DESIGN AND FABRICTION OF 3D BALL MILLING ATTACHMENT

A Project Report
Submitted to
SRI VENKATESWARA COLLEGE OF ENGINEERING & TECHNOLOGY
(AUTONOMOUS)
(Affiliated to JNTUA, Ananthapuramu)
In partial fulfillment of the
Requirements for the award of the Degree of
BACHELOR OF TECHNOLOGY
IN
MECHANICAL ENGINEERING
During the Academic Year 2018-19
By
Y. Rajesh 15781A03G7
G. Dileep Kumar Reddy 16785A0319
Y. Vinay Kumar Reddy 15781A03G4
Y. Rohith Roy 15781A03G5
P. Vikesh 15781A03G3
Y. Tarun Kumar 15781A03G6
Under the Guidance of

Dr . A. MAHAMANI,M.E, Ph.D.

DEPARTMENT OF MECHANICAL ENGINEERING

SRI VENKATESWARA COLLEGE OF ENGINEERING & TECHNOLOGY
(AUTONOMOUS)
(Affiliated to JNTUA, Ananthapuramu & Approved by A.I.C.T.E. New Delhi)
(Accredited by N.B.A., New Delhi & NAAC, Bangalore)
R.V.S. Nagar, Chittoor-517127
ANDHRAPRADESH
2019
 SRI VENKATESWARA COLLEGE OF ENGINEERING & TECHNOLOGY
(AUTONOMOUS)
R.V.S.NAGAR, CHITTOOR-517127
DEPARTMENT OF MECHANICAL ENGINEERING

CERTIFICATE
This is to certify that the Project report entitled ‟DESIGN AND FABRICTION OF

3D BALL MILLING ATTACHMENT” is a bonafide work carried out by

Y. Rajesh 15781A03G7
G. Dileep Kumar Reddy 16785A0319
Y. Vinay Kumar Reddy 15781A03G4
Y. Rohith Roy 15781A03G5
P. Vikesh 15781A03G3
Y. Tarun Kumar 15781A03G6
during the academic year 2018-19 is submitted to the faculty of Mechanical Engineering, in
partial fulfillment of the requirements for the award of degree of BACHELOR OF
TECHNOLOGY in MECHANICAL ENGINEERING from Sri Venkateswara College of
Engineering & Technology (Autonomous), Affiliated to Jawaharlal Nehru Technological
University Anantapur, Ananthapuramu.

Signature of the Supervisor Signature of the Head of the Department

Dr . A. MAHAMANI, M.E, Ph.D., Dr . A. MAHAMANI, M.E, Ph.D.,
Professor & HOD Professor & HOD
Department of Mechanical Engineering, Department of Mechanical Engineering,
SVCET, SVCET,
Chittoor. Chittoor.

External Viva-Voce held on:____________

Signature of the Internal Examiner Signature of the External Examiner

i
 SRI VENKATESWARA COLLEGE OF ENGINEERING & TECHNOLOGY
(AUTONOMOUS)
R.V.S. NAGAR, CHITTOOR-517127
DEPARTMENT OF MECHANICAL ENGINEERING

DECLARATION

We, Y. Rajesh 15781A03G7

G. Dileep Kumar Reddy 16785A0319
Y. Vinay Kumar Reddy 15781A03G4
Y. Rohith Roy 15781A03G5
P. Vikesh 15781A03G3
Y. Tarun Kumar 15781A03G6
hereby declare that the Project report entitled “DESIGN AND FABRICTION OF 3D
BALL MILLING ATTACHMENT” done by under the guidance of Dr . A.
MAHAMANI, M.E, Ph.D., Sri Venkateswara College of Engineering & Technology,
Chittoor is submitted in partial fulfillment of the requirements for the award of the degree of
BACHELOR OF TECHNOLOGY in MECHANICAL ENGINEERING.

This is a record of bonafide work carried out by us and the results embodied in this project
have not been reproduced or copied from any source. The results embodied in this project
report have not been submitted to any other university or institute for the award of any other
degree or diploma.
Signature of the student
Y. Rajesh 15781A03G7
G. Dileep Kumar Reddy 16785A0319
Y. Vinay Kumar Reddy 15781A03G4
Y. Rohith Roy 15781A03G5
P. Vikesh 15781A03G3
Y. Tarun Kumar 15781A03G6

ii
 ACKNOWLEDGMENT

The satisfaction and euphoria that accompany the successful completion of any task
would be incomplete without the mention of people who made it possible, whose constant
guidance and encouragement crowned our efforts with success. It is a pleasant aspect that
we have now the opportunity to express our gratitude for all of them.
The first person we would like to thank is our guide Dr . A. MAHAMANI, M.E, Ph.D.,
Professor in the Department of Mechanical Engineering, SVCET, Chittoor. His wide
knowledge and logical way of thinking have made a deep impression on us. His
understanding, encouragement and personal guidance have provided the basis for this thesis.
He is a source of inspiration for innovative ideas and his kind support is well known to all
his students and colleagues.
We wish to thank Dr . A. MAHAMANI, M.E, Ph.D., Professor and Head of the
Department of Mechanical Engineering, SVCET, Chittoor, who has extended his support for
the success of this project.
We wish to thank Prof. Dr. C. VIJAYA BHASKAR REDDY, M.I.S.T.E., Ph.D., professor
and principal of SVCET, Chittoor, who has extended his support for the success of this
project.
We would also like to express our sincere gratitude to Mr. S. Jawahar, M. Tech, M.B.A.,
Assistant Professor of the Department of Mechanical Engineering for his valuable support.
Last but not least, we thank our faculty, family members and friends for their moral
support and constant encouragement. We are very much thankful to one and all for the
successful completion of the project.

Project Associates:
Y. Rajesh 15781A03G7
G. Dileep Kumar Reddy 16785A0319
Y. Vinay Kumar Reddy 15781A03G4
Y. Rohith Roy 15781A03G5
P. Vikesh 15781A03G3
Y. Tarun Kumar 15781A03G6

iii
 ABSTRACT

High Energy Ball Milling is the process of mechanical breakdown of solids into smaller
particles without changing their state of aggregation. It may be used to create particles of a
certain size and shape. It works on the principle of impact and attrition i.e., size reduction is
done by impact as the balls drop from the near the top of the shell. Besides material synthesis,
high-energy ball milling is a way of modifying the conditions in which chemical reactions
usually take place either by changing the reactivity of as milled solids or by inducing
chemical reactions during milling. Its function is used to grind and blend materials for use
in mineral dressing process, paints, pyrotechnics, ceramics and selective laser sintering. It is
generally used for mixing and conversion purpose. It can pulverize the solid state particles
into a small size particles. Its main advantage is to produce very fine powders (particle size
less than or equal to 10 microns).
In the previous attempts or trails , they are unable to attach the ball milling equipment to
the radial drilling machine and also they did not run the machine with three relative motions
simultaneously . This drawback made us to do this attempt by using three motions in-order
to achieve the final result.
The main aim of the proposed project is to design and fabricate the 3D ball milling
attachment with three relative moments. One rotary motion is given to the container with the
help of motor which rotates in clockwise direction and the other rotary and linear motions
are given to the stirrer which rotates in anticlockwise direction.
In-order to resolve the problem the container and the stirrer is operated with a constant
speed of 856.5 rpm and 824.5 rpm. The feed rate i.e., 0.12 cm/sec which is given to the stirrer
must be constant throughout the process.
At the end of the project we have founded the actual size of the particle after operating
the 3D ball mill attachment under different time of milling which is to be measured and
reported and also compared the size of different types of materials.

Keywords: SOLIDWORKS software, container, stirrer and motor

iv
 CONTENTS

CERTIFICATE i
DECLARATION ii
ACKNOWLEDGEMENT iii
ABSTRACT iv
CONTENTS v
LIST OF FIGURES viii
LIST OF TABLES xi
LIST OF GRAPHS xii
ABBREVIATIONS xiii

CHAPTER 1: INTRODUCTION 1-12

1.1. Definition of HEBM or MA 1
1.2. Mechanical alloying &milling 1
1.3. Historical perspective 3
1.4. 2D & 3D ball mill 6
1.5. Different types of Ball mills 7
1.5.1. Planetary mills 7
1.5.2. Attritors or Stirred ball mills 9
1.5.3. SPEX shaker mills 10
1.6. Safety Hazards 11
1.7. Applications of Ball mill 12
1.8. Motivation 12

CHAPTER 2: LITERATURE SURVEY 13-19

2.1. Mechanical Milling 13
2.2. 1D Nanomaterials Synthesized using
HEBM & Annealing process 14
2.3. Past working review 15

CHAPTER 3: METHODOLOGY 20-22

3.1. Explanation and objective of 3D ball milling attachment 20
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 3.2. Flow chart of overall progress 20
3.3. Demands of successful processing and economical production 21
CHAPTER 4: MODELLING 23-32
4.1. Introduction 23
4.2. Details and modelling of 2D Views of all components 24
4.3. Assembly and Animation of 3D ball mill using
SOLIDWORKS Software 29
4.4. Assembly in 2D view & Different motions shown in the model 31

CHAPTER 5: DESIGN 33-37

5.1. Introduction 33
5.2. Design calculations 33
5.2.1. Selection of Container 33
5.2.2. Selection of Motor 34
5.2.3. Selection of Motor Shaft 35
5.2.4. Selection of Stirrer 36

CHAPTER 6: FABRICATION 38-42

6.1. Introduction 38
6.2. Specifications of all the components in detailed manner 38
6.3. Fabrication of all the components 41

CHAPTER 7: ATTACHMENT TO THE RADIAL DRILLING MACHINE 43-44

7.1. Introduction 43
7.2. Experimental setup 43
7.3. Working 44

CHAPTER 8: RESULT AND DISCUSSION 45-72

8.1. Materials chosen for Testing purpose 45
8.1.1. Precautions for Testing 47
8.2. Test-1: Size reduction of Egg Shells 47
8.3. Test-1: Results 55
8.4. Test-2: Size reduction of aluminium oxide 56
8.5. Test-2: Results 62
8.6. Test-3: Size reduction of aluminium powder 63
8.7. Test-4: Results 70
vi
CHAPTER 9: CONCLUSIONS 73
CHAPTER 10: FUTURE SCOPE 74

