and brackish water, to clean industrial effluents and recover
valuable constituents, to concentrate, purify, or fractionate macromolecular mixtures
in the food and drug industries, and to separate gases and vapours in petrochemical
processes. They are also key components in energy conversion and storage systems,
in chemical reactors, in artificial organs, and in drug delivery devices.

The membranes used in the various applications differ widely in their


structure, in their function and the way they are operated. However, all membranes
have several features in common that make them particularly attractive tools for the
separation of molecular mixtures. Most important is that the separation is performed
by physical means at ambient temperature without chemically altering the constituents
of a mixture. This is mandatory for applications in artificial organs and in many drug
delivery systems as well as in the food and drug industry or in downstream processing
of bio-products where temperature-sensitive substances must often be handled.
Furthermore, membrane properties can be tailored and adjusted to specific separation
2

tasks, and membrane processes are often technically simpler and more energy
efficient than conventional separation techniques and are equally well suited for large-
scale continuous operations as for batch-wise treatment of very small quantities.

Although synthetic membranes are widely used as valuable scientific and


technical tools in a modern industrialized society, they are not very well defined in
terms of their structure and function. The most prominent association that many
people have when thinking of a membrane resembles that of a filter, i.e. a device
capable of separating various components from a mixture according to their size (D.
Bhattacharyya & D. A.Butterfield, 2003).

Another characteristic property of a membrane is its perm selectivity, which is


determined by differences in the transport rates of various components in the
membrane matrix. The permeability of a membrane is a measure of the rate at which a
given component is transported through the membrane under specific conditions of
concentration, temperature, pressure, and/or electric field. The transport rate of a
component through a membrane is determined by the structure of the membrane, by
the size of the permeating component, by the chemical nature and the electrical charge
of the membrane material and permeating components, and by the driving force, i.e.
concentration, pressure or electrical potential gradient across the membrane. The
transport of certain components through a membrane may be facilitated by certain
chemical compounds, coupled to the transport of other components, or activated by a
chemical reaction occurring in the membrane. These phenomena are referred to as
facilitated, coupled, or active transport.

Synthetic membranes are not nearly as complicated in their structure or


function as biological membranes. They have only passive transport properties and
are usually less selective and energy efficient. In general, however, they have
significantly higher chemical and mechanical stability, especially at elevated
temperature. The selectivity of synthetic membranes is determined by a porous
structure according to their size or through a homogeneous structure according to the
solute solubility and diffusivity. The permeability of the membrane for different
components, however, is only one parameter determining the flux through the
membrane. Just as important as the permeability is the driving force acting on the
3

permeating components. Some driving forces such as concentration, pressure, or


temperature gradients act equally on all components, in contrast to an electrical
potential driving force, which is only effective with charged components. The use of
different membrane structures and driving forces has resulted in a number of rather
different membrane processes such as reverse osmosis, micro-, ultra- and nano-
filtration, dialysis, electro-dialysis, Donnan dialysis, pervaporation, gas separation,
membrane contactors, membrane distillation, membrane-based solvent extraction,
membrane reactors, etc.

1.2. TYPES OF MEMBRANE

1.2.1. Isotropic Membranes

There are different types of isotropic membranes viz. microporous membrane,


nonporous dense membrane and electrically charged membrane (Richard W. Baker,
2004). The isotropic membrane is shown figure 1.1.

a) Microporous Membranes: A microporous membrane is very similar in structure


and function to a conventional filter. It has a rigid, highly voided structure with
randomly distributed, interconnected pores. However, these pores differ from those
in a conventional filter by being extremely small, on the order of 0.01 to 10 μm in
diameter. All particles larger than the largest pores are completely rejected by the
membrane.

b) Nonporous, Dense Membranes: Nonporous, dense membranes consist of a dense


film through which permeates is transported by diffusion under the driving force of
a pressure, concentration, or electrical potential gradient. The separation of various
components of a mixture is related directly to their relative transport rate within the
membrane, which is determined by their diffusivity and solubility in the membrane
material. Thus, nonporous, dense membranes can separate permeates of similar size
if their concentration in the membrane material (solubility) differs significantly.

c) Electrically Charged Membranes: Electrically charged membranes can be dense


or microporous, but are most commonly very finely microporous, with the pore
walls carrying fixed positively or negatively charged ions. A membrane with fixed
4

positively charged ions is referred to as an anion-exchange membrane because it


binds anions in the surrounding fluid. Similarly, a membrane containing fixed
negatively charged ions is called a cation-exchange membrane.

Figure 1.1 Schematic diagrams of isotropic membranes

1.2.2. Anisotropic Membranes

The transport rate of a species through a membrane is inversely proportional to


the membrane thickness. High transport rates are desirable in membrane separation
processes for economic reasons; therefore, the membrane should be as thin as
possible. Conventional film fabrication technology limits manufacture of
mechanically strong, defect-free films to about 20 μm thickness. Anisotropic
membranes (Figure 1.2) consist of an extremely thin surface layer supported on a
much thicker, porous substructure.

The surface layer and its substructure may be formed in a single operation or
separately. In composite membranes, the layers are usually made from different
polymers. The separation properties and permeation rates of the membrane are
determined exclusively by the surface layer; the substructure functions as a
mechanical support. The advantages of the higher fluxes provided by anisotropic
membranes are so great that almost all commercial processes use such membranes.
5

Figure 1.2 Schematic diagrams of anisotropic membranes

1.3. MEMBRANE STRUCTURE AND MATERIAL

Synthetic membrane can be fabricated from a large number of different


materials. It can be made from organic or inorganic materials including solids such as
metal or ceramic, homogeneous films (polymers), heterogeneous solids (polymeric
mixes, mixed glasses), and liquids (R. H. Perry & D. H. Green , 1997).

1.3.1. Polymeric Membrane:

Polymeric membranes lead the membrane separation industry market because


they are very competitive in performance and economics many polymers are
available, but the choice of membrane polymer is not a trivial task. A polymer has to
have appropriate characteristics for the intended application. The polymer has to be a
suitable membrane former in terms of its chains rigidity, chain interactions, stereo
regularity, and polarity of its functional groups. The polymer has to be obtainable and
reasonably priced to comply with the low cost criteria of membrane separation
process. The most common polymers in membrane synthesis are cellulose acetate,
Nitrocellulose, and cellulose esters (CA, CN, and CE), polysulfone (PS), polyether
sulfone(PES), polyacrilonitrile (PAN), polyamide, polyethylene and polypropylene
(PE and PP), poly-tetrafluoro ethylene (PTFE), polyvinylidene fluoride (PVDF),
polyvinylchloride (PVC).
6

1.3.2. Ceramic Membrane:

Ceramic membranes are made from inorganic materials (such as alumina,


titania, zirconia oxides, recrystallised silicon carbide or some glassy materials). By
contrast with polymeric membranes, they can use in separations where aggressive
media (acids, strong solvents) are present. They also have excellent thermal stability
which makes them usable in high temperature membrane operations.

1.4. ADVANTAGES AND DISADVANTAGES OF MEMBRANE


TECHNOLOGY

In many applications, e.g. water desalination and purification the membrane


processes compete directly with the more conventional water treatment techniques.
However, compared to these conventional procedures membrane processes are often
energy efficient, simpler to operate and yield a higher quality product. The same is
true for the separation, concentration, and purification of drugs and food products or
in medical and pharmaceutical applications. These membrane processes have in
addition to high energy efficiency, simple operation, easy up and down scaling the
advantage of operating at ambient temperature avoiding any change or degradation of
products.

In water desalination reverse osmosis or electro-dialysis can be used.


Depending on local conditions, including water quality, energy cost and the required
capacity of the desalination plant, either electro-dialysis or reverse osmosis can be the
more efficient process. For very large capacity units and in case a power plant can be
coupled with the desalination unit, distillation is generally considered to be more
economical. For surface water purification and waste-water treatment membrane
processes, micro and ultra-filtration are competing with flocculation, sand bed
filtration, carbon adsorption, ion-exchange and biological treatment. In these
applications the membrane processes are usually more costly but generally provide a
better product water quality. Very often a combination of conventional water
treatment procedures with membrane processes results in reliable and cost-effective
treatment combined with high product water quality.
7

The environmental impact of all membrane processes is relatively low. There


are no hazardous chemicals used in the processes that have to be discharged and there
is no heat generation. The only effluent in desalination by reverse osmosis is a
concentrated brine solution. In seawater desalination this brine causes little problems
since it can be discharged directly into the sea. However, in brackish water
desalination the discharge of the concentrated brine can cause problems such that
brine post-treatment procedures might be necessary. Also, in surface water treatment
further processing of the concentrated effluent might be necessary (Richard W. Baker,
2004).