REFERENCES 75

vii
 List of the Figures
S.no. Fig No: Description Page No:
1. Fig No 1.1 Mechanical alloying 2
2. Fig No 1.2 2D Ball Milling 6
3. Fig No 1.3 3D Ball Milling 7
4. Fig No 1.4 Planetary Ball Mill 8
5. Fig No 1.5 Working Principle of Planetary Ball Mill 8
6. Fig No 1.6 Attritors Ball Mill 9
7. Fig No 1.7 Working Principle of Attritors Ball Mill 10
8. Fig No 1.8 Shaker Ball Mill 10
9. Fig No 1.9 Working Principle of Shaker Ball Mill 11
10. Fig No 4.1 Impeller 24
11. Fig No 4.2 Impeller in 2D view 25
12. Fig No 4.3 Container 26
13. Fig No 4.4 Container in 2D view 26
14. Fig No 4.5 Motor shaft 27
15. Fig No 4.6 Motor shaft in 2D view 27
16. Fig No 4.7 Supporting column along with motor part 28
17. Fig No 4.8 Supporting column along with motor part in 2D view 29
18. Fig No 4.9 Assembly of 3D ball milling 30
19. FigNo 4.10 Assembly in 2D view 31
20. FigNo 4.11 Different motions 32
21. Fig No 5.1 Container Volume 34
22. Fig No 5.2 Stirrer 36
23. Fig No 6.1 Equipment stand along with motor 41
24. Fig No 6.2 Container attached to a motor shaft 41
25. Fig No 6.3 Fabricated 3D ball milling system 42
26. Fig No 7.1 Attachment to the radial drilling machine 43

viii
27. Fig No 8.1 Egg shells 45
28. Fig No 8.2 Egg shells were washed several times in deionised 45
water
29. Fig No 8.3 Al O powder 46
30. Fig No 8.4 Al powder 47
31. Fig No 8.5 Egg shells after clean wash 48
32. Fig No 8.6 Egg shells filled in container 48
33. Fig No 8.7 Electronic digital weighting scale 48
34. Fig No 8.8 Before milling test report of egg shells 49
35. Fig No 8.9 Before milling egg shell sample 49
36. FigNo 8.10 Egg shell powder filled in container 50
37. FigNo 8.11 Egg shells after 30 minutes 50
38. FigNo 8.12 After 30 minutes milling test report of egg shells 51
39. FigNo 8.13 Egg shells after 1hour 51
40. FigNo 8.14 After 1hour milling test report of egg shells 52
41. FigNo 8.15 Egg shells after 2hours 53
42. FigNo 8.16 After 2hours milling test report of egg shells 53
43. FigNo 8.17 Egg shells after 3hours 54
44. FigNo 8.18 After 3hours milling test report of egg shells 55
45. FigNo 8.19 Before milling Al O powder sample 56
46. FigNo 8.20 Before milling test report of Al O powder 57
47. FigNo 8.21 Al O powder filled in container 57
48 FigNo 8.22 Al O powder after 30minutes 58
49. FigNo 8.23 After 30 minutes milling test report of Al O powder 58
50. FigNo 8.24 Al O powder after 1 hour 59
51. FigNo 8.25 After 1hour milling test report of Al O powder 59
52. FigNo 8.26 Al O powder after 2 hours 60
53. FigNo 8.27 After 2 hours milling test report of Al O powder 60
54. FigNo 8.28 Al O powder after 3hours 61

ix
55. FigNo 8.29 After 3 hours milling test report of Al O powder 62
56. FigNo 8.30 Before milling Al powder sample 63
57. FigNo 8.31 Before milling test report of Al powder 64
58. FigNo 8.32 Al powder filled in container 65
59. FigNo 8.33 Al powder after 30 minutes 65
60. FigNo 8.34 After 30 minutes milling test report of Al powder 66
61. FigNo 8.35 Al powder after 1 hour 66
62. FigNo 8.36 After 1 hour milling test report of Al powder 67
63. FigNo 8.37 Al powder after 2 hours 67
64. FigNo 8.38 After 2 hours milling test report of Al powder 68
65. FigNo 8.39 Al powder after 3 hours 69
66. FigNo 8.40 After 3 hours milling test report of Al powder 69

x
 List of the Tables

S.no. Table no: Description Page No:

1. Table 1.1 Attributes of mechanical alloying 5
2. Table 1.2 Important milestones in the development of 5
mechanical alloying
3. Table 6.1 Specifications of all the components 39
4. Table 8.1 Egg shell size reduction data table 55
5. Table 8.2 Al O powder size reduction data table 62
6. Table 8.3 Al powder size reduction data table 70
7. Table 8.4 Comparing particle size reduction of all the 71
materials
8. Table 8.5 Comparing size reduction of all the materials 72

xi
 List of the Graphs

S.no. Graph.no Title of the Graph Page No:

1. Graph 8.1 Size reduction of Egg shells 56
2. Graph 8.2 Size reduction of Al O powder 63
3. Graph 8.3 Size reduction of Al powder 70
4. Graph 8.4 Comparing particle size reduction of all the 71
materials

xii
 Abbreviations

Short From Full Form

HEBM High Energy Ball Milling
MA Mechanical Alloying
bcc body centered cubic
fcc face centered cubic
hcp hexagonal close packed
INCO International Nickel Company
TD Thoria Dispersed
ODS Oxide Dispersion Strengthened
ISMANAM International Symposia on Mechanically Alloyed,
Metastable and Non-crystalline Materials
i.e., that is
1D One Dimensional
2D Two Dimensional
3D Three Dimensional
CNTs Carbon Nano-Tubes
CVD Chemical Vapour Deposition
SWNTs Single-Walled Nano-Tube
MWNTs Multi-Walled Nano-Tubes
hrs hours
min minutes
BPR Ball to Powder Ratio
RPM Revolution Per Minute
nm nanometer
emu/g electromagnetic unit per gram
µm micrometer
Wt% Weight percentage
mm millimeter
cm centimeter
ANSI American National Standards Institute
ISO International Organization for Standardization
GIS German Institute for Standardization
GOST Euro-ASIAN Council for Standard
JIS Japan Industrial Standard
BSI British Standard Institution
∅ diameter
V Container Volume
L Container Length
d container diameter
m mass
kg⁄m kilogram per cubic meter
kg kilogram
T Torque
lb-ft pound-feet
N-m Newton meter
A Amperes
v volts
xiii
 P Power
w Watts
D Shaft Diameter
N Critical speed
N 75% of critical speed
hp horse power
Al O Aluminium Oxide
Al Aluminium powder
cm/sec centimeter per second
gm grams
etc., etcetera
Zr-Ni Zirconium-Nickel
C Carbon
BN Boron Nitride
Zn Zinc
Sic Silicon carbide
Fe-Co-Ni-B-Si-Nb Iron-Cobalt-Nickel-Boron-Silicon-Niobium
Zn-O Zine-Oxide
WC Water Closed
FexN Iron-Nitrogen
Fe-Ni Iron-Nickel
Fe-Ni-B-Mo Iron-Nickel-Boron-Molybdenum
Ni-Fe Nickel-Iron
SEM Scanning Electron Microscope
Co-Ti Cobalt-Titanium
Fe Iron
Fe-Co Iron-Cobalt
Ms Maximum saturation Magnetization
H-c minimum coercivity
TEM Transmission Electron Microscope

xiv
CHAPTER 1
 INTRODUCTION

1.1. Definition of HEBM or MA

High Energy Ball Milling or Mechanical Alloying is the process of mechanical

breakdown of solids into smaller particles without changing their state of aggregation. It may
be used to create particles of a certain size and shape. It works on the principle of impact and
attrition i.e., size reduction is done by impact as balls drop from the near the top of the shell.
It is used to produce very fine powders. It mainly consists of a container which is attached
with a motor , Impeller , Balls to be milled and a supporting column or a base. Generally ball
mill is a cylindrical device which contains a rotary motion and this motion is used to grind
and blend raw materials.

1.2. Mechanical alloying & milling

Mechanical alloying is a type of grinder used to grind and blend many materials into fine
powder. It has been used to produce nanocrystal line materials. Until now nanocrystal line
metals with a grain size from 5 to 22nm have been obtained by ball milling for fcc, bcc and
hcp. A compromise between good interparticle or inter-crystalline bonding and minimum
porosity on the one hand and a minimized coarsening of the grain structure on the other has
to be made. It is therefore important to investigate the thermal stability and grain growth
behavior of nanocrystalline materials. It is used to grind many kinds of raw materials so the
basic properties of the milling bodies are their mass and size, ware rate, influence on the
particle breakage rate and energy efficiency of the grinding process. Nearly all materials can
be processed, including metals, organics and pharmaceutical, as well as composites or low-
dimensional structures. Ceramic materials can be produced either indirectly or directly via
Mechanical alloying. There are two ways of grinding: first the dry way and the second is the
wet way. There is another type of Mechanical alloying called High Energy Ball Milling.
High Energy Ball Milling is smaller than 2D ball milling and mainly used in the laboratories
for grinding sample material like ceramic or other raw material to a very small size or
powder. Usually High Energy Ball Milling consists at least one grinding jar and must be
operated in a closed system. For the more efficient grinding there is some specific operating
speed that needed. When it is controlled by the speed, the load nearest the wall of the
cylinders will break and it quickly followed by other particle in the top curves and form a
sliding stream containing several layers of balls separated by material of varying thickness.
There is some action caused by the turning of individual balls or pebbles and secondary
1
movements having the nature of rubbing or rolling contacts occur inside the cylinder.
Moreover, in this type of mill, it has been considered as high energy. It is because, the milling
stock and balls come off the wall and the effective centrifugal force reaches up to twenty
times gravitational acceleration as shown in Fig 1.1 [1].

Fig 1.1 Mechanical alloying

In both rotation–revolution relationships, the specific impact energy increases with an

increase in the rotation-to-revolution speed ratio in the initial stage and then falls around the
critical speed ratio. The highest value in the specific impact energy of balls during milling
can be achieved effectively around this critical speed. Anyhow, the rate of breakage decrease
as fines accumulate in the bed and applies to all sizes in mill. As the amount of powder is
increased, the collision spaces between the balls are filled and higher rates of breakage are
obtained. Besides that, the maximum grinding rate shifts toward higher rotational speed
range as the ball size becomes large. The particle size distribution width was lowered by
using larger grinding balls in dry condition. The optimum milling time depends on the type
of mill, size of the grinding medium, temperature of milling, ball-to-powder ratio. The
optimum ball size distribution is thus determined by the amount and combination of grinding
balls of different diameters in the make-up charge. Regarding the speed of the jar which
cause cascading effect, when rotation speed of milling jar without lifter bar is below 75% of
critical revolutions per minute (rpm), balls slide in the jar. As rotation speed of milling jar
increases up to 93% and 140%, the mode of balls motion changes to cascading and
cataracting type, respectively. By setting even one lifter bar in the jar, balls move as
cascading mode and cataracting mode at 37% and 56% of critical rpm, respectively. As

2
number of lifter bars increases, the necessary rotation speeds of milling jar for cascading
mode and cataracting mode decreases drastically.

1.3. Historical perspective

Mechanical alloying (MA) is a powder processing technique that allows production of

homogeneous materials starting from blended elemental powder mixtures. John Benjamin
and his colleagues at the Paul D. Merica Research Laboratory of the International Nickel
Company (INCO) developed the process around 1966. The technique was the result of a long
search to produce a nickel-base superalloy, for gas turbine applications, that was expected to
combine the high-temperature strength of oxide dispersion and the intermediate-temperature
strength of gamma-prime precipitate. The required corrosion and oxidation resistance was
also included in the alloy by suitable alloying additions. Benjamin has summarized the
historic origins of the process and the background work that led to the development of the
present process. In the early 1960s, INCO had developed a process for manufacturing
graphitic aluminum alloys by injecting nickel-coated graphite particles into a molten
aluminum bath by argon sparging. A modification of the same technique was tried to
inoculate nickel-based alloys with a dispersion of nickel-coated, fine refractory oxide
particles. The purpose of nickel coating was to render the normally unwetted oxide particles
wettable by a nickel-chromium alloy. The early experiments used metal-coated zirconium
oxide and this did not yield the desired result. A thorough analysis revealed that the reason
for the failure of the experiment was because the vendor had supplied powder that was
zirconia-coated nickel rather than nickel-coated zirconia. Since the reaction of aluminum
with nickel produces a strong exothermic reaction, the heat generated cleansed the surface
of the graphite and lowered the surface energy. On this basis, it was assumed that coating of
the refractory oxide with aluminum would be ideal to produce the exothermic reaction. This
also did not prove successful. When some other attempts also failed to yield the desired
result, out of desperation, attention was turned to the ball milling process that had been used
earlier to coat hard phases such as tungsten carbide with a soft phase such as cobalt or nickel.
It was also known that metal powder particles could be fractured by subjecting them to heavy
plastic deformation. Use of special chemicals could be employed to produce finer particles
by preventing cold welding, suggesting that at some stage cold welding could be as rapid as
fracturing. The reactivity of the element also had to be considered. Taking all these factors
into consideration, Benjamin decided to produce composite powder particles by:
 using a high energy mill to favour plastic deformation required for cold welding and
reduce the process times,
3
  using a mixture of elemental and master alloy powders (the latter to reduce the
activity of the element, since it is known that the activity in an alloy or a compound
could be orders of magnitude less than in a pure metal),
 eliminating the use of surface-active agents which would produce fine pyrophoric
powder as well as contaminate the powder, and
 relying on a constant interplay between welding and fracturing to yield a powder
with a refined internal structure, typical of very fine powders normally produced,
but having an overall particle size which was relatively coarse, and therefore stable.