A disadvantage of membrane processes is that in many applications, especially


in the chemical and petrochemical industry, their long-term reliability is not yet
proven. Furthermore, membrane processes sometimes require excessive pre-treatment
due to their sensitivity to concentration polarization and membrane fouling due to
chemical interaction with water constituents. Furthermore, membranes are
mechanically not very robust and can be destroyed by a malfunction in the operating
procedure. However, significant progress has been made in recent years, especially in
reverse osmosis seawater desalination, in developing membranes which not only have
significantly better overall performance but which also show better chemical and
thermal stability and are less sensitive to operational errors.
2. LITERATURE REVIEW

2.1. REVIEW OF LITERATURE

Fumio Abe and Tadashi Fujita invented a separation membrane to be utilized,


beginning with gas-separation, in a wide variety of separation such as microfiltration,
ultrafiltration, reverse osmotic separation. A separation membrane was produced by
glassy porous membrane having substantially reticular microspores with an average
pore size of about 0.01µm to about 5 µm, obtained by a glassy-phase-separation
treatment, which glassy porous membrane being fixed on the surface of porous
support having an excellent mechanical strength, so that it is possible to reduce
sufficiently the thickness of porous membrane to about l0-500 µm and, furthermore,
in the process the metallic or ceramic membrane is deposited on the surface of phase-
separable glassy membrane which is suitable for depositing membrane thereupon by a
gaseous phase method and possesses an appreciable strength, vapour deposited
membrane having uniform, fine microspores with an average pore size of about
0.05µm to about 2 µm, can be produced with high stability. (Fumio Abe; Tadashi
Fujita , 1987)

Tim Van Gestel et al. prepared of novel hybrid metallic–ceramic membranes,


based on a porous 316L stainless-steel support material. The optimized membranes
were made by deposition of a fine suspension with a particle size of ~180 nm, a
colloidal sol with a particle size of ~30 nm and a nano-particle sol with a particle size
of ~5 nm and show a comparable multilayer structure as current ceramic membranes
for micro-filtration, ultra-filtration and nano-filtration and gas separation. The
essential new features of the membranes include the use of an alternative metallic
support material, which provides a high mechanical stability to the membrane (Tim
Van Gestel, 2008).

Kenneth L. Rubow et al. applied a novel manufacturing process to fabricate


Hiflow Nickel media that has high pore volume fraction and fine porosity for 0.1µm
particle filtration. The pore volume fraction in Hiflow Nickel media ranges from 40 to
65%. The flow pores are tortuous in nature and flow path lengths are long. Therefore,
9

even though the pore dimensions on the porous surface appear to be micrometre size
due to high surface roughness, the finer subsurface pores, high tortuosity and long
flow paths provide effective obstacle to the passage of sub-micron particles through
the media. This sintered metal microfiltration media was used for wastewater recovery
and other industrial liquid/solid separation processes (Dr. Kenneth L. Rubow, 1999).

Kew-Ho Lee et al. invented a method for preparing a metallic membrane,


which comprises dissolving a transition metal of Period 3 and its alloy particle
powder and synthetic polymer in a fixed ratio; radiating or casting to prepare a
membrane precursor; oxidizing the synthetic polymer on the membrane precursor
under a mixed gaseous atmosphere of nitrogen and hydrogen; and sintering the
membrane precursor at a predetermined temperature. The metallic membrane
prepared by this process has excellent mechanical and chemical properties and
enables to maintain a relatively small pore size and high porosity than traditional
membranes (Lee Kew-ho, Kim In-chu & Choi In-hwan, 2008).

Rune Bredesen et al. developed a method for manufacturing a composite


membrane structure of a thin metal membrane, for example of silver, palladium or
palladium alloys, for use in selective diffusion of gasses. The metal material for the
membrane is applied by sputtering as a coating on a base member having a low
surface roughness, to a desired thickness. The coating is pulled off from the base
member so as to form the metal membrane, and the metal membrane is placed on a
supporting substrate (Rune Bredesen, 2000).

Robert S. Zeller developed a high-porosity metallic membrane element


comprising a sintered element having at least about 55% porosity, the sintered
element comprising a matrix of substantially inter connected pores, each of the pores
being defined by a plurality of dendritic metallic particles. the author also disclosed a
method of making the high-porosity metallic membrane element which includes
depositing by air-laying techniques a substantially uniform low-density bed of a
sinterable dendritic material into a mould suitable for applying compressive force
thereto, compressing the low-density bed of sinterable dendritic material to form a
green form. The developed filter devices exhibit superior porosity and face velocities
(Robert S. Zeller, 1996).
10

Aalami–Aleagha et al. used the wire arc spraying technology for preparing
porous stainless steel membrane. The metallic membrane can be produced in disk and
tube shapes and various sizes. Wire arc spraying is an inexpensive process to produce
a porous structure in a short time. This technique has been used previously to produce
metal layers as a membrane for purifying water. In this paper, author investigated the
possibility of producing metallic membranes by the economic technology of arc
spraying for concentration of glucose solution. The essential purpose of this study was
to investigate the effect of alterations in arc spraying parameters such as stand-off
distance and atomizer air pressure on prepared membrane characteristics (Aleagha-
Aalami, S. S. Madaen & P. Daraei, 2008).

Dinesh Rakwal et al. investigated the slicing of germanium wafers from single
crystal, gallium-doped ingots using wire electrical discharge machining. Wafers with
a thickness of 350µm and a diameter of 66mm were cut using 75 and 100 µm
molybdenum wire. Wafer characteristics resulting from the process such as the
surface profile and texture are analysed using a surface profiler and scanning electron
microscopy. Detailed experimental investigation of the kerf measurement was
performed to demonstrate minimization of material wastage during the slicing process
using WEDM in combination with thin wire diameters. A series of timed etches using
two different chemical etchants were performed on the machined surfaces to measure
the thickness of the recast layer. Cleaning of germanium wafers along with its quality
after slicing is demonstrated by using Raman spectroscopy (Dinesh Rakwal, 2009).

Ree-Ho Kim et al. used a filtration technique using a metal membrane was
designed and developed for efficient and safe use of rainwater. The treatment system
consists of a feed tank containing rainwater and a metal membrane submerged into
the tank. Experiments were performed to compare filtration characteristics of
rainwater in a storage tank, roof runoff, and roof garden runoff. Ozone bubbling as
well as aeration in the feed side was considered to reduce membrane fouling and
inactivate microorganisms. Metal membranes appear to be suitable to clarify
rainwater because of their high treatment efficiency of microorganisms and
particulates. The major fouling mechanism for the metal membrane filtration was pore
blockage (Kim Reeho, Lee Sangho & Kim Jongoh, 2005).
11

S.R. Nithin Aravind et al. find the five optimal control parameters input
voltage, current, speed, pulse on/off time to maximize metal removal rate and
minimize surface roughness on wire-cut electrical discharge machining (WEDM).
WEDM is an electro thermal production process in which a thin single strand metal
wire in conjunction with de-ionised water, allows the wire to cut through metal by the
use of heat from electrical sparks. For the purpose to get a best solution to maximize
MRR and reduce SR, they used optimize parameters using Taguchi method. Also we
compare experimental reading with Taguchi optimum result to know the optimal
solution (S.R. Nithin Aravind, 2012).

Rajesh Choudhary et al. conducted investigations on the machining of EN-31


die steel with different electrode materials (copper, brass and graphite) with electrical
discharge machining (EDM) process. In this the analysis and evaluation of heat
affected zones (HAZ) of the workpiece surfaces machined using different tool
electrodes by EDM was studied. The kerosene oil of commercial grade has been used
as dielectric fluid. The effect of various important EDM parameters such as pulse
duration, peak current and discharge gap voltage has been investigated to yield the
responses in terms of material removal rate and surface roughness. Further the
detailed analysis of heat affected regions has been carried out by using scanning
electron microscopy (SEM) and optical microscopy (OM). Experimental results
indicate that copper as a tool electrode shows a good response towards MRR, whereas
brass gives superior surface finish as compared to other tool electrodes. From the
micro-structural analysis study it has been observed that heat affected zone is much
deeper in the specimen machined by graphite electrode as compared to other tool
electrodes (Rajesh Choudhary, 2010).
12

2.2. PROBLEM IDENTIFICAION

2.2.1. Problems with Polymeric Membrane:

Polymeric membranes cannot be used in high chloride environments, extreme


pH environments, at temperatures in excess of approximately 100⁰C and high
pressures. The applicability of polymeric membranes is also limited in slurries
containing high solids concentration, where the failure may be due to abrasion, or
high pressure. Disposal of polymeric membrane often poses an environmental
problem, and disposal of contaminated media is difficult and expensive (Dr. Kenneth
L. Rubow, 1999).

2.2.2. Problems with Ceramic Membrane:

Ceramic membranes are strong but brittle, and must be sealed using polymeric
seals. The temperatures and corrosive environments that the seals can withstand limit
the use of ceramic membranes. Ceramic membranes have low fracture toughness,
therefore, back-pulsing or thermal cycling may introduce cracks, and the cracks may
propagate rapidly leading to final brittle failure. The ceramic membrane are also
characterised by very high weights and considerable production costs of the components.
(Dr. Kenneth L. Rubow, 1999).

In order to overcome such problems with polymeric and ceramic membranes,


metallic membranes are used in membrane filtration process. Metallic membranes
have higher fracture toughness, high thermal shock resistance and are completely
weldable. But the most of the porous metal filters are made by sintered metal
particles, which are also characterised by very high weights and considerable
production cost. Moreover, it is necessary to maintain a good condition of sintered
particle to reproduce the same filtration characteristics. The dense metal membranes
mostly made up of Palladium (Pd) and its alloys are being considered for a variety of
filtering operation. Palladium, however, is very expensive. As a result, there is need to
focus on development of thin metallic membrane with thickness ranging from
submicron to several tens of microns.
13

So in the present study a machining of metallic membrane through electric


discharge machining is studied. In this technique there is no sintering of particles,
instead of that, a metal a machined using WEDM to develop a thin metallic
membrane. Moreover, using a WEDM, we can develop a thin membrane of various
metals like aluminium, stainless steel, etc. Also membrane developed from titanium
can resist to high temperature and acid and base solutions.

2.3. OBJECTIVE OF PROJECT

1. To develop a metal membrane using Electric Discharge Machining.


2. To analyse the characteristics of a metal membrane.

2.4. METHEDOLOGY OF PROJECT


1. Study of Research papers for understanding recent techniques and process for
development of metal membrane.
2. Study of WEDM mechanism and its different controlling parameters.
3. Study of previously developed metal membrane and its application.
4. Trail machining of membrane on aluminium.
5. Testing of various characteristics for metal membrane like porosity,
permeability, pore size and pore size distribution.
6. Development of membranes of different thickness and analyses of its
different characteristics.
7. Validating the result and deriving the conclusions.
14

Figure 2.1 Flow Chart of Methodology


3. WIRE-CUT EDM

3.1. INTRODUCTION
The wire-cut EDM uses a very thin wire 0.02 to 0.03 mm in diameter as an
electrode. The work piece is machined by electric spark discharges between the thin
electrode and the work (anode) by moving either the work piece or wire (like a band
saw). In WEDM, a thin copper or brass wire is used as the electrode to machine the
work piece as programmed; hence forming electrode is not needed. This feature helps
reduce man-hours requirements and ensures grater economy due to use of an
inexpensive electrode material. Since the electrode is constantly feed during
machining, its wear can be practically neglected. Since, the new portion of wire
electrode is constantly supplied at a speed of about 10 to 30 mm/sec machining can be
continued without any accumulation of chips and gases and a uniform surface of
about 5 to 10 µm Rmax. Therefore the dies machined by this process without any
polishing. A total machining tolerance of 0.01 mm is possible and better temperature
control and machining know-how may provide a machining tolerance as close as 0.05
mm. By using this process, complicated and very minute shapes can be machined by
unskilled operators using program alone. EDM machines can be operated unattached
for a very longer time at high operating rate. Straight holes can be produce to close
tolerances. The typical electrode materials used are tungsten, graphite, copper and
brass. The wire rotates in orbital direction, which decreases electrode wear and
increases the accuracy and surface finish.

WEDM has tremendous potential in its applicability in the present day metal
cutting industry for achieving a considerable dimensional accuracy, surface finish and
contour generation features of products or parts. Moreover, the cost of wire
contributes only 10% of operating cost of WEDM process. The difficulties
encountered in the die sinking EDM are avoided by WEDM, because complex design
tool is replaced by moving conductive wire and relative movement of wire guides.
16

3.2. PRINCIPLE OF OPERATION OF WIRE-CUT EDM

The WEDM machine tool comprises of a main worktable (X-Y) on which the
work piece is clamped; an auxiliary table (U-V) and wire drive mechanism. The main
table moves along X and Y-axis and it is driven by the D.C servo motors. The
travelling wire is continuously feed from wire feed spool and collected on take up
spool which moves though the work piece and is supported under tension between a
pair of wire guides located at the opposite sides of the work piece. The lower wire
guide is stationary whereas the upper wire guide, supported by the U-V table, can be
displaced transversely along U and V-axis with respect to lower wire guide. The
upper wire guide can also be positioned vertically along Z-axis by moving the quill.

A series of electrical pulses generated by the pulse generator unit is applied


between the work piece and the travelling wire electrode, to cause the electro erosion
of the work piece material. As the process proceeds, the X-Y controller displaces the
worktable carrying the work piece transversely along a predetermined path
programmed in the controller. While the machining operation is continuous, the
machining zone is continuously flushed with water passing through the nozzle on both
sides of work piece. Since water is used as a dielectric medium, it is very important
that water does not ionize. Therefore, in order to prevent the ionization of water, an
ion exchange resin is used in the dielectric distribution system to maintain the
conductivity of water.

In order to produce taper machining, the wire electrode has to be tilted. This is
achieved by displacing the upper wire guide (along U-V axis) with respect to the
lower wire guide. The desired taper angle is achieved by simultaneous control of the
movement of X-Y table and U-V table along their respective predetermined paths
stored in the controller. The path information of X-Y table and U-V table is given to
the controller in terms of linear and circular elements via NC program. Figure 3.1
exhibits the schematic diagram of the basic principle of WEDM process (Saha,
Singha, & Pal, 2008). The complete block diagram of WEDM is shown in Figure 3.2.
Figure 3.3 shows the detail of WEDM cutting gap (N. Tosun and Cogun, 2003).
17

Figure 3.1 Schematic diagram of the basic principle of WEDM process

Figure 3.2 Block diagram of WEDM


18

3.3. MECHANISM OF MATERIAL REMOVAL IN WEDM


PROCESS
The mechanism of metal removal in wire electrical discharge machining
mainly involves the removal of material due to melting and vaporization caused by
the electric spark discharge generated by a pulsating direct current power supply
between the electrodes. In WEDM, negative electrode is a continuously moving wire
and the positive electrode is the work piece. The sparks will generate between two
closely spaced electrodes under the influence of dielectric liquid. Water is used as
dielectric in WEDM, because of its low viscosity and rapid cooling rate (Y. K. Lok
and T.C. Lee, 1997).

No conclusive theory has been established for the complex machining process.
However, empirical evidence suggests that the applied voltage creates an ionized
channel between the nearest points of the work piece and the wire electrodes in the
initial stage. In the next stage the actual discharge takes place with heavy flow of
current and the resistance of the ionized channel gradually decreases. The high
intensity of current continues to further ionize the channel and a powerful magnetic
field is generated. This magnetic field compresses the ionized channel and results in
localized heating. Even with sparks of very short duration, the temperature of
electrodes can locally rise to very high value which is more than the melting point of
the work material due to transformation of the kinetic energy of electrons into heat.
The high energy density erodes a part of material from both the wire and work piece
by locally melting and vaporizing and thus it is the dominant thermal erosion process.
19

Figure 3.3 Detail of WEDM cutting gap

3.4. VARIOUS INPUT PARAMETERS OF WEDM


1. Pulse off time (Toff)
2. Pulse on time (Ton)
3. Pulse peak current (Ip)
4. Pulse peak voltage (Vp)
5. Duty factor (D)
6. Wire feed (Wf)
7. Dielectric flushing pressure (Fp)
8. Supply voltage (Vs)
9. Dielectric
10. Wire electrode material
11. Servo feed (Sf)
12. Wire tension (Wt)
20

3.5. VARIOUS OUTPUT PARAMETERS OF WEDM


1. Surface roughness (SR)
2. Material removal rate (MRR)
3. Spark gap
4. Power consumption

3.6. PROCESS PARAMETERS OF WEDM AND ITS INFLUENCE


ON WEDM

1. Pulse on time (Ton):

The pulse on time is referred as Ton and it represents the duration of time in
micro seconds (μs) for which the current is flowing in each cycle (Figure 3.4).
During this time the voltage (Vp) is applied across the electrodes. The equivalent
time setting in micro seconds is given in Appendix B. The single pulse discharge
energy increases with increasing Ton period, resulting in higher cutting rate. With
higher values of Ton, however, surface roughness tends to be higher. The higher
value of discharge energy may also cause wire breakage.