This method of making the composite powders reproduced the properties of TD (thoria
dispersed) nickel synthesized by a completely different process. Encouraged by this success,
experiments were conducted to produce a nickel-chromium- aluminium-titanium alloy
containing a thoria dispersoid. This was also successfully produced, first in a small high-
speed shaker mill and later in a one-gallon stirred ball mill, starting the birth of MA as a
method to produce oxide dispersion strengthened (ODS) alloys on an industrial scale.
This process, as developed by Benjamin, was referred to as ``milling/ mixing'', but Mr.
Ewan C. MacQueen, a patent attorney for INCO coined the term mechanical alloying to
describe the process in the first patent application, and this term has now come to stay in the
literature.
Mechanical alloying is normally a dry, high-energy ball milling technique and has been
employed to produce a variety of commercially useful and scientifically interesting
materials. The formation of an amorphous phase by mechanical grinding of an Y-Co
intermetallic compound in 1981 and in the Ni-Nb system by ball milling of blended
elemental powder mixtures in 1983 brought about the recognition that MA is a potential non-
equilibrium processing technique. Beginning from the mid-1980s, a number of
investigations have been carried out to synthesize a variety of stable and metastable phases
including supersaturated solid solutions, crystalline and quasicrystalline intermediate phases,
and amorphous alloys. Additionally, it has been recognized that powder mixtures can be
mechanically activated to induce chemical reactions, i.e., mechanochemical reactions at
room temperature or at least at much lower temperatures than normally required to produce
pure metals, nanocomposites, and a variety of commercially useful materials. Efforts were
also under way since the early 1990s to understand the process fundamentals of MA through
modeling studies . Because of all these special attributes, this simple, but effective,
processing technique has been applied to metals, ceramics, polymers, and composite
materials. The attributes of mechanical alloying are listed in Table 1.1. and some important
milestones in the development of the field are presented in Table 1.2. The technique of MA
4
to synthesize novel alloy phases and to produce oxide dispersion strengthened materials has
attracted the attention of a large number of researchers during the past 10 years or so. A
number of stand-alone conferences have been organized on this topic. Mechanical alloying
has become an integral part of the triennial international conferences on Rapidly Quenched
Metals (redesignated now as Rapidly Quenched and Metastable Materials) since RQ VI held
in Montreal, Canada in 1987. Additionally, the proceedings of the International Symposia
on Mechanically Alloyed, Metastable, and Nanocrystalline Materials (ISMANAM) contain
many papers on mechanical alloying and these are regularly published in ``Materials Science
Forum'' by Trans Tech Publications, Zurich, Switzerland. A book on ``Mechanical Alloying''
has been recently published. The literature on mechanical alloying and milling available
between 1970 and 1994 has been collected together in an annotated bibliography published
in 1995. A short-lived journal entitled ``International Journal of Mechanochemistry and
Mechanical Alloying'' was started in 1994. Several reviews have also appeared over the past
ten years with emphasis on a particular topic, but the present article is an attempt to review
all aspects of MA in a comprehensive and critical manner at one place and present the
potential and limitations of this technique as a non-equilibrium processing tool [2].

Table 1.1. Attributes of mechanical alloying

Production of fine dispersion of second phase (usually oxide) particles

Extension of solid solubility limits Refinement of grain sizes down to nanometer range
Synthesis of novel crystalline and quasicrystalline phases Development of amorphous
(glassy) phases
Disordering of ordered intermetallics
Possibility of alloying of difficult to alloy elements
Inducement of chemical (displacement) reactions at low temperatures
Scaleable process

Table 1.2. Important milestones in the development of mechanical alloying

1966 Development of ODS nickel-base alloys

1981 Amorphization of intermetallics
1982 Disordering of ordered compounds
1983 Amorphization of blended elemental powder mixtures
1987/88 Synthesis of nanocrystalline phases
1989 Occurrence of displacement reactions
1989 Synthesis of quasicrystalline phases

5
1.4. 2D & 3D ball mill

2D Ball Mill

2D ball mill is defined as the mechanical breakdown of larger particles into smaller
particles by using two motions i.e; one rotary motion is given to the vial and the other rotary
motion is given to stirrer. The vial is filled with stainless steel balls about 25% and the
remaining portion is left free & with the help of stirrer the balls which are filled in container
is milled & finally the larger particles are changed to a smaller particles as shown in Fig 1.2
(source from https://goo.gl/images/dn6rJb).

Fig 1.2 2D Ball Milling

3D Ball Mill

The present project is the 3D Ball Mill which uses three relative motions i.e., two rotary
motions and one linear motion. One rotary motion is given to the vial which is connected
with the motor and the other rotary motion is given to the stirrer which is operated by a
drilling machine by assembling it to the machine and the linear motion is also given to the
stirrer with the hand movement in the machine as shown in Fig 1.3.

6
 Fig 1.3 3D Ball Milling

1.5. Different types of Ball mills

Different types of high-energy milling equipment are used to produce mechanically

alloyed/milled powder. They differ in their design, and additional arrangement for cooling,
heating, and so forth.

1.5.1. Planetary mills

Planetary Ball Mill for conducting MA experiments is the ball mill (referred to as
Pulverize) in which a few hundred grams of the powder can be milled at the same time.
These are manufactured by Fritsch. The planetary ball mill owes its name to the planet-like
movement of its vials. These are arranged on a rotating disk, and a special drive mechanism
causes them to rotate around their own axes. The centrifugal force produced by the vials
rotating around their own axes and that produced by the rotating support disk both act on the
vial contents, consisting of the material to be ground the grinding balls. Since the vial and
the supporting disk rotate in opposite direction, the centrifugal forces alternately act in like
and opposite direction as shown in Fig 1.4 (source from http://www.fritsch.com).

7
 Fig 1.4 Planetary Ball Mill

Fig 1.5 Working Principle of Planetary Ball Mill

1.5.2. Attritors or Stirred ball mills

A conventional ball mill consists of a rotating horizontal drum half-filled with small steel
balls. As the drum rotates the balls drop on the metal powder that is being ground; the rate
of grinding increases with the speed of the rotation. At high speed, however, the centrifugal
force acting on the steel balls exceeds the force of gravity, and the balls are pinned to the

8
wall of the drum. At this point the grinding acting stops. An attritor (a ball mill capable of
generating higher energies) consists of a vertical drum containing a series of impellers. The
impellers energize the ball charge, the dry particles are subjected to various forces such as
impact, rotation, tumbling, and shear. This causes powder size reduction because of the
collisions between balls and container wall, and between balls, agitator shaft, and impellers.

Fig 1.6 Attritors Ball Mill

Therefore, micrometer-rang fine powders can be easily produced. Attritors are the mills
in which large quantities of the powder (from few pounds to about 100lb). The velocity of
the grinding medium in the attritors is much lower (about 0.5 m/s) than in the planetary or
SPEX mills, and consequently the energy of milling in the attritors is low. The setup of
attritors ball mill is shown in Fig 1.6(source from https://goo.gl/images/dn6rJb) and it’s
working principle in Fig 1.7 (source from https://goo.gl/images/JGeD75).
The principle of Attritor dry grind processing is achieved by an expanded moving bed of
media. This condition is described as kinematic porosity. The dry particles are subjected to
various forces such as impact, rotational, tumbling, and shear; therefore, micron range fine
powders can be easily achieved. Additionally, combinations of these forces creates a more
spherical particle than other impact-type milling equipment.
The Attritor’s versatility is gained by the ability to operate under a broad range of
conditions.
For example, grinding media type, size, and amount; different machine speeds; variable
loading or feed rate of raw material. In addition to reducing particle size, Attritors also can
create the highest intensity intimate blending of dissimilar materials. Specific chemicals or
9
additives can also be introduced to the mill during the grinding process to achieve the
ultimate dispersing or coating on the dry solid particles.

Fig: 1.7 Working Principle of Attritors Ball Mill

1.5.3. SPEX shaker mills

Fig 1.8 SPEX Shaker Ball Mill

SPEX Shaker mills, such as SPEX mills, as shown in Fig 1.8 (source from
https://goo.gl/images/m32mQK) which mill about 10-20 g of the powder at a time, are most
commonly used for laboratory investigation and for alloy screening purposes. These mills
are manufactured by SPEX CerPrep. The common version of the mill has one vial,
containing the powder sample and grinding balls, secured in the clamp and swung
energetically back and

10
 Fig 1.9 Working Principle of SPEX Shaker Ball Mill

forth several thousand times a minute. The back-and-forth shaking motion is combined with
lateral movements of the ends of the vial, so that the vial appears to be describing a figure of
8 or infinity symbol as it moves. With each swing of the vial the balls impact against the
sample and the end vial, both milling and mixing the sample. Because of the amplitude
(about 50mm) and speed (about 1200 rpm) of the clamp motion, the ban velocities are high
(on the order of 5 m/s) and consequently the force of the ball’s impact is unusually great.
Therefore, these mills can be considered as high-energy variety and its working principle as
shown in Fig 1.9 (source from https://goo.gl/images/zssoQC).

1.6. Safety Hazards

The safety hazards related to the MA process include heat evolution, reaction rates, gas
evolution causing pressure build-up in the milling chamber or ancillary equipment, and
finally explosions. As mentioned earlier, the temperature increases during milling operations
due to energy added via the mechanical system used to drive the mill, and heat generated by
exothermic processes occurring during the milling process. If this temperature exceeds some
critical ‟reaction temperature” for one or more of the components being milled, uncontrolled
reactions can occur and can lead to explosions. This heat generated can also increase the
reaction rates of the system. Gases may also be produced during milling due to the
decomposition of PCAs or due to the reactions between the components. Some of the gases
produced may be flammable and so the potential for fire or explosion exists. Some safety
hazards exist which are related to handling of MA powders. The mechanically alloyed
powders are very fine in size and consequently have a large surface area. Such powders have
an increased tendency toward pyrophoricity. The cleaner and fresh powder surfaces
produced during MA accentuate their sensitivity to pyrophoricity. Special precautions
should also be taken during unloading of the powders after MA. Immediately after MA, the
powders are hot (or at least warm) and therefore the lid should not be immediately opened
11
and the powder exposed to atmosphere. In such an event, the powder may catch fire because
of interaction with the oxygen. This is much more important when dealing with powders like
magnesium[3].

1.7. Applications of Ball mill

 The ball mill is used for grinding materials such as coal , pigments and felspar for
pottery.
 Used for the grinding of explosive materials.

Widely used in production lines for powders such as cement, silicates, refractory material,
fertilizer, glass ceramics, etc. as well as for ore dressing of both ferrous & non-ferrous metals.

1.8. Motivation

In the previous attempts or trails , they are unable to attach the ball milling equipment to
the radial drilling machine and they did not operate the ball milling process with three
relative motions simultaneously and finally they didn’t achieved the required fine size of the
particle within less duration after operating the process with two relative motions by varying
time . This drawback made us to do this attempt by adding another motion to the system and
to achieve the final size of the particle.

In this chapter we have discussed about the introduction of high energy ball milling or
mechanical alloying. The different types of ball mills which are used in the previous
experiments is also clearly explained. In the next chapter we present various works of
different authors done on high energy ball milling.