2. Pulse off time (Toff):

The pulse off time is referred as Toff and it represents the duration of time in
micro seconds (μs) between the two simultaneous sparks (Figure 3.4). The voltage
is absent during this part of the cycle. The equivalent time setting in micro
seconds is given in Appendix B. With a lower value of Toff, there is more number
of discharges in a given time, resulting in increase in the sparking efficiency. As a
result, the cutting rate also increases. Using very low values of Toff period,
however, may cause wire breakage which in turn reduces the cutting efficiency.
As and when the discharge conditions become unstable, one can increase the Toff
period. This will allow lower pulse duty factor and will reduce the average gap
current.
21

Ton Toff

Vp

t(µs)

Figure 3.4 Series of electrical pulses at the inter electrode gap

3. Pulse Peak Current (Ip):

The peak current is represented by Ip and it is the maximum value of the


current passing through the electrodes for the given pulse. The Ip setting current
range available on the present WEDM machine is 10 – 230 ampere which is
applied in steps of 10 ampere. Increase in the Ip value will increase the pulse
discharge energy which in turn can improve the cutting rate further. For higher
value of Ip, gap conditions may become unstable with improper combination of
Ton, Toff & Vs settings. As and when the discharge conditions become unstable one
must reduce the Ip value (Tarng & Chung, 1995).

4. Pulse Peak Voltage (Vp):

Pulse peak voltage setting is for selection of open gap voltage. Increase in the
Vp value will increase the pulse discharge energy which in turn can improve the
cutting rate. The pulse peak voltage setting range available on the machine is 1 to
4. Normally it is selected at value 3.

5. Wire Feed (Wf):

Wire feed is the rate at which the wire-electrode travels along the wire guide
path and is fed continuously for sparking. The wire feed range available on the
present WEDM machine is 1–15 m/min in steps of 1m/min. It is always desirable
to set the wire feed to maximum. This will result in less wire breakage, better
machining stability and slightly more cutting speed.
22

6. Spark Gap Set Voltage:

The spark gap set voltage is a reference voltage for the actual gap between the
work piece and the wire used for cutting. The Vs voltage range available on the
present machine is 0 - 99 volt and is applied in steps of 1 volt.

7. Dielectric Flushing Pressure (Fp):

Flushing Pressure is for selection of flushing input pressure of the dielectric.


The flushing pressure range on this machine is either 1 (High) or 0 (low). High
input pressure of water dielectric is necessary for cutting with higher values of
pulse power and also while cutting the work piece of more thickness. Low input
pressure is used for thin work piece and in trim cuts.

8. Servo Feed (Sf):


Servo feed setting decides the servo speed; the servo speed, at the set value of
Sf, can vary in proportion with the gap voltage (normal feed mode) or can be held
constant while machining (with constant feed mode).

9. Wire Tension (Wt):

Wire tension determines how much the wire is to be stretched between upper
and lower wire guides. This is a gram-equivalent load with which the
continuously fed wire is kept under tension so that it remains straight between the
wire guides. More the thickness of job more is the tension required. Improper
setting of tension may result in the job inaccuracies as well as wire breakage.

10. Material Removal Rate (MRR):

MRR is usually expressed as cubic mm per hour (mm3/hr). Mathematically


written as: [Electrode area (mm2) x Depth of cut (mm)] / Time of cut (min)
Achieving an efficient MRR is not simply a matter of good machine setting. It
also includes direct energy dissipated in the EDM process. This energy can be
dissipated in three ways:

a. In the work piece: MRR is influenced by the thermal conductivity of


work piece. Copper for example has a low melting point but has also
23

low MRR as it is a good conductor of heat. On the other hand, steel has
a high melting point but a low thermal conductivity, hence has a higher
MRR.
b. In the gap: Particles in the work gap will contribute significantly to
slowing down the MRR.
c. In the electrode: The electrode and the work piece selection also
influence the MRR.

11. Gap Size:

This is one of the most crucial parts of the EDM system. The size of the gap is
governed by the servo control system whose motion is controlled by gap width
sensors. They control the motion of the ram head or the quill which in turn the gap
size. Typical values of the gap size are between 0.01 to 0.05 mm, although gap
sizes as small as of several hundred to several thousands of micrometres can be
found depending on the application, current, voltage and the dielectric media. To
maintain a constant gap size the feed rate should be equal to the MRR. The gap
size governs the possibility of sparking and arcing.

12. Surface Finish:

The EDM process produces surface that contains a layer of recast spattered
metal which is usually hard and cracked. Below this recast layer it is possible to
have some surface alterations due to abusive machining. These are more
pronounced when we use abusive machining conditions. The last layer is the heat
affected zone or the annealed layer, which has only been heated, not melted. The
depth of the recast and the heat affected zone is determined by the heat sinking
ability of the material and the power used for the cut. The altered metal zone
influences the quality of the surface integrity. Other machining processes like
Laser Beam Machine (LBM) and Electro Chemical Machining (ECM) produce
the same kind of surface alterations as in EDM.
24

3.7. ADVANTAGES OF WEDM PROCESS


1. As continuously travelling wire is used as the negative electrode, so electrode
fabrication is not required as in EDM.
2. There is no direct contact between the work piece and the wire, eliminating the
mechanical stresses during machining.
3. WEDM process can be applied to all electrically conducting metals and alloys
irrespective of their melting points, hardness, toughness or brittleness.
4. Users can run their work pieces over night or over the weekend unattended.

3.8. DISADVANTAGES OF WEDM PROCESS


1. High capital cost is required for WEDM process.
2. There is a problem regarding the formation of recast layer.
3. WEDM process exhibits very slow cutting rate.
4. It is not applicable to very large work piece.

3.9. APPLICATIONS OF WEDM PROCESS

The present application of WEDM process includes automotive, aerospace,


mould, tool and die making industries. WEDM applications can also be found in the
medical, optical, dental, jewellery industries, and in the automotive and aerospace R
& D areas (Newman, Ho, Rahimifard, & Allen, 2004).

The machine’s ability to operate unattended for hours or even days further
increases the attractiveness of the process. Machining thick sections of material, as
thick as 200 mm, in addition to using computer to accurately scale the size of the part,
make this process especially valuable for the fabrication of dies of various types. The
machining of press stamping dies is simplified because the punch, die, punch plate
and stripper, all can be machined from a common CNC program. Without WEDM,
the fabrication process requires many hours of electrodes fabrication for the
conventional EDM technique, as well as many hours of manual grinding and
polishing. With WEDM the overall fabrication time is reduced by 37%, however, the
processing time is reduced by 66% (G. F. Benedict, 1987).
4. MACHINING OF MEMBRANE ON WEDM

4.1. WIRE-CUT EDM


In order to develop a membrane, the following setup is made available at
Mechanical Engineering Department, V.N.I.T., Nagpur. The WEDM machine is
utilized for the machining of membrane. The WEDM machine basically consists of:

1. Work piece counter movement control unit


2. Work piece mounting table
3. Wire drives section for feeding the wire at a constant tension
4. Machining power supply
5. A unit, which supplies a dielectric fluid with constant specific resistance.

The machining includes workpiece of aluminium of uniform thickness on the


Ezee Cut Plus model of WEDM. The machining process includes the study of various
input parameters and the output parameters of WEDM. Since WEDM is a necessary
process with a high cost, it is required that appropriate machining parameters are
selected for machining operation. The machine which is used for machining of
membrane is shown in figure 4.1.
26

Figure 4.1 Ezee Cut Plus Wire EDM


27

Table 4.1 Technical Specification of WDEM

Control Panel E2 – 01

Control Mode CNC, Close Loop

Simultaneously Controlled Axis X, Y, U, V

Control Panel Size 550 x 800 x 1830 mm

Input Program Format G Code

Control Panel Weight 175 kg

Display 15” Colour Monitor

Minimum Input Command 0.001 mm

Minimum Increment 0.001 mm

Power Requirement 415 V / 50 Hz / 3 Phase, 1.5 KVA Max.

Electrode Material 0.25 mm Brass wire

Cathode Electrode

Anode Work Material


28

Figure 4.2 Control panel of WDEM


29

4.2. INPUT PARAMETER

Here input parameters are set manually. These set values can be detected from
the control panel, display system for displaying wire feed sensed by sensor, etc. For
example, pulse peak current is set by operating keyboard of control panel monitor,
wire feed is set by observing value at display system, etc.