12
CHAPTER 2
 LITERATURE SURVEY

In the previous chapter we have presented the introduction to high energy ball milling. In
this chapter we are presenting the different works which are done by different authors . We
have studied the work done by different authors in different journals and gathered some
information about how to fabricate a ball mill.
The literature of various techniques explained in a detailed manner are as follows:

2.1. Mechanical Milling

M.H. Enayati et al., In this paper they said that Mechanical Milling (MM) is usually
carried out using a ball mill. A ball mill, (a type of grinder) is a cylindrical device used in
grinding or mixing materials like ceramic raw materials ores, paints and chemicals. Ball
mills rotates around a horizontal axis and the drums of the ball mill are partially filled with
the material to be ground plus the grinding medium. Different materials that are used as
media include ceramic balls, flint pebbles and stainless steel balls. An internal cascading
effect reduces the material to a fine powder. Industrial ball mills generally operate
continuously, by taking the fed at one end and discharging at the other end. Larger to
medium-sized ball mills are mechanically rotated on their axis , but small ones normally
consist of a cylindrical capped container that sits on two drive shafts (pulleys and belts are
used to transmit rotary motion). High-quality ball mills are potentially expensive and can
grind mixture particles to as small as 5nm, enormously increasing surface area and reaction
rates. The grinding works on the principle of critical speed. The critical speed can be
understood as that speed after which the steel balls (which are responsible for the grinding
of particles) start rotating along the direction of the cylindrical device, thus causing no
further grinding [4].

Ball mills are used extensively in the Mechanical alloying process in which they are not
only used for grinding but for cold welding as well with the purpose of producing alloys
from powders.

There are many types of grinding media suitable for use in a ball mill, each material
having its own specific properties and advantages. Common in some applications are
stainless steel balls.

While usually very effective due to their high density and low contamination of the
material being processed, stainless steel balls are unsuitable for some applications, including:

13
  Black powder and other flammable materials require brass, non-sparking lead,
bronze or antimony grinding media.
 Contamination by iron of sensitive substances such as ceramic raw materials. In this
application flint grinding or ceramic media is used. Ceramic media are also very
corrosive resistant materials.

High density alumina media (90-95% alumina) are widely used in ceramic industry to
grind frits, glazes, clay bodies and other ingredients. These are more expansive than silica
or silex media but are more efficient.

2.2. 1D Nanomaterials Synthesized using HEBM & Annealing process

Ying Chen et al., said that One-dimensional (1D) nanomaterials including nanotubes,
nanowires and nanorods have many new properties and functionalities that lead to a large
range of promising applications. Therefore, there is a strong demand for pure carbon
nanotubes (CNTs) in large quantities and low costs, but this remains a major technical
challenge so far. Many synthesis methods have been developed during the last decade. The
popular processes include electric arc discharge, laser ablation, chemical vapor deposition
(CVD), and ball milling–annealing methods. Among them, the ball milling–annealing
method, consisting of a pre-ball milling and a subsequent thermal annealing process, can
produce much larger quantities of nanotubes due to a solid-state process without any vapor
phase and the large milling capability. Both single-walled nanotubes (SWNTs) and multi-
walled nanotubes (MWNTs) have been produced using the ball milling–annealing method.
Low production costs are also expected from the relatively simple milling equipment and
low-temperature annealing process. In addition, the ball milling–annealing method can
produce other nanotubes and nanowires such as boron nitride (BN) nanotubes. It actually
becomes a successful method for the large production of high yield commercial BN
nanotubes. Both nanotube size and structures (cylindrical and bamboo-type) can be
controlled. The ball milling and annealing method has been adopted by many research
groups in synthesis of different nanotubes since it was first reported in 1999. Tang et al.
obtained BN nanotubes and horns from a mixture of B and Ga2O3 after first ball milling for
6 h and subsequent annealing up to 1550 1C in NH3 gas. Bae et al. have produced BN
nanotubes by first ball milling of B powder, followed by annealing in NH3 gas in the
temperature range of 1000–1200 1C. Li et al. have produced TiTe2 nanotubes by annealing
the ball-milled mixture of Ti and Te powders, and they claim that the ball-milling treatment
is essential for the nanotube formation. Multi-walled and open-ended TiSe2 nanotubes are
also synthesized by using the ball milling–annealing method. The above research works
14
demonstrate that the ball-milling technique, which is generally regarded as a traditional
technique with a history of several centuries, could become an important tool in 1D
nanomaterial synthesis. One important reason is that most of the above research works uses
actually a new ball milling technique: high-energy ball milling (HEBM), which is very
different from the traditional ball-milling technique[5].

The major differences between conventional ball milling and the HEBM include:

 the impact energy of HEBM is typically 1000 times higher than the
conventional ball milling energy. The dominant events in the conventional
ball milling are particle fracturing and size reductions, which correspond to,
actually, only the first stage of the HEBM;
 a longer milling time is generally required for HEBM to activate and
complete the structural changes and chemical reactions;
 HEBM requires the controls of milling atmosphere and temperature which
are crucial to create the desired structural changes or chemical reactions.

HEBM can cover most work normally performed by conventional ball milling. Therefore,
conventional ball milling equipment cannot be used directly to conduct any HEBM work
and specially designed ball mills with a higher milling energy are used for HEBM purposes.
The new HEBM technique has produced many new metastable materials which cannot be
synthesized using thermal equilibrium processes in past several decades, for example,
amorphization of ZrNi alloys under a dynamic equilibrium between mechanical driven
disordering or amorphization process and thermal reordering process , mechanical alloying
of nanocrystalline compounds , nanoparticle-reinforced metal nanocomposite, and nano-
porous materials. Controlled reactive ball milling has produced nanosized particles of metal
oxides, nitrides, hydrides and carbides at room temperature. In addition to the direct
synthesis of nanomaterials during the milling process, 1D materials (nanotubes and
nanowires) can be produced by combining the HEBM and controlled thermal annealing
processes. Large-quantity production of nanotubes in C and BN and nanowires in Zn and
Sic has been achieved and related formation mechanisms will be discussed.

2.3. Past working review

W. Pilarczyk of Institute of Engineering Materials and Biomaterials, Poland, have studied

the structure and properties of Fe-Co-Ni-B-Si-Nb alloy prepared by mechanical alloying
method. In this paper the test material was the mixture of iron, cobalt, nickel, boron, silicon,
niobium material with different proportions. The mechanical alloying process was done
15
using high energy SPEX 8000 mill of the shaker type under inert argon atmosphere. The ball
to powder weight ratio is 9:1 and the powder were grounds for 10, 45, 100hrs. The crystallite
size is measured by using Scherrer`s method. The conclusion of this paper was that powder
structure becomes more homogeneous after 100hrs of mechanical alloying with the particle
size in the range of 0.4µm [6].
D.A. Sanchez of Universidad Autonoma de Coahuila, Mexico, have reported that the
material used for experiment was high purity cobalt nitrate hexahydrate, iron nitrate, sodium
hydroxide, citric acid monohydrate and ethylene glycol. In ball milling experiment milling
was performed in a planetary ball mill, the milling time is 4hours at a speed of 300rpm with
ball to powder mass ratio 10:1. After 4hr of ball milling the materials have improved
crystallinity of magnetic phase with increasing temperature the growth of crystalline from
5nm to 26nm has also been reported[7].
A.M. Glushenkov, Department of Electronic Materials Engineering, Research School of
Physical Science and Engineering, Australia have performed reactive ball milling
experiments to produce nanocrystalline Zn-O. The experiment were carried out in oxygen
atmosphere leading to nano-crystalline Zn-O. Initially the powder particle size was 150
microns after 100hrs of milling the powder particles had crystallite size of 10 to 100nm. The
conclusion drawn from this paper is that mechanochemical procedure is simple and
applicable to producing material in large quantities and the oxidation of zinc is a gradual
process in contrast to combustion oxidations of other metals [8].
S.R.Mishra et al., University of Memphis, USA, have studied the magnetic properties of
iron nitride – alumina nanocomposite materials prepared by high-energy ball milling. In this
study milling was carried out in Pulverisette-5 planetary ball mill with WC vials and WC
balls. Starting material used for milling was 99.9% pure 50µm iron nitride powders. The ball
to powder weight ratio (BPR) was 20:1. Milling was conducted at 400 rpm. Powder particles
were milled for 64h. The reduction in the particle size of Fe N leads to a decrease in the
saturation magnetization (62.5 emu/g) and a corresponding increase in the coercivity. The
observed enhancement in coercivity results from a combination of particle size effect,
surface defects, and mechanical stress [9].
The presence of a super paramagnetic component in the Mossbauer spectra and the
decrease in saturation magnetization are related to the grain size. The observed increase in
the isomer shift and rapid decrease in hyperfine field in the highly dispersed magnetic
particles of (FexN)0.2(Al2O3) are compatible with surface defects.
R.V. Ramanujan et al., School of Materials Engineering, Nanyang Technological
University, Singapore, have studied the mechanical alloying of Fe-Ni based nanostructured

16
magnetic materials. The various alloys composition Fe49Ni38B18Mo4 , Fe49Ni46Mo5 and
Fe42Ni40B18 were processed from elemental powders by mechanical alloying of Fritsch
pulverisette 5 planetary ball milling under argon atmosphere from pure elemental powder
iron, nickel, boron and molybdenum. The ball to powder ratio was kept constant at 8:1. The
milling speed was 300rpm for milling times ranging from1to 100h. Initially the raw material
particle size was iron-35µm, nickel150µm, boron-46µm, and molybdenum 3 to 5µm [10].
The grain size of alloy composition of Fe49Ni38B18Mo4 was 6nm; correspondingly alloys
of Fe49Ni46Mo5 and Fe42Ni40B18 yielded particles with grain size in the range of 8 to 20nm.
They have reported that addition of molybdenum and boron have a dramatic effect on the
magnetic properties of mechanically alloyed Fe and Ni based material.

D. Oleksakova et al., Slovakia Germany, have studied the soft magnetic properties of Ni-
Fe compacted powder alloys. In this paper they have reported mechanical milling using high
energy planetary ball mill in hardened steel vials with steel balls. The milling was performed
in the protective argon atmosphere with ball to powder ratio of 6:1 and with a speed of 180
rpm. The conclusions of this paper are that Ni-Fe (81wt% of Ni) form from a single –phase
system and the mechanical milling of Ni-Fe (81wt% of Ni) results in decrease in coercivity
as a function of grain size [11].

H.R. Madhaa Hosseini, have studied preparation of nanocrystalline Fe-Si-Ni soft

magnetic powders by mechanical alloying and it’s on the magnetic properties and
microstructure of these alloys. In this research work the powder mix were ball milled under
argon atmosphere, iron, silicon and nickel with a ball to powder ratio 10:1 and speed
700rpm. The initial grains size was 400nm, after 100 hours of milling the grain size reduced
to 12nm. Detailed characterization of the powders has been done using SEM, and X-Ray
analysis. Finally they have concluded that the milled powders had metastable bcc solid
solution of Si and Ni in Fe with a fine particle structure. The maximum saturation
magnetization (Ms) and minimum coercivity (H-c) were obtained at the optimum
composition of Fe85Si10Ni5 after 70hrs milling [12].

El-Eskandarany et al., studied the effect of milling speed in a Fritch pulverisette-5 mill.
They reported that the time required for the formation of an amorphous phase in the Co-Ti
system decreased with an increase in the rotation speed. While it took 200h for the formation
of the amorphous phase at a speed of 65 rpm, it took only 100h at 125rpm and 24h at 200rpm.
They had observed acyclic crystalline amorphous crystalline transformation on continued
milling [13].

17
 Yang Yuanzheeng, et al, at the Academia Sinica, Heifa have studied nano-structure of
iron formed by mechanical milling. They have conducted the experiments using
Pulverisette-5 planetary ball mill with steel vials and steel balls. The starting material used
was iron powders with an average particles size of 76 µm powders. The ball to powder
weight ratio (BPR) was 20:1. Milling speed was set to 230 rpm and powder particles were
milled for 80h in one vial. Powder sample was picked up from the vials after selected interval
of milling time to see the change in shape and size reduction of powder sample. The powder
milling resulted in particles with grain size of up to 6nm and the conclusion of this work is
that mechanical grinding is an effective method to produce nanometer powders of pure
elements [14].

R. Hamzaoui of University de Technologie de Belfort-Montbeliard, France, has studied

the structure and mag netic properties of nanocrystalline mechanically alloyed Fe-10wt %
Ni and Fe-20 wt. %Ni alloys of mixtures. The average particle size of Fe was 7µm and Ni
was 250µm; the ball to powder ratio 10:1, and rotational speed was kept constant at 400rpm.
They have reported that the crystallite size decreases from 54±1.5 to 10.4±1.5nm and the
internal strain ε increases from 0.10 ± 0.05 to 0.69 ± 0.05. The crystalline size and lattice
strain with respect to Fe-20 Ni is D= 51.2±1.5 to 9.8± 1.5 nm for 96hrs of milling and lattice
strain ε = 0.11± 0.05% to 0.72 ±0.05 %. The conclusion of this work is Fe and Ni powders
form solid solution accompanied by grain refinement and grins size reduced resulted in an
increase of the magnetization and a decrease of the coercivity values [15].

The effect of milling speed during milling of a Fe-7wt % C-6wt % powder blend in a
planetary ball mill was investigated at three different speeds of 80, 100, and 120 rpm by
Rochman et al. They noted that the solid solubility of carbon in iron increased with
increasing speed of operation of the mill for the same milling time. For example, they
reported that on 100h of milling, the solid solubility of C in α-Fe was 0.2 at % at 80rpm, 0.5
at% 100rpm, and 1.3 at % 120rpm [16]

H.F. Li and Ramanujan, School of Materials Engineering, Nanyang Technological

University, Singapore, have studied the microstructure evolution and formation of
nanocrystalline Fe-Co based alloys by mechanical alloying. They have reported that
planetary ball milling of 22 mesh iron powder with 100mesh cobalt powders with a ball to
powder ratio 10:1 and speed of 300rpm would result in powder particle size of 3.3 µm after
70hrs. Table 1 shows the reduction in particle size as a function of milling time and
composition. They have characterized the powders using SEM, TEM and X-ray analysis.
Finally they have concluded that the milled powders are not magnetically soft but a variation
18
in coercivity with milling time has been observed that is related to the microstructural
evolution. After 5hours of milling, the saturation magnetization for the unalloyed Fe50Co50
and Fe44.5Co44.5P7B4 were 175.7emu/g and 167.2 emu/g [17].

Aim of the Project

The main aim of the proposed project is to design and fabricate the 3D ball milling
attachment with three relative moments. One rotary motion is given to the container with the
help of motor which rotates in clockwise direction and the other rotary and linear motions
are given to the stirrer which rotates in anticlockwise direction. In-order to resolve the
problem the container and the stirrer is operated with a constant speed of 856.5 rpm and
824.5 rpm. The feed rate i.e., 0.12 cm/sec which is given to the stirrer must be constant
throughout the process.

In this chapter we have clearly explained about the past review work done by the different
authors about the high energy ball milling. The methodology of the proposed project is
clearly explained in the next chapter.

19
CHAPTER 3
 METHODOLOGY

In the previous chapter, We have presented about the past review work done by the
researchers. The methodology following for our project is based on their work and we have
modified some of the information taken from their journals. The present chapter clearly
explains about the methodology of the present project we followed.

3.1. Explanation and objective of 3D ball milling attachment

Typically, the 3D ball milling attachment consists of a cylindrical jar mounted on an

appropriate basis which is attached to a motor and allows rotation motions. The top part of
the jar or vial is designed like a removable cap which is used to fill the jar with material and
after completing the process the material which is in final state must be taken out from the
jar and testing is to be done to the final material. The stirrer or impeller which is with 12mm
dia is inserted in the chuck of the drilling machine and by operating the equipment with two
motions i.e., linear & rotary motions is applied to the impeller.
Finally, the variation of Sic particle size under various spindle speed, chamber speed,
rotating impeller speed and time of milling is measured & reported.

3.2. Flow chart of overall progress

The following flow chart describes the overall progress of the project :-

Start

Selection of project title and

discussion with supervisor

Collections of journals and

Resources regarding project title

Modelling in solidworks(3 types)

& selecting one of the model

Assumption of Design Specifications

20
 Material Purchasing

Fabricating the Ball Mill

Attachment to the Drilling M/C

Run the ball mill

No
Test the Not in small
small particles particles

Yes

Measure the size of the small particles

Final documentation

End

3.3. Demands of successful processing and economical production

In the laboratory stage, the main criteria is the successful processing. Small quantities of
product mostly received by batch modes are suitable. To perform a successful process, a high
and homogeneous kinetic energy of ball impacts is necessary. To monitor the influence of
the processing onto the product, often a controlled atmosphere as well as a controlled
temperature is needed. Temperature control is critical as the transfer of heat from the
spherical milling media into a cooling system of the grinding chamber is naturally poor. The
level of contamination is of major importance. In principle, any kind of the here discussed
processing without impurities from the milling tools is not possible. Whit respect to this, the
contamination must be acceptable either by quality or by quantity.
21
 In case of an industrial application, several additional demands must be obeyed: Most
important is the reproducibility of the processing that must lead to a homogeneous product.
A homogeneous product can only be guaranteed if there are no dead-zones in the process
where a dead-zone is described as an area where powder can be located but the milling tools
have no access. The worst-case effect would be that the processed product would be polluted
with non- or not completely processed starting material. Very important is the scalability of
the process where it is naturally preferable to scale up proportional based on laboratory
testing. With respect to this, the device itself should be scalable which means availability of
large industrial systems based on the same principle than small laboratory units. Due to the
fact that the high kinetic processing leads to high (large) and active surfaces, the oxidation
reaction is of an extremely high kinetic. Often materials are treated, that in principle exhibit
a high affinity to oxygen and nitrogen. Therefore the processing but also charging and
discharging which means loading and unloading the material must be done under vacuum or
inert gas condition. This leads to a necessary availability of air-lock systems and
gas/vacuum-tight devices in many cases.
The product costs shall be as low as possible which, regarding the producing costs refers
to a short processing time, to a high degree of automatic, to a low proportion of workforce
as well as to low investment, operation and maintenance costs. The protection of human and
nature is of major importance. The final goal can be summarized as a 100 % process-control.

In this chapter, We have clearly explained about the overall process of the project in the
name of methodology. In-order to design and fabricate the 3D ball milling attachment to
the radial drilling machine, we have to create a model by using SOLIDWORKS software
is clearly explained in the next chapter.

22
CHAPTER 4
 MODELLING

In the previous chapter, We have discussed about the overall process of our project in the
name of methodology. In this present chapter, We have created a model of all the
components which are required to our project by using SOLIDWORKS software.

4.1. Introduction

SolidWorks is a solid modeler, and utilizes a parametric feature-based approach which

was initially developed by PTC (Creo/Pro-Engineer) to create models and assemblies. The
software is written on Parasolid-kernel. Parameters refer to constraints whose values
determine the shape or geometry of the model or assembly. Parameters can be either numeric
parameters, such as line lengths or circle diameters, or geometric parameters, such as tangent,
parallel, concentric, horizontal or vertical, etc. Numeric parameters can be associated with
each other through the use of relations, which allows them to capture design intent.
Design intent is how the creator of the part wants it to respond to changes and updates.
For example, you would want the hole at the top of a beverage can to stay at the top surface,
regardless of the height or size of the can. SolidWorks allows the user to specify that the hole
is a feature on the top surface, and will then honor their design intent no matter what height
they later assign to the can. Features refer to the building blocks of the part. They are the
shapes and operations that construct the part. Shape-based features typically begin with a 2D
or 3D sketch of shapes such as bosses, holes, slots, etc. This shape is then extruded or cut to
add or remove material from the part. Operation-based features are not sketch-based, and
include features such as fillets, chamfers, shells, applying draft to the faces of a part, etc.
Building a model in SolidWorks usually starts with a 2D sketch (although 3D sketches
are available for power users). The sketch consists of geometry such as points, lines, arcs,
conics (except the hyperbola), and splines. Dimensions are added to the sketch to define the
size and location of the geometry. Relations are used to define attributes such as tangency,
parallelism, perpendicularity, and concentricity. The parametric nature of SolidWorks means
that the dimensions and relations drive the geometry, not the other way around. The
dimensions in the sketch can be controlled independently, or by relationships to other
parameters inside or outside of the sketch. In an assembly, the analog to sketch relations are
mates. Just as sketch relations define conditions such as tangency, parallelism, and
concentricity with respect to sketch geometry, assembly mates define equivalent relations
with respect to the individual parts or components, allowing the easy construction of
assemblies. SolidWorks also includes additional advanced mating features such as gear and
23
cam follower mates, which allow modeled gear assemblies to accurately reproduce the
rotational movement of an actual gear train.
Finally, drawings can be created either from parts or assemblies. Views are automatically
generated from the solid model, and notes, dimensions and tolerances can then be easily
added to the drawing as needed. The drawing module includes most paper sizes and
standards (ANSI, ISO, GIS, GOST, JIS, BSI and SAC).

4.2. Details and modelling of 2D Views of all components

To model and assemble the 3D ball milling attachment components as by using

SolidWorks 2013 version. The tools required to model this project equipment requires a
personal computer in which a SolidWorks software is installed, sketch, extrude, fillet, etc.

Impeller model details along with 2D views

1. Open SolidWorks 2013 icon> select front plane>normal to>sketch.

2. Select circle from tool bar>dia ∅8mm>extrude boss/base upto 150mm.
3. Select the front plane of the sketch>normal to>sketch>select hexagon upto 13.40 mm of
length and angle is 178.20°.
4. Extrude boss base upto 5mm.
5. Open file> save Impeller.
The following Fig 4.1 shows the impeller model

Fig 4.1 Impeller

The following Fig 4.2 shows the 2D view of the impeller

24
 Fig 4.2 Impeller in 2D view

Container model details along with 2D views

1. File>new>part>select front plane>normal to>select sketch>take circle of 60mm dia from

tool bar>extrude it upto 80mm.
2. Select front plane>normal to>sketch>take circle with 50mm dia>cut extrude upto 70mm.
3. Select front plane>normal to>sketch>take circle of 60mm>extrude it upto 10mm.
4. Select front plane>normal to>sketch>circle of 8mm> cut extrude to 30mm.
5.Select front plane>normal to>sketch>circle of 8mm> cut extrude to 30mm on the other
side of the component.