4.3. MACHINING TECHNIQUE FOR DEVELOPMENT OF


MEMBRANE
The machining of membrane on WEDM is carried on aluminium square bar of
width 1.25 inch and round bar of diameter 1.25 inch using brass wire of 250 µm
diameter. The aluminium work piece is mounted on a table of WEDM and slicing of
the work piece is done using simple straight line program on WEDM.

Before slicing a work piece a reference machining is carried out on the


aluminium workpiece. This reference cut is done for maintaining the parallelism on
both sides during the slicing. The pictorial representation of reference cutting is
shown in figure 4.3.

Figure 4.3 Reference machining of workpiece


30

After reference machining on the workpiece, the microscopic study of


machined surface reveals the presence of three kinds of layers, e.g., recast layer, heat
affected zone (HAZ) and converted layer. Figure 4.4 shows the three kinds of layers
developed on the machined surface. If molten material from the workpiece is not
flushed out quickly, it will resolidify and harden due to the cooling effect of the
dielectric and gets adhered to the machined surface. This thin layer of about 2.5-50
μm is formed and is called re-cast layer. It is extremely hard, brittle and porous and
may contain micro cracks. Beneath the recast layer, a HAZ is formed due to rapid
heating and quenching cycles during EDM. This layer is approximately 25 μm thick.
The heating-cooling cycle and diffused material during machining are the responsible
reasons for the presence of this zone. Thermal residual stresses, grain boundary
weaknesses, and grain boundary cracks are some of the characteristics of this zone.
Conversion zone (or converted layer) is identified below the HAZ and is characterized
by a change in grain structure from the original structure (Rajesh Choudhary, 2010).

Figure 4.4 Schematic diagram of three kinds of layers on an WEDM machined


surface

After machining the reference cut, a slicing of the aluminium workpiece is


done using a simple straight line program on WEDM to form an aluminium
membrane. The thickness of the slicing program is adjusted in such a way that the
membrane obtained after slicing having average thickness between 90 – 180 µm.
Figure 4.5 shows the schematic representation of the slicing of workpiece.
31

Figure 4.5 Schematic representation of the slicing of workpiece

The thickness of the sliced workpiece is between 90 – 180 µm and having


average thickness of 120 µm. The dense parent material layer, which is beneath the
HAZ layer, is getting converted into the recast layer due to the slicing of the
workpiece. This recast layer gets deposited on both sides of the sliced surface. HAZ
and the recast layer are fundamentally porous in nature due to inherent cracks and
micro craters. These craters are randomly distributed across the surface and are
interconnected. This very interconnection of the craters is responsible for the
development of the porous metallic membrane shown in figure 4.6.

Figure 4.6 Schematic diagram of cross section of machined membrane


32

Figure 4.7 shows the actual photograph of WEDM during slicing of


aluminium workpiece.

Workpiece

Wire

Workpiece Holder
Wire Guide
Rollers

Figure 4.7 Slicing of the aluminium work piece on WEDM

The numbers of membranes are machined using this technique by varying the
input parameters (i.e. Pulse). In this experimentation the membranes are machined
using two different pulses. The pulse decides the value of Ton and Toff. In particular
sample 1 is machined by using pulse 3 and sample 2 is machined by using pulse 4.
Details of Ton and Toff values for different pulses are given in Appendix B.

The various input parameters for sample 1 and sample 2 is given in table 4.2.
Figure 4.8 (a) and figure 4.8 (b) shows the picture of control panel window for sample
1 and sample 2 respectively. Figure 4.9 shows the actual photograph of the membrane
samples.
33

Table 4.2 Input Parameters

Input Parameter Fix Parameters Variable Parameters

 Pulse = 3
 Wire Feed rpm = 800 rpm
Sample 1  Ton = 0.15 mSec.
 Spark Gap = 25 micron
 Toff = 0.52 mSec.
 Upper Pressure = 0.1 kg/cm2
 Lower Pressure = 0.2 kg/cm2
 Pulse = 4
 Supply Voltage = 75 Volt
Sample 2  Ton = 0.08 mSec.
 Pulse Peak Current = 0.5 Amp
 Toff = 0.56 mSec.

(a) (b)
Figure 4.8 Control panel window

Figure 4.9 shows the actual picture of both the membrane samples.

Sample 1 Sample 2

Figure 4.9 Membrane samples


5. MEMBRANE CHARACTERISATION

Membrane processes are playing an ever-increasing role as


environmental engineers continue to seek sustainable methods for water treatment,
wastewater reclamation, groundwater restoration, and pollution prevention. Mitigation
of membrane fouling and maximization of water productivity are essential for
optimizing membrane processes. Membrane fouling results from the attachment,
accumulation, or adsorption of substances onto the membrane surface and/or within
the membrane pores; it hinders membrane performance and shortens membrane life.
Physical and chemical interactions between solutes or particles and the membrane
interface substantially affect water productivity and the rate at which membrane
fouling occurs.

A variety of techniques and approaches are routinely used for characterizing


the physical and chemical properties of membrane surfaces. Measuring the contact
angle that is formed when a droplet of water is placed on the membrane surface is
used to quantify the hydrophobicity / hydrophilicity of the membrane surface. Atomic
force microscopy is used to both quantify and visualize the morphology or roughness
of membrane surfaces. While numerous other characteristics like porosity, pore size
and pore distribution may be measured for membrane surfaces. This strong interest is
attributed to the relative importance of each of these properties in determining
permeate flux rates, solute rejection, and fouling characteristics for micro porous
(microfiltration, ultrafiltration) membrane.

5.1. CONTACT ANGLE MEASUREMENTS

The contact angle (θ) that is formed at the three-phase interface between solid,
liquid, and gas/vapour phases (Figure 5.1) may be used to obtain information
regarding membrane surface energy properties. The information that is gathered from
contact angle analysis may be used to calculate specific surface energy properties
(van-der Waals, Lewis acid-base) for detailed interfacial analyses, as well as for
qualitatively assessing the wettability, or hydrophobicity/hydrophilicity, of a
membrane surface.
35

There are many methods for determining the contact angle of liquid on the
surface, out of which the static sessile drop method is commonly used. The sessile
drop contact angle is measured by a contact angle goniometer using an optical
subsystem to capture the profile of a pure liquid on a solid substrate. The angle
formed between the liquid/solid interface and the liquid/vapour interface is the contact
angle. Angles measured in such a way are often quite close to advancing contact
angles (Mittal, 2006).

For the membrane to be used as a filtration unit for liquid the contact angle
must be less than 90º (θ < 90º), so that the liquid wet the surface of membrane. As a
result of this, the liquid can easily penetrate through the pores in the membrane.

Figure 5.1 Digital image of a liquid droplet on a dry surface in which the contact
angle (θ) is measured according to the sessile drop method.

The contact angle is measured according to the sessile drop method. In this
method a distilled water drop is placed on the dry and clean surface of the membrane.
The front sectional image is taken through camera as shown in figure 5.2.
36

Water Droplet

Membrane Surface

Contact Angle (θ)

Figure 5.2 Water droplet on membrane surface

The measurement of contact angle is done through image processing tool in


MATLAB 2014a. In this tool the image shown in figure 5.2 is processed and two
lines are drawn on the image. The first line is drawn parallel to the membrane surface
while the second is drawn tangent to the droplet. In order to calculate the equilibrium
contact angle, the tangent line is drawn on both side of the droplet. Using the
MATLAB program (Appendix A) the angle between the membrane surface and line
tangent to droplet is calculated. The program window of the MATLAB program is
shown in figure 5.3.
37

Figure 5.3 MATLAB program window

The output window is marked on the figure 5.3 which shows the inclination of
the membrane with respect to the horizontal plane and angle between the membrane
surface and the tangent to the water droplet.
38

The contact angle is calculated as:

( ) (Eq. 5.1)

Therefore,

Contact angle (θ1) = 44.58º - 0.46º

Contact angle (θ1) = 44.12º

Similarly, on the other side contact angle is calculated and its value is θ2 = 43.11º

The Equilibrium Contact angle is calculated as:

( ) (Eq. 5.2)

Therefore,

Equilibrium Contact angle (θ) = 43.61º

The value of contact angle is 43.61º which is less than 90º, hence the water
wets the membrane surface and it can penetrate easily through the pores of the
membrane.