The following Fig 4.3 and Fig 4.4 shows the model and 2D view of the container in
detailed manner:

25
 Fig 4.3 Container

Fig 4.4 Container in 2D view

26
Motor shaft model details along with 2D views

1. File>new>part>select front plane>normal to>sketch>take circle with 8mm dia from the
tool bar and extrude it upto 45mm.
2. Open File>Save as motor shaft.
The following Fig 4.5 and Fig 4.6 shows the model and 2D view of the motor shaft

Fig 4.5 Motor shaft

Fig 4.6 Motor shaft in 2D view

27
Supporting column along with motor model details along with 2D views

1. File>new>part>select front plane>normal to>sketch>select rectangle from the tool

bar>length 300mm & width 30mm>extrude boss/base upto 40mm.
2. Select top plane>click normal to on sketch>sketch rectangle>40mm width & 200mm
length >extrude boss/base upto 30mm.
3. Select top plane>click normal to>sketch>take circle> with 8mm dia> click cut extrude
upto 82mm.
4. Select top plane>click normal to on the sketch>take rectangle from tool bar> length
280.62mm &width 74.28mm.
5. Extrude it upto 10mm.
6. Give the fillets>select four edges of the column>10mm fillet.
7. Select top plane on the base>click normal to >sketch>take rectangle of length 50mm &
width 30mm>extrude it upto 10mm.
8. Take top plane>select circle>8mm dia>cut extrude it upto 10mm.
9. Open file>save as>supporting column along with motor part.
The following Fig 4.7 and Fig 4.8 shows the model and 2D view of the supporting column
along with motor part:

Fig 4.7 Supporting column along with motor part

28
 Fig 4.8 Supporting column along with motor part in 2D view

4.3. Assembly and Animation of 3D ball mill using SolidWorks Software

Assembly

1. Open solidworks>file>new>assembly>insert components>all components are to be

selected by clicking on browse( container, impeller, motor shaft, supporting column along
with motor part).
2. Mate the components using coincident mate(motor bottom circle and shaft circle).
3. Mate the components using concentric mate(shaft top circle and container circle).
4. Mate the components using concentric mate(supporting column top circle and impeller).
5.Open file>save as> Assembly.

Animation
1. Open the motion study>switch of the orientation and camera views.
2. Start the motor>select the rotary motor>motor location(impeller)> motion>constant
speed>100RPM>click ok.

29
3. Start the motor>select the linear motor>motor location(impeller) and component to move
relative to(container inside)> motion>and constant speed>5mm/s>click ok.
4. Start the motor>select the rotary motor>motor location (container)> motion>constant
speed>100RPM>click ok.
5. Calculate the result.
6. So that the animation video is done and runs with three motions(one linear and two rotary
motions).
7. This video clearly explains our project.
8. File > open >save as >animation of 3D ball mill .
The following Fig 4.9 shows the Assembly of 3D ball milling

Fig 4.9 Assembly of 3D ball milling

30
4.4. Assembly in 2D view and Different motions shown in the model

The following Fig 4.10 shows the 2D view of Overall assembly process:

Fig 4.10 Assembly in 2D view

Different motions :
The different types of motions which are used in this model are two rotary motions which
is given to the container and stirrer or impeller and one linear motion which moves up and
down is given to the stirrer itself .These three motions which are used in model is operated
simultaneously.

31
 The following Fig 4.11 shows the operations of different motions :-

Impeller
Anti- Clockwise direction Rotary motion
Linear motion of
impeller
supporting column

Clockwise
direction rotary motion of
container

container

motor shaft
motor head

base

Fig 4.11 Different motions

In this present chapter, We have created a model of 3D ball milling attachment by using
a SolidWorks software which is required to design and fabricate the 3D ball milling
equipment. This model clearly explains the overall process of our project. In the next chapter,
We are going to explain the calculations required for the design process.

32
CHAPTER 5
 DESIGN

In the previous chapter, We have presented a model of 3D ball milling attachment by

using the SolidWorks software. In this chapter, We are explaining the calculations required
for the 3D ball mill attachment in-order to know the details of the components.

5.1. Introduction

In general way designing means a plan or a scheme for giving shape to something, for
forming an idea about or for conceiving something. In this attempt we have designed the
volume of the container, mass of the container and we have calculated the torque , motor
speed and power. These calculations are done by design process to avoid mistakes or
problems that arise during fabrication and assembly stage.

5.2. Design calculations

The following are the design calculations which are required for the need of fabrication
purpose.

5.2.1. Selection of Container

The main component of the 3D ball milling attachment is the container or a jar or a vial
with the length and diameter of a reasonable proportion. The material used in fabrication
for a container is steel. It is attached with a motor shaft to install rotation motion for the
container. The speed of the container with and without load is calculated by using a non-
contact digital tachometer . The volume of the container is given by the formula
Container Volume (V)=L.𝜋. (𝑑 2)
Where,
L=Length of the container
𝑑=dia of the container
𝜋=3.14159
From specifications we know,
L=20cm=0.2m
𝑑=15cm=0.15m
.
V=0.2 × 𝜋 × ( )

⸫V=0.003534𝑚

33
 The following Fig 5.1 shows the container volume.

Fig 5.1 Container Volume

Mass: It is the product of volume and density.
Mass(m)=volume×density
=0.003534𝑚 × 𝑑𝑒𝑛𝑠𝑖𝑡𝑦
Since, according to specifications provided by Changsha Deco equipment company
limited, the density of stainless steel balls is 7930 𝑘𝑔⁄𝑚 .
Due to stainless steel balls have to fill upto 25% then it is given as
m=0.25 × 0.003534 × 7930
m=7kg

5.2.2. Selection of Motor

To generate the speed and control the speed of rotation , we decided to use a Moto-
Reducer .To this motor a regulator is to be given in order to regulate or vary the speed of the
motor. For the present trial,
we have chosen a 1hp motor to rotate the container with a maximum speed.

Motor torque:
It is a force which tends to cause rotation. It is given as
×
T=

Where, T torque (in lb-ft)

HP= horse power=1HP
5252= constant
rpm= revolutions per minute=1460
×
T= (lb-ft) ( ⸫lb-ft= pound-feet)

34
 =3.59lb-ft
T=4.86N-m

Current which is shown in ammeter when connected to the motor is 3.5A.

To control this high speed a dimmer-stat must be used.
Voltage supply given to the ac motor is 220V.
Speed of the motor is measured by using non-contact tachometer in RPM:-1460 rpm.
Power
Capacity to do something,
Power(P)=Voltage×current
=220𝑣 × 3.5𝑎𝑚𝑝
P=770watts

5.2.3. Selection of Motor Shaft

A shaft is a rotating member usually circular in cross-section , which is used to transmit

power and rotational motion.
In this 3D ball mill design , the shaft which is running with a rotary motion a container
is attached.

SHAFT DIAMETER
The size of the shaft ( diameter ) required to drive the ball mill can be estimated by
using the equation stated below :
. × ×
D= 𝑚𝑚

Where, P = Shaft power of the mill = 1hp

N = 75% of critical speed of the mill in rpm
CRITICAL SPEED
It is the speed at which unwanted vibration happens when a vessel is rotating. The
critical speed of the jar is given by the equation
.
critical speed (𝑁 )=
√

where,
D = Mill diameter = 15mm
d= Diameter of stainless steel balls=10mm

.
critical speed (𝑁 )= =18.91rpm
√

Since, to find shaft diameter we need to know the N value

35
 ⸫ N = 75% of critical speed of the mill in rpm = .
= 77.20rpm

Now,
. × ×
Shaft diameter D= 𝑚𝑚

. × ×
= .
𝑚𝑚

D=25.82mm

BALL-TO-POWDER RATIO
The ball to powder ratio ( BPR ) or charge ratio is another milling parameter and
represents the weight ratio of the milling balls to the powder charge. A wide range of BPR
have been used in a variety of investigations from values as low 1:1 to as high 220:1.
EXTENT OF FILLING OF THE MILLING CHAMBER
It is necessary that is enough space for the balls and the powder particles to move around
freely in the milling chamber . The volume of the container must be filled with 25% with
the required material.

5.2.4. Selection of Stirrer

A stirrer is a rotating device which is used to mix and reduce the size of the particles
inside the ball mill. In this trail, we have designed a stirrer with 11mm diameter and 29cm
length which is inserted to the chuck for the radial drilling machine. The speed of the stirrer
will rotates between 60 to 800 rpm as shown in Fig 5.2.

11mm
29cm

Fig 5.2 Stirrer

36
Extent of filling the vial:

Since the alloying among the powder particles occurs due to the impact forces exerted on
them, it is necessary that there is enough space for the balls and the powder particles to move
around freely in the milling container. Therefore, the extent of filling the vial with the powder
and the balls is important. If the quantity of the balls and the powder is very small, then the
production rate is very small. On the other hand, if the quantity is larger, then there is not
enough space for the balls to move around and so the energy of the impact is less. Thus, care
has to be taken not to overfill the vail; generally about 50% of the vail space is left empty.

In this present chapter, We have clearly mentioned the values of the design calculations
for our project. In the next chapter, We have taken the values from the design calculations
in the design chapter and started the fabrication process of 3D ball milling attachment.

37
CHAPTER 6
 FABRICATION

In the previous chapter, We have presented the design calculations for the requirement of
our project. These design calculations plays a dominant role in 3D ball mill attachment. In
this chapter, We are going to fabricate all the components which are required for attachment
purpose.

6.1. Introduction

Generally, fabrication is the action or process of manufacturing or inventing something.

In this fabrication we have done the 3D ball mill attachment and assembled it to the radial
drilling machine. The ball mill fabrication was done based on the below specifications and
the material is selected according to the requirement. The components of the 3D ball mill
attachment are container, motor, supporting stand and stirrer. The following table shows the
material selected for the fabrication of the 3D ball milling attachment

6.2. Specifications of all the components in detailed manner

A specification is a kind of requirement specification, and may show functional block

diagrams. A design or product specification describes the features of the solutions for the
Requirement Specification, referring to either a designed solution or final produced solution.
It is often used to guide fabrication/production. Sometimes the term specification is here
used in connection with a data sheet (or spec sheet), which may be confusing. A data sheet
describes the technical characteristics of an item or product, often published by a
manufacturer to help people choose or use the products. A data sheet is not a technical
specification in the sense of informing how to produce.
The components which are used in this fabrication chapter are container, plates, stirrer
and the steel balls.
The dimensions of all the components which are used in the 3D ball milling attachment
to the radial drilling machine is given below in a detailed manner in the below table 6.1.
After giving the clear dimensions of all the components in the below table 6.1 we went
for the fabrication process of the 3D ball mill components.
The components like container, plates etc., which mostly used in this fabrication process
is made up steel.

The below Table 6.1 shows the specifications of all the components in detailed manner.

38
Table 6.1 Specifications of all the components

S.no Name of the Figures Dimensions

components

Material:- Steel
Length:- 20cm
1. Container Inner Diameter:-15cm
Outer Diameter:-
15.8cm
Thickness:- 4mm

Material:- Steel
Use:- For opening and
2. Plates closing the container.
Diameter:-18cm
Thickness:-5mm

Material:- Steel
3. Stirrer Length:- 29cm
Diameter:-11mm

Type:-Ac motor
Speed:-1460rpm
4. Motor Power:-1hp
Current:-3.5amp

39
5. Equipment Materials:-Steel
support stand Length:-39cm
Height:-48cm

Use:- To measure the

6. Stopwatch time

7. Tachometer Use:-To find out the

speed of the
container(non-contact
digital type)

8. Stainless Diameter of different

steel balls size of balls:-5mm,
10mm, 15mm

Voltage: 0-300volts
9. Variac It is used for controlling
the speed of motor

40
6.3. Fabrication of all the components

The fabrication of all the components is done systematically . An equipment support stand
with 39×48 cm is to be fabricated and then the 1HP motor is seated in the equipment support
stand and fitted it with a nuts and bolts. To the high speed motor shaft which is with 25.82mm
diameter a container is attached which is made up of steel with dimensions 20cm height and
outer diameter 16cm .Then the stirrer with 29cm long is inserted through the 16mm plates
into the container which is made with a steel.
The fabrication or the assembly of all the components is shown in the below Fig: 6.3.
After finishing the fabrication part the total setup is attached to the radial drilling machine in
the laboratory.