5.2. SURFACE MORPHOLOGY

Surface morphology basically deals with the surface roughness of the


membrane surface. Surface roughness is measured using surface roughness tester. The
membrane surface can be scanned in vacuum, air, or water and no sample preparation
is necessary. The roughness value is measured in terms of average roughness (Ra).
Chung et al. determined the relationship between Ra and the water flux and separation
performance of UF membranes. As Ra decreased, flux decreased and rejection
increased (Chung, Qin, Huan, & Toh, 2002).

The average roughness value of membrane is determined using MITITOYO


Surface Measurement Surftest SV – 3000. This instrument functions on the basis of
39

tracing principle. It traces the surface with the help of sensitive sensor. This output of
sensor is converted into required surface properties using SURFPAK – SV software.
The machine is shown is figure 5.4.

Figure 5.4 Surface Roughness Measurement Surftest SV - 3000

The average roughness value of membrane surface of two samples shown in


figure 5.5 is taken in two directions i.e. in the direction of the motion of wire and in
the direction perpendicular to the direction of motion of wire. The cut-off length of
testing of Ra value is taken as 0.8 mm and evaluation length of 4 mm. The resolution
is taken as 0.01µm and stylus speed of 0.1 mm/sec. The graph of average surface
roughness of sample 1 and 2 is shown in figure 5.6 and figure 5.7 respectively.
40

Sample 1 Sample 2

Figure 5.5 Membrane tested for surface roughness

Figure 5.6 Graph of surface roughness of sample 1

Figure 5.6 (a) shows the graph of surface roughness and average roughness
value of sample 1 taken in direction of motion of wire, whereas figure 5.6 (b) shows
that of taken in perpendicular direction of motion of wire. The value of Ra in the
direction of motion of wire is 4.134 µm, whereas that in the perpendicular direction of
motion of wire, the Ra value is 2.984 µm.
41

Figure 5.7 Graph of surface roughness of sample 2

Figure 5.7 (a) shows the graph of surface roughness and average roughness
value of sample 2 taken in direction of motion of wire, whereas figure 5.7 (b) shows
that of taken in perpendicular direction of motion of wire. The value of Ra in the
direction of motion of wire is 5.965 µm, whereas that in the perpendicular direction of
motion of wire, the Ra value is 9.962 µm.
42

5.3. POROSITY OF MEMBRANE


Porosity is a measure of the void (i.e. empty) spaces in the material and
generally expressed in percentage between 0 to 100%. Porosity can be estimated
through volumetric measurements of membrane samples. The porosity can be
calculated using a balance volume method which is expressed in equation 5.4.

Vb = Vg + Vp (Eq. 5.4)

Where, Vb – Bulk Volume

Vg – Grain Volume

Vp – Pore Volume

Bulk volume measurements are classified into two types: linear measurement
and displacement methods. Linear measurement is simply physically measuring the
sample with a venire calliper and then applying the appropriate geometric formula.
This method is quick and easy, but is subject to human error and measurement error if
the sample is irregularly shaped. Displacement methods rely on measuring either
volumetrically or gravimetrically the fluid displaced by the sample. Gravimetric
methods observe the loss in weight of the sample when immersed in a fluid, or
observe the change in weight of a pycno-meter filled with mercury and with mercury
and the sample. Volumetric methods measure the change in volume when the sample
is immersed in fluid.

The bulk volume of the two membrane samples shown in figure 5.5 is
calculated using a linear measurement.

Sample 1:

Vb1 = length × breadth × thickness

Vb1 = 31.65 × 31.52 × 0.11 mm

Vb1 = 109.73 mm3


43

Sample 2:

Vb2 = × (diameter)2 × thickness

Vb2 = × 31.24 × 0.18 mm

Vb2 = 137.97 mm3

A pore volume is measured using a method called as the fluid re-saturation


method. A clean and dried sample is weighted, saturated with a liquid of known
density, and then reweighed. The difference in weight (Wsat - Wdry) is divided by the
density of the fluid gives the value of the pore volume.

Liquid

Sample Immersed
in Liquid

Figure 5.8 Fluid Re-saturation Method


For the measurement of the pore volume of the membrane samples, weights of
the dry and clean samples are taken using a weighing machine (Wdry). Then the
samples are immersed in the turpentine solution for 2 days and taken out and then
weight is taken (Wsat) shown in figure 5.9. Here turpentine solution is taken, since it
has a low surface tension than that of water and also lower density than that of water.
The density of turpentine solution is ρ = 870 kg/m3.

The pore volume (Vp) is calculated using equation 5.5.

(Eq. 5.5)
( )

Weight of liquid displaced = Wsat - Wdry (Eq. 5.6)


44

Porosity is calculated using the equation 5.7.

Porosity (Ø) = (Eq. 5.7)

Figure 5.9 Membrane samples immersed in turpentine solution

The calculated value of pore volume and porosity is shown in table 5.1

Table 5.1 Pore volume and porosity

Weight of liquid Pore Volume


Sample Wsat (gm) Wdry (gm) Porosity (Ø)
displaced, W (gm) (Vp) mm3

Sample 1 0.2637 0.2545 0.0092 10.574 9.63%

Sample 2 0.4069 0.3969 0.01 11.49 8.33%


45

5.4. PORE SIZE AND PORE SIZE DISTRIBUTION


The pore size and pore size distribution is measured using Scanning Electron
Microscope (SEM). The SEM (Model JEOL-6380A) used for measurement is shown
in figure 5.10. For scanning electron microscopy (SEM) measurements a sample
surface is exposed to a narrow beam of electrons in vacuum. Secondary electrons are
liberated from the surface and detected. The highly focused and optical zoomed image
is obtained using SEM.

Figure 5.10 Scanning Electron Microscope (SEM)


46

Both the surface of the membrane samples are scanned using SEM and the
scanned images are obtained as shown in figure 5.11. The image obtained from SEM
shows the pores on the membrane surface.

(a) (b)

(c) (d)

Figure 5.11 SEM image of membrane surface

5.4.1. Pore Size:

The pore size of the membrane is measured using image processing tool of the
MATLAB 2014a. The diameter of the pores is measured using a program which
processes the SEM image which is having a calibrated scale of 10 µm and 5 µm.
Using this calibrated scale the diameter of pore is measured using interpolation
technique. The program window of the MATLAB is shown in figure 5.12.
47

Figure 5.12 Program window of MATLAB

The average diameter range of the pores of sample 1 (Figure 5.11, a & b) is 1 -
6 µm. The diameters value is shown in figure 5.13 and 5.14

Figure 5.13 Pore diameters of sample 1 (Side 1)


48

Figure 5.14 Pore diameters of sample 1 (Side 2)

Similarly, the diameter of the pores on the sample 2 (Figure 5.11 c & d)
having a range of 3 - 8 µm. The diameters value is shown in figure 5.15 and 5.16.

Figure 5.15 Pore diameters of sample 2 (Side 1)


49

Figure 5.16 Pore diameters of sample 2 (Side 2)

5.4.2. Pore Size Distribution:

The pore-size distribution is the relative abundance of each pore size in a


representative area of membrane. Pore size distribution includes the number of pores
of a specific size on the membrane surface. Major importance of a membrane’s pore
size distribution is that it relates to other membrane properties in a complex and useful
way. It indicates complexity of structure in far more detail than porosity alone. The
spatial variation of pore size is an important characteristic of the medium. The pore
distribution is also measured using MATLAB program (Appendix A). The program
window of MATLAB is shown in figure 5.12. For the measurement of the distribution
of pores the SEM images of the membrane surface is used. Table 5.2 and figure 5.17
show the pore size distribution of membrane sample 1. Similarly, table 5.3 and figure
5.18 show the pore size distribution of membrane sample 2.
50

Table 5.2 Pore size Distribution (Sample 1)

Range (µm) Diameter (µm) Frequency

0 to 1 0 0
1 to 2 1 5
2 to 3 2 15
3 to 4 3 4
4 to 5 4 2
5 to 6 5 1
6 to 7 6 0
7 to 8 7 0
8 to 9 8 0
9 to 10 9 0

16

14

12
Frequncy of pores

10

0
0 1 2 3 4 5 6 7 8 9
-2
Pore Diameter in microns

Figure 5.17 Pore size distribution chart (Sample 1)


51

Table 5.3 Pore size Distribution (Sample 2)

Range (µm) Diameter (µm) Frequency

0 to 1 0 0
1 to 2 1 1
2 to 3 2 9
3 to 4 3 4
4 to 5 4 3
5 to 6 5 2
6 to 7 6 1
7 to 8 7 0
8 to 9 8 0
9 to 10 9 0

9
8
7
6
Frequency

5
4
3
2
1
0
0 1 2 3 4 5 6 7 8 9 10
-1
Pore Diameter in microns

Figure 5.18 Pore size distribution chart (Sample 2)


52

5.5. PERMEABILITY OF MEMBRANE


Permeability is very important characteristics of the membrane. Permeability
of membrane gives rate at which the fluid can be filtered through the membrane. This
is called as the flux of the membrane.

The permeability of the membrane samples is measured using a dead end


filtration apparatus shown in figure 5.19.

Inlet

Air Inlet Pressure Gauge

Test Membrane

Magnetic Stirrer Outlet

Figure 5.19 Dead end filtration apparatus

In order to test the permeability of membrane samples, membrane samples are


pasted on the 0.45 mm thick aluminium sheet. This is done because the sample size of
membrane which is to be tested on the apparatus is much larger than that of
membrane machined through WEDM. Hence the metallic membranes are pasted on
53

the aluminium sheet. Figure 5.20 shows the membrane samples pasted on aluminium
sheet.

Aluminium Sheet of
thickness 0.45 mm

Porous Metal
Membrane

Figure 5.20 Metallic membrane pasted on aluminium sheet

Figure 5.21 Metallic Membrane placed on Apparatus


54

The dead end filtration apparatus is generally used to determine the water flux
of the membrane. The water flux (L/m2-hr) of the membrane is calculated using the
equation 5.8.

Water Flux = (Eq. 5.8)

Where,

V - Volume of premeated water (L)

A - Effective area of the membrane (mm2)

t - Time duration for collecting the premeated water (hr.)

The determination of the water flux is done using the dead end filtration
apparatus. In this method a known volume of water is pour into the apparatus fitted
with the test metallic membrane. The pressure is applied on the water through air
compressor and its value is kept constant at 10 kg/cm2. Time is measured till the
complete volume of water is collected from the outlet if the apparatus. Before the
membrane to be fitted on the apparatus its effective area is calculated using linear
measurement technique.

Three types of membrane are tested which are having different effective
surface area and membrane thickness. Figure 5.22 shows the samples tested for the
measurement of water flux. The value of effective area and flux is summarized in the
table 5.4.
55

Sample 1 Sample 2 Sample 3

Figure 5.22 Membrane Samples Tested for Water Flux

Table 5.4 Summarized Effective Area and Water Flux


Average thickness 2
Effective Area Flux (L/m - hr)
Sample 2 of membrane 2
(mm ) (mm) @ 10 kg/cm

Sample 1 740.05 0.12 mm 3378.16

Sample 2 1045.2 0.15 mm 1103.94

Sample 3 532.6 0.18 mm 563.9


6. RESULT AND DISCUSSION

The machining of membrane on WEDM is carried on aluminium square bar of


width 1.25 inch and round bar of diameter 1.25 inch using brass wire of 250 µm
diameter. After many trails of machining the desired thickness of slicing is
determined. This thickness and other input parameters are varied to obtained different
types of membrane. The various characteristics of membrane are studied and
following results are obtained regarding the characteristics of membrane.

6.1. CONTACT ANGLE

The information that is gathered from contact angle analysis may be used to
calculate specific surface energy properties for detailed interfacial analyses, as well as
for qualitatively assessing the wettability, or hydrophobicity/hydrophilicity, of a
membrane surface. The contact angle is measured using sessile drop method. The
value of the contact angle obtained from that method is

Equilibrium Contact angle (θ) = 43.61º

The value of contact angle is 43.61º which is less than 90º, hence the water
wets the membrane surface and it can penetrate easily through the pores of the
membrane. This membrane can be used for the water filtration, because for the
membrane filtration the liquid must wet the membrane surface.

6.2. SURFACE MORPHOLOGY

The surface morphology of a membrane deals with the measurement of


surface roughness of the membrane surface. The surface roughness of two membranes
samples are tested in the direction parallel to the motion of the wire as well as in the
perpendicular of the wire. The average roughness value of both the membrane surface
is shown in the table 6.1.
57

Table 6.1 Average roughness of Membrane

Average Roughness
Average Roughness
Sample (In Perpendicular Direction to
(In Parallel Direction to wire)
Wire)
Sample 1 4.343 µm 2.984 µm
Sample 2 5.695 µm 9.962 µm

There is a relation between average roughness and water flux. As Ra


decreased, flux decreased and rejection increased. Here Sample 1is having lesser Ra
value as compared to that of sample 2. Hence, the flux sample 2 is slightly higher than
that of sample 1.

6.3. POROSITY OF MEMBRANE


The porosity of the membrane is measured using fluid re-saturation method in
which the two membrane samples are immersed in the turpentine solution and weight
of both samples are measured before and after immersion in liquid to calculate the
porosity. The value of porosity of both membranes is shown in table 6.2.

Table 6.2 Porosity of membrane

Sample Porosity
Sample 1 9.63 %
Sample 2 8.33%

The porosity of Sample 1 is slightly higher than that of sample 2. Hence for
the more porosity of membrane sample 1 is preferred.

6.4. PORE SIZE AND PORE SIZE DISTRIBUTION


The pore size and pore distribution is measured using Scanning Electron
Microscope (SEM). The measurement of the pore size and pore size distribution is
done on the two membrane samples. The minimum / maximum and the average pore
size are shown in table 6.3 for both membrane samples.
58

Table 6.3 Average pore size

Minimum pore Maximum pore Average pore


Sample
diameter (µm) diameter (µm) diameter (µm)
Sample 1 1.82 µm 6.18 µm 3.55 µm
Sample 2 1.84 µm 7.44 µm 5.35 µm

The pore size distribution of both the membrane sample is shown in figure
5.17 and 5.18 respectively. It is observed that the average pore size of the membrane
sample 1 is slightly smaller than that of membrane sample 2. In the pore size
distribution the maximum numbers of pores size are lie in between range of 2 – 3 µm
for membrane sample 1, whereas for membrane sample 2, the maximum pores size
are lie between ranges of 1.5 – 2.5 µm. But the pores density is more in sample 1
(Figure 5.11 a & b) as compared to that of sample 2 (Figure 5.11 c & d).

The membrane sample 1 is having a smaller average pore size as compared to


that of sample 2. Moreover, sample 1 has also more pore density as compared to that
of membrane sample 2. Hence for the more pore density and smaller pore size
membrane sample 1 is preferred.

6.5. PERMEABILITY AND FLUX


Permeability of membrane gives rate at which the fluid can be filtered through
the membrane. This is called as the flux of the membrane. The permeability of the
membrane samples is measured using a dead end filtration apparatus shown in figure
5.19.

Three different types of membrane samples are taken for the determination of
the water flux which is having different effective area and thickness as shown in
figure 5.22. The comparative result of water flux of the three membrane samples and
some other polymeric membrane is shown in table 6.4.
59

Table 6.4 Comparison of water flux

Flux (lit/m2 - hr.)


Sample
@ 10 kg/cm2

Sample 1 3378.16

Sample 2 1103.94

Sample 3 563.9

PVDF Membrane 158.83

PES Membrane 109.11

The metal membrane developed from wire-EDM machining is having much


more higher water flux as compared to polymeric membrane like PVDF and PES.

4000
3500
Water flux (L/m2-h)

3000
2500
2000
1500
1000
500
0
0.1 0.15 0.2
Thickness of membrane (mm)

Figure 6.1 Comparison of water flux

It is also observed that as the thickness of the metal membrane increases the
water flux is decreases gradually. Figure 6.1 shows the variation of the water flux
depending on the thickness of metal membrane.
60

6.6. APPLICATION OF MEMBRANE


The metal membrane developed from WEDM machining is having an average
pore size in between 2 – 7 µm. The water flux is also very high of this metal
membrane as compared to polymeric membrane.

Application of the membrane is basically depends on the pore size of the


membrane. Based on the pore size of the membrane one can decide that which
particles permitted to pass through membrane and which particles get rejected by the
membrane. The pore size of the membrane is lie between ranges of 2 – 7 µm which
comes under the micro-filtration in the pressure driven membrane system (Figure
6.2). In pressure driven membrane system external air pressure is applied to drive the
fluid through membrane. The micro-filtration spectrum is lie between pore size of 0.1
- 10 µm and pressure range of 700 – 1500 KPa. The metal membrane developed from
WEDM can be used for micro-filtration of water with higher flux. The particles which
can be removed from micro-filtration are shown in figure 6.3.