Fig 6.1 Equipment stand along with motor

The above Fig 6.1 shows the motor which is fitted to the equipment stand.

Fig 6.2 Container attached to a motor shaft

41
 The above Fig 6.2 shows the container which is attached to a motor shaft which rotates
in a clockwise direction with a constant speed of 856.5 is fitted to the equipment stand and
this setup is attached to the base of the radial drilling machine. The fabricated 3D ball mill
system of all the components along with the stirrer which is to be inserted in the drilling
machine is shown in the following Fig 6.3

Fig 6.3 Fabricated 3D ball milling system

In this present chapter, We have fabricated all the components which are required for the
attachment purpose. In the next chapter, We have given an attachment of the fabricated 3D
ball mill setup to the radial drilling machine.

42
CHAPTER 7
 ATTACHMENT TO THE RADIAL DRILLING MACHINE

In the previous chapter, We have presented the fabrication of 3D ball milling attachment
components. In this present chapter, We are going to attach the 3D ball mill setup to the
radial drilling machine.
7.1. Introduction
All the components which are designed and fabricated is attached to a radial drilling
machine . Stirrer which contains 11mm diameter with two different motions is fixed in the
place of drill spindle with the help of chuck. Speed of the stirrer and container is done
constantly with different varying time .
The experimental setup is attached to the radial drilling machine is to run and reduce the
size of the particles into powders within a short duration. The container which is attached
with a 1 hp motor is operated with a 75% of the critical speed. The speed of the motor is
controlled by using a dimmer stat.
7.2. Experimental setup
The attachment of the 3D ball milling experiment setup is shown in the below Fig 7.1.

Fig 7.1 Attachment to the radial drilling machine

43
7.3. Working

3D ball milling attachment works on the principle of impact attrition i.e., size reduction
is done by impact as balls drop from the near the top of the shell. It is the process of
mechanical breakdown of solid particles into nano-powders without changing their state of
aggregation. 3D ball mill uses three relative motions simultaneously (two rotary & one linear
motion). The main objective of this project is to produce very fine powders with a particle
size of 10 microns . The purpose of using three simultaneous motions is used to decrease
the operating duration. The components used in this attachment contains a container , stirrer
and 1hp motor . The container which contains 25% of stainless steel balls and 30% work
material rotates in clockwise direction. It is opposite to the direction of stirrer which rotates
in anticlockwise direction and the linear motion is also given to the stirrer itself. All the
components which are designed and fabricated is attached to a radial drilling machine .
Stirrer which contains 12mm diameter with two different motions is fixed in the place of
drill spindle with the help of chuck. Speed of the stirrer and container is done with different
varying speed . Performance of the 3D ball milling is evaluated by mixing ratios of two
components. Because all of the solids in a ball mill are forced to endure thousands of impacts
by the grinding media over several hours, final particle size of 10 microns can be achieved
and with narrow size distribution. Because ball mills are closed systems there is no chance
for the finely divided solids to escape. Several of the independent variables can be reliably
controlled including mill cylinder speed, particle size, and operation time.

In this chapter, We have presented the attachment of 3D ball mill setup to the radial
drilling machine. In-order to operate the machine with three relative motions simultaneously
we have given this attachment. In the next chapter, We went for testing procedure to find the
final result i.e., final size of the particle.

44
CHAPTER 8
 RESULT AND DISCUSSION

In the previous chapter we have given an attachment of fabricated 3D ball mill setup to
the radial drilling machine. In this chapter, We have chosen three types of materials and
operated the 3D ball mill equipment under different time of milling. At the end of mill
operation we have founded the actual size of the particles and compared the values of three
materials under constant container speed, stirrer speed and feed rate.

8.1. Materials chosen for Testing purpose:

Test 1
For this test, Egg Shells are chosen in order to find out the size of the particle is
reducing or not as shown in Fig 8.1.

Fig 8.1 Egg shells

Firstly, hen egg shells are collected from the local hotels. To remove the impurity and
interference material the egg shells were washed several times in deionised water which is
show in below figure and after clean wash the egg shell are exposed to sun rays. This solution
is used for the size reduction purpose in the laboratory as shown in Fig 8.2.

Fig 8.2 Egg shells were washed several times in deionised water
45
Test 2

Aluminium oxide is a white to off white, fine-grained powder, highly porous form. For
this test, Al O is chosen in order to find out the size of the particle is reducing or not.

Fig 8.3 𝐴𝑙 𝑂 powder

Al O powder of 0.5kg is taken with a size of 40 microns and filled it in a container to

reduce the size of the Al O containing 40 microns to less than 10 microns as shown in
Fig 8.3.

TEST 3

For this test, Al powder is chosen in order to find out the size of the particle is reducing
or not.
Al powder of 1kg is taken with a size of 30 microns and filled it in a container to
reduce the size of the Al O containing 30 microns to less than 10 microns.
The following figure shows the content of the ‟ALUMINIUM POWDER” which is
going to be tested as shown in Fig 8.4.

46
 Fig 8.4 𝐴𝑙 powder

8.1.1. Precautions for Testing

 Do not enter the laboratory without shoes.

 Switch off the motor when there are heavy vibrations.
 After filling the container it must be closed with a plate.
 Avoid more than 75% of the critical speed.
 Test the sample size before and after testing with the help of the microscope.
 Fix the container to the motor shaft tightly.
 Three motions must be carried simultaneously while operating.
 Fix the equipment stand to the base properly.
 The dust caused by the samples and the stainless steel balls in the vial or container
must be cleaned.
 Switch off the main after completing the test.

8.2. Test-1
Size reduction of Egg Shells

The below Figure 8.6 shows the material of egg shell which is to be grinded for about 10
minutes in a mixer. After 10 minutes the powder which is formed in the mixer is taken in a
bowl and with the help of electronic digital weighting scale which is shown in Fig 8.7 the
powder weight of 250grams is measured and filled in the container. The below Fig 8.5 shows
the solid egg shell particles which is washed in deionized water.

47
 Fig 8.5 Egg shells after clean wash

The deionized egg shells after clean wash is grinded in a mixer about 10 minutes and
filled this powder in a container as show below. Before filling the container the egg shells
powder is allowed to measure in a micro scope in-order to find the exact particle size before
milling.

Fig 8.6 Egg shells filled in container

Fig 8.7 Electronic digital weighting scale

48
MICRO SCOPE REPORT

The micro scope report of egg shell powder before starting the 3D milling operation.

Fig 8.8 Before milling test report of egg shells

. . . . .
The average size of the egg shells is calculated as =

= 43.23microns.
Before milling sample of the egg shells is collected in a polythene cover as shown
below Fig 8.9.

Fig 8.9 Before milling egg shell sample

49
TEST FOR 30 MINUTES

Fill the container with stainless steel balls about 25% and also fill the egg shell powder
of 250grams and operate the 3D ball mill for 30 minutes and take the sample from the
container the sample is allowed to measure in the micro scope. The following figure shows
the percentage of the stainless steel balls and egg shell powder after 30 minutes.

Fig 8.10 Egg shell powder filled in container

The 30 minutes samples is collected for the container in polythene cover as shown in
Fig 8.11.

Fig 8.11 Egg shells after 30 minutes

MICRO SCOPE REPORT

The sample which is collected from the container after operating the 3D ball mill with
constant container speed of 856.5 rpm and constant stirrer speed of 824.5rpm with feed rate
of 0.12cm/sec is taken in a polythene cover and tested in micro scope. The micro scope report
of egg shell powder after 30 minutes is as shown in the Fig 8.12.

50
 Fig 8.12 After 30 minutes milling test report of egg shells

. . . . .
The average size of the egg shells is calculated as =

=26.68microns.
Size reduction in 30 minutes = initial size-final size =43.23-29.68 =13.55𝜇𝑚.

TEST FOR 1 HOUR

Fig 8.13 Egg shells after 1hour

51
 Similarly, after milling the 250grams of egg shells powder for 1hour the sample is
collected in a polythene as shown in the Fig 8.13.

MICRO SCOPE REPORT

The micro scope report of egg shell powder after 1hour is as shown in the Fig 8.14.

Fig 8.14 After 1hour milling test report of egg shells

. . . . .
The average size of the egg shells is calculated as =

=17.33microns.
Size reduction in 60 minutes = initial size-final size =43.23-17.33 =25.9𝜇𝑚.

TEST FOR 2HOURS

After operating the 3D ball mill with constant container speed of 856.5 rpm and constant
stirrer speed of 824.5rpm with feed rate of 0.12cm/sec and 250grams of egg shells powder
for 2 hours the sample is collected in a polythene cover as shown in Fig 8.15. The collected
sample is tested in the micro scope to know the exact size of the particles.

52
 Fig 8.15 Egg shells after 2hours

MICRO SCOPE REPORT

The micro scope report of egg shell powder after 1hour is as shown in the Fig 8.16.

Fig 8.16 After 2hours milling test report of egg shells

53
 . . . . .
The average size of the egg shells is calculated as =

=9.96microns.
Size reduction in 120 minutes = initial size-final size =43.23-9.96 =33.27𝜇𝑚.

TEST FOR 3HOURS

After operating the 3D ball mill with 250grams of egg shells powder for 3hours the sample
is collected in a polythene cover as shown in the Fig 8.17. The collected sample is tested in
the micro scope to know the exact size of the particles.

Fig 8.17 Egg shells after 3hours

MICRO SCOPE REPORT

The sample which is collected from the container after operating the 3D ball mill with
constant container speed of 856.5 rpm and constant stirrer speed of 824.5rpm with feed rate
of 0.12cm/sec is taken in a polythene cover and tested in micro scope. The micro scope report
of egg shell powder after 3hours is as shown in the Fig 8.18.

From the below test report ,

. . . . .
The average size of the egg shells is calculated as =

=4.62microns.
Size reduction in 180 minutes = initial size-final size =43.23-4.62
=38.61𝜇𝑚.

54
 Fig 8.18 After 3hours milling test report of egg shells

8.3. Test-1
Results

The below Table 8.1 shows the size reduction of egg shells by varying the time.

Table 8.1 Egg shell size reduction data table

Size
S. Time in Particle size reduction Container Stirrer Feed rate
No (min) (microns) (microns) speed speed (cm/sec)
(rpm) (rpm)

1. Before 43.23 - 856.5 824.5 0.12

milling

2. 30 29.68 13.55 856.5 824.5 0.12

3. 60 17.33 25.9 856.5 824.5 0.12

4. 120 9.96 33.27 856.5 824.5 0.12

5. 180 4.62 38.61 856.5 824.5 0.12

55
 Size reduction of Egg shells
50
45
Particle size reduction in (microns) 40
35
30
25
20 Grain size
15
10
5
0
Before milling 30 60 120 180
Time in (minutes)

Graph 8.1 Size reduction of Egg shells

The above Graph 8.1 shows the size reduction of egg shells under different time of
milling.

8.4. Test-2
Size reduction of Aluminium oxide

Before Milling

Take the sample of the Al O powder in the polythene cover before starting the operation
of ball mill and allow the powder to measure in micro scope. The below Fig 8.19 shows the
sample of the Al O powder before milling.

Fig 8.19 Before milling 𝐴𝑙 𝑂 powder sample

56
MICRO SCOPE REPORT
The micro scope report of Al O powder before starting the 3D milling operation.

Fig 8.20 Before milling test report of 𝐴𝑙 𝑂 powder

. . . . .
The average size of the Al2O3 is calculated as =

=36.49microns.
TEST FOR 30 MINUTES

Fig 8.21 𝐴𝑙 𝑂 powder filled in container

57
 Fill the container with stainless steel balls about 25% along with Aluminium oxide
powder of 250grams and operate the 3D ball mill for 30 minutes and take the sample from
the container and fill it in the polythene cover as show in Fig 8.22 and allow the sample to
measure in the micro scope. The following figure shows the percentage of the stainless steel
balls and Al O powder after 30 minutes.