Figure 6.2 Micro-filtration function


61

Figure 6.3 Micro-filtration spectrum for water

The metal membrane developed through WEDM is also tested for the
rejection of glucose from the aqueous glucose solution. The testing of glucose
rejection is done using dead end filtration apparatus shown in figure 5.19. The 10%
glucose solution is made by adding 20 gm of glucose in 200 ml of distilled water. The
initial and final glucose concentration is measured using refractometer. The
refractometer works on the principle of refractive index. Figure 6.4 shows the
refractometer used for measuring the concentration of the glucose solution. One or
two drop of solution is dropped on test lid and reading in percentage of concentration
is shown on scale when seen from eye piece.

Figure 6.4 Refractometer


62

The percentage of rejection of glucose solution through metal membrane and


other polymeric membrane is shown in table 6.5. The rejection of glucose is slightly
higher in metal membrane as compared to polymeric membrane.

Table 6.5 Glucose Rejection Through Different Membrane

Sr. No. Sample Percentage of Rejection

1. Metal Membrane 3-6%

2. PVDF Membrane 2-4%

3. PES Membrane 2–4%

The metal membrane developed through WEDM is also tested for the
decolourization of contaminated water. For the testing, contaminated water is taken
and filtered using dead end filtration apparatus (Figure 5.19) and the output result is
shown in figure 6.5. The metal membrane decolorized the contaminated water to a
good extent.

Before After

Figure 6.5 Decolourization of contaminated water


7. CONCLUSIONS

7.1. CONCLUSIONS

The novel process of machining of metal membrane on WEDM is developed


and following conclusions are drawn from the various results of membrane
characterisation.

1. The metal membrane is developed through slicing an aluminium


workpiece on WEDM.
2. The porosity of this metal membrane is 8 – 10%.
3. The pore size range of the metal membrane lies between 2 – 6 µm and
it can be used for micro-filtration of water with higher flux as
compared to polymeric membrane.
4. This metal membrane can also be used for the decolourization of the
contaminated water with higher flux as compared to polymeric
membrane.
5. The metal membranes are machined at two different parameters viz.
pulse 3 and pulse 4. Pulse decides the Ton and Toff time of machining.
6. The membrane machined at pulse 3 parameter is comparatively having
lower average surface roughness value than that of membrane
machined at pulse 4 parameter.
7. The water flux of the membrane is affected by the surface roughness
of the membrane. This implies that the water flux of membrane
machined at pulse 3 parameter is comparatively higher than that of
membrane machined at pulse 4 parameter.
8. It is observed that the membrane machined at pulse 3 parameter is
having higher porosity as compared to that of membrane machined at
pulse 4 parameter. Hence the porosity of membrane is affected by the
pulse-on time and pulse-off time of WEDM.
9. The average pore size of the membrane machined at pulse 3 parameter
is smaller than that of membrane machined at pulse 4 parameter.
64

10. Moreover the pore density (i.e. number of pores on membrane) is


higher in membrane developed from pulse 3 parameter.
11. It is also observed that the water flux through membrane decreases
with an increase in the thickness of metal membrane. Hence the water
flux of the metal membrane is inversely proportional to the thickness
of metal membrane. As the thickness increases the water flux through
membrane decreases.

7.2. FUTURE SCOPE

 Research on the proposed methodology can be done much deeper by changing


various other input parameter of WEDM.
 Using the proposed methodology development of membrane of other metal
like stainless steel, die steel, titanium, etc. can be done and various membrane
characterisations can be studied.
 The techniques like ANOVA can be used for finding out the controlling
parameter for the porosity and pore size of the membrane.
 The optimization of the input parameters can be done for the development of
membrane of various other materials.
 The application of membrane developed from WEDM can be studied by
stacking multiple membranes together.
REFERENCES

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Metallic Membrane for Concentration of Glucose Solution. ASM International , 519–
524.

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of Metallic Membrane Using Wire Arc Spraying. Journal of Membrane Science , 541-
548.

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251-266.

D. Bhattacharyya & D. A.Butterfield. (2003). New Insights into Membrane Science


and Technology: Polymeric and Biofunctional Membranes. Amsterdam: Elsevier.

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wafers machined by wire electrical discharge machining. Journal of Materials
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Lee Kew-ho, Kim In-chu & Choi In-hwan. (2008). Method for Preparing Metallic
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APPENDIX A

1) MATLAB Program for Measurement of Contact Angle:

clc;

Image=imread('J:\IMG_20150512_132839.jpg');

imshow(Image);

hold on;

title(char(['Click two points from right to left to define


membrane surface.']));

[x,y]=ginput(2);

m1 = (y(1) - y(2)) / (x(2) - x(1));

a1 = atand(m1);

title(char(['Click two points from bottom to top of drop to


define tangent to drop.']));

[x,y]=ginput(2);

m2 = (y(1) - y(2)) / (x(2) - x(1));

a2 = atand(m2);

title(sprintf('Membrane Inclination = %f deg, Tangent


Inclination = %f deg.', a1, a2));

end
2) MATLAB Program for Measurement of Pore Size and Pore Size Distribution:

clear all;
clc
Image=imread('H:\Project\vivek sem rpt\2_4.jpg');
imshow(Image);
hold on;
calib_dist=10;
title(char(['Click any two points to define the
scale.','Distance between two points is ' num2str(calib_dist)
' microns.']));
[x,y]=ginput(2);
dist_in_p=sqrt((x(2)-x(1))^2+(y(2)-y(1))^2);
calib_factor=calib_dist/dist_in_p;
title(char(['Click two points to find pore diameter.']));
n=2;
freq(1:10) = 0;
while (1)
diameter = 0;
for i=1:n
title(char(['Click two points to define diameter. Run
no.: ' num2str(i)]));
[x,y]=ginput(2);
diameter(i) = sqrt( (x(2)-x(1))^2 + (y(2)-y(1))^2 ) *
calib_factor;
end
diameter(n) = sqrt( (x(2)-x(1))^2 + (y(2)-y(1))^2 ) *
calib_factor
Avgdiameter=sum(diameter)/n
freq(ceil(Avgdiameter))= freq(ceil(Avgdiameter)) + 1

title(char(['Avg thichness is: ' num2str(Avgdiameter) '


microns.']));
end
APPENDIX B
Spark Pulse Timing Chart with Variation in Pulse and Current:
1. Pulse = 1
ton = 5 µsec.
toff = 5 µsec.
Ton = 0.12 msec.

ton toff
Ton Toff

Current Selection Toff (mSec)


0 1.75
1 1.72
2 1.66
3 1.64
4 1.60
5 1.56
6 1.52
7 1.48
8 1.46
9 1.38
10 1.32
11 1.361
12 1.28
13 1.24
14 1.20
15 1.16
16 1.10
17 1.08
18 1.04
19 1.00
20 0.96
21 0.84
22 0.83
23 0.82
24 0.80
25 0.78
26 0.73
27 0.70
28 0.66
29 0.63
30 0.56
31 0.52
32 0.49
2. Pulse = 2
ton = 16 µsec.
toff = 16 µsec.
Ton = 0.16 msec.

ton toff
Ton Toff

Current Selection Toff (mSec)


0 1.50
1 1.48
2 1.44
3 1.40
4 1.36
5 1.32
6 1.30
7 1.26
8 1.22
9 1.16
10 1.12
11 1.08
12 1.04
13 1.00
14 0.98
15 0.96
16 0.84
17 0.78
18 0.82
19 0.78
20 0.74
21 0.70
22 0.66
23 0.64
24 0.58
25 0.54
26 0.50
27 0.48
28 0.40
29 0.31
30 0.36
31 0.32
32 0.28
3. Pulse = 3
ton = 18 µsec.
toff = 18 µsec.
Ton = 0.15 msec.

ton toff
Ton Toff

Current Selection Toff (mSec)


0 1.48
1 1.44
2 1.40
3 1.36
4 1.34
5 1.30
6 1.26
7 1.22
8 1.18
9 1.14
10 1.10
11 1.06
12 1.00
13 0.98
14 0.94
15 0.84
16 0.80
17 0.84
18 0.76
19 0.74
20 0.70
21 0.64
22 0.60
23 0.56
24 0.54
25 0.52
26 0.48
27 0.42
28 0.40
29 0.29
30 0.23
31 0.27
32 0.235
4. Pulse = 4
Ton = 0.08 msec

Toff
Ton

Current Selection Toff (mSec)


0 1.54
1 1.50
2 1.48
3 1.42
4 1.40
5 1.36
6 1.32
7 1.28
8 1.24
9 1.20
10 1.16
11 1.12
12 1.08
13 1.04
14 1.00
15 0.96
16 0.92
17 0.88
18 0.84
19 0.80
20 0.76
21 0.72
22 0.68
23 0.66
24 0.62
25 0.56
26 0.54
27 0.50
28 0.46
29 0.42
30 0.40
31 0.36
32 0.32

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