Fig 8.22 𝐴𝑙 𝑂 powder after 30minutes

MICRO SCOPE REPORT

The micro scope report of Al O powder before starting the 3D milling operation.

Fig 8.23 After 30 minutes milling test report of 𝐴𝑙 𝑂 powder

58
 . . . . .
The average size of the Al O powder is calculated as =

=26.85microns.
Size reduction in 30 minutes = initial size-final size =36.49-26.85 =9.64𝜇𝑚.

TEST FOR 1 HOUR

Similarly, after milling the 250grams of Al O powder for 1hour the sample is collected
in a polythene as shown below Fig 8.24.

Fig 8.24 𝐴𝑙 𝑂 powder after 1 hour

MICRO SCOPE REPORT

The micro scope report of Al O powder after 1hour is as shown in the Fig 8.25.

Fig: 8.25 After 1hour milling test report of 𝐴𝑙 𝑂 powder

59
 .
The average size of the Al O powder is calculated as =

=12.59microns.
Size reduction in 60 minutes = initial size-final size =36.49-12.59=23.86𝜇𝑚.

TEST FOR 2HOURS

After operating the 3D ball mill with constant container speed of 856.5 rpm and constant
stirrer speed of 824.5rpm with feed rate of 0.12cm/sec and 250grams of Al O powder for
2hours the sample is collected in a polythene cover as shown below Fig 8.26. The collected
sample is tested in the micro scope to know the exact size of the particles.

Fig 8.26 𝐴𝑙 𝑂 powder after 2 hours

MICRO SCOPE REPORT

Fig 8.27 After 2 hours milling test report of 𝐴𝑙 𝑂 powder

60
 The micro scope report of Al O powder before starting the 3D milling operation as
shown in above Fig 8.27.
. . . . .
The average size of the Al O powder is calculated as =

=8.22microns.
Size reduction in 120 minutes = initial size-final size =36.49-8.22=28.23𝜇𝑚.

TEST FOR 3HOURS

After operating the 3D ball mill with 250grams of Al O powder for 3 hours the sample
is collected in a polythene cover as shown below Fig 8.28. The collected sample is tested in
the micro scope to know the exact size of the particles.

Fig 8.28 𝐴𝑙 𝑂 powder after 3hours

MICRO SCOPE REPORT

The sample which is collected from the container after operating the 3D ball mill with
constant container speed of 856.5 rpm and constant stirrer speed of 824.5rpm with feed rate
of 0.12cm/sec is taken in a polythene cover and tested in micro scope. The micro scope report
of 𝐴𝑙 𝑂 powder after 3hours is as shown in the Fig 8.29.

From the below test report ,

. . . . . .
The average size of the Al O powder is calculated as =

=2.66microns.

Size reduction in 180 minutes = initial size-final size =36.49-2.66

=33.79𝜇𝑚.

61
 Fig 8.29 After 3 hours milling test report of 𝐴𝑙 𝑂 powder

8.5. Test-2
Results

The below Table 8.2 shows the size reduction of Al O by varying the time of milling.

Table 8.2 𝐴𝑙 𝑂 powder size reduction data table

Size
S. Time in Particle size reduction Container Stirrer Feed rate
No (min) (microns) (microns) speed speed (rpm) (cm/sec)
(rpm)

1. Before 36.45 - 856.5 824.5 0.12

milling

2. 30 26.85 9.6 856.5 824.5 0.12

3. 60 12.59 23.86 856.5 824.5 0.12

4. 120 8.22 28.23 856.5 824.5 0.12

5. 180 2.66 33.79 856.5 824.5 0.12

62
 Size reduction of aluminium oxide
40

Particle size reduction in (microns)

35

30

25

20

15 Grain size

10

0
Before milling 30 60 120 180
Time in (minutes)

Graph 8.2 Size reduction of 𝐴𝑙 𝑂 powder

The above Graph 8.2 shows the size reduction of Al O powder under different time of
milling.

8.6. Test-3
Size reduction of aluminium powder

Before Milling
Take the sample of the Al powder in the polythene cover before starting the operation of
ball mill and allow the powder to measure in micro scope. The below Fig 8.30 shows the
sample of the Al powder before milling.

Fig 8.30 Before milling 𝐴𝑙 powder sample

63
MICRO SCOPE REPORT

The micro scope report of Al powder before starting the 3D milling operation.

Fig 8.31 Before milling test report of 𝐴𝑙 powder

. . . . .
The average size of the 𝐴𝑙 powder is calculated as =

=37.26microns.

TEST FOR 30 MINUTES

Fill the container with stainless steel balls about 25% along with Aluminium powder of
250grams and operate the 3D ball mill for 30 minutes and take the sample from the container
and fill it in the polythene cover as show in Fig 8.32 and allow the sample to measure in the
micro scope. The following figure shows the percentage of the stainless steel balls and Al
powder after 30 minutes.

64
 Fig 8.32 𝐴𝑙 powder filled in container

Fig 8.33 𝐴𝑙 powder after 30 minutes

MICRO SCOPE REPORT

The micro scope report of 𝐴𝑙 powder before starting the 3D milling operation
From the below test report,
. . . . .
The average size of the 𝐴𝑙 powder is calculated as =

=24.87microns.
Size reduction in 30 minutes = initial size-final size =37.26-24.87
=12.39𝜇𝑚.

65
 Fig 8.34 After 30 minutes milling test report of 𝐴𝑙 powder

TEST FOR 1 HOUR

Similarly, after milling the 250grams of Al powder for 1hour the sample is collected in
a polythene as shown below Fig 8.35.

Fig 8.35 𝐴𝑙 powder after 1 hour

66
MICRO SCOPE REPORT

The micro scope report of Al powder after 1hour is as shown in the Fig 8.36.

Fig 8.36 After 1 hour milling test report of 𝐴𝑙 powder

. . . .
The average size of the Al powder is calculated as =

=16.25microns.
Size reduction in 60 minutes = initial size-final size =37.26-16.25
=21.01𝜇𝑚.

TEST FOR 2HOURS

After milling the 250grams of Al powder for 2 hours the sample is collected in a
polythene as shown below Fig 8.37.

Fig 8.37 𝐴𝑙 powder after 2 hours

67
MICRO SCOPE REPORT

The micro scope report of Al powder after 2 hours is as shown in the Fig 8.38.

Fig 8.38 After 2 hours milling test report of 𝐴𝑙 powder

. . . . .
The average size of the Al powder is calculated as =

=8.66microns.
Size reduction in 120 minutes = initial size-final size =37.26-8.66
=28.6𝜇𝑚.

TEST FOR 3HOURS

Fill the container with stainless steel balls about 25% along with Aluminium powder of
250grams and operate the 3D ball mill for 3 hours and take the sample from the container
and fill it in the polythene cover as show in Fig 8.37 and allow the sample to measure in the
micro scope. The following figure shows the percentage of the stainless steel balls and Al
powder after 3 hours.
68
 Fig 8.39 𝐴𝑙 powder after 3 hours

MICRO SCOPE REPORT:

The micro scope report of Al powder after 3 hours is as shown in the Fig 8.40.

Fig 8.40 After 3 hours milling test report of 𝐴𝑙 powder

. . . . .
The average size of the 𝐴𝑙 powder is calculated as =

=3.44microns.
Size reduction in 180 minutes = initial size-final size =37.26-3.44
=33.82𝜇𝑚.
69
8.7. Test-4
Results

The below Table 8.3 shows the size reduction of 𝐴𝑙 powder by varying the time of
milling.

Table 8.3 𝐴𝑙 powder size reduction data table

Size
S. Time in Particle size reduction Container Stirrer Feed rate
No (min) (microns) (microns) speed speed (cm/sec)
(rpm) (rpm)

1. Before 37.26 - 856.5 824.5 0.12

milling

2. 30 24.87 12.39 856.5 824.5 0.12

3. 60 16.25 21.01 856.5 824.5 0.12

4. 120 8.66 28.6 856.5 824.5 0.12

5. 180 3.44 33.82 856.5 824.5 0.12

Size reduction of aluminium powder

40
Particle size reduction in (microns)

35

30

25

20

15 Grain size

10

0
Before milling 30 60 120 180
Time in (minutes)

Graph 8.3 Size reduction of 𝐴𝑙 powder

The above Graph 8.3 shows the size reduction of 𝐴𝑙 powder under different time of
milling.

70
COMPARISON TABLE

The below Table 8.4 shows the particle size of all the materials at different time of
milling.

Table 8.4 Comparing particle size reduction of all the materials

S. No Time in (min) Particle size of Particle size of Particle size of 𝐀𝐥

Egg shells 𝐀𝐥𝟐 𝐎𝟑 powder powder
(microns) (microns) (microns)

1. Before milling 43.23 36.45 37.26

2. 30 29.68 26.85 24.87

3. 60 17.33 12.59 16.25

4. 120 9.96 8.22 8.66

5. 180 4.62 2.66 3.44

Comparison of all materials

50
45
40
particlle size in(microns)

35
30
25 Egg shells
20 Alunimium oxide
15 Alunimium powder
10
5
0
Before milling 30 60 120 180
Time in (minutes)

Graph 8.4 Comparing particle size reduction of all the materials

The above Graph 8.4 shows the particle size reduction of all the materials under
different time of milling.

71
COMPARISON TABLE

The below Table 8.5 shows the comparison of size reductions of all the materials at
different time of milling.

Table 8.5 Comparing size reduction of all the materials

S. No Time in (min) Size reductions Size reductions Size reductions of

of Egg shells of 𝐀𝐥𝟐 𝐎𝟑 𝐀𝐥 powder
(microns) powder (microns)
(microns)

1. Before milling 43.23 36.45 37.26

2. 30 13.55 9.6 12.39

3. 60 25.9 23.86 21.01

4. 120 33.27 28.23 28.6

5. 180 38.61 33.79 33.82

By absorbing the above Table 8.5 and Graph 8.4 we have noticed that the size reduction
of aluminium oxide which is brittle in nature is more when compared to the size reduction
of remaining two materials i.e., egg shells and Al powder which are ceramic and ductile in
nature.

At the end of this chapter, We have absorbed that size reduction of aluminium oxide
which is brittle in nature is more when compared to the size reduction of remaining two
materials i.e., egg shells and Al powder which are ceramic and ductile in nature by varying
under different time of milling. In the next chapter, We have given a conclusion about our
project.

72
CHAPTER 9
 CONCLUSIONS

From our objectives, we have successfully achieved the main objective which is to Design
and Fabricate the 3D ball milling attachment with three relative motions that can grind solid
particles into smaller particles. Before going to the design calculations we have created a
model by using a SOLIDWORKS software by showing a three relative motions
simultaneously in the animation clip . One rotary motion which rotates in the clockwise
direction is given to the container with a constant speed of 856.5 rpm and the other rotary
motion which rotates in anticlockwise direction with a constant speed of 824.5 rpm is given
to the stirrer. To the same stirrer a linear motion is also given with a constant feed rate of
0.12cm/sec. The feed rate which is given in this project is a manual operation. After creating
the model, we went through the design process in which the container volume , critical speed
, mass , stirrer length , stirrer diameter and selection of motor is calculated . Further, we went
into the fabrication work in which a container with 15.8cm diameter and 20cm length is
attached to the motor shaft .After fabricating all the components ,the 3D ball mill setup is
attached to the radial drilling machine . Then the 3D ball mill setup is allowed for testing
purpose. In this present project, we have chosen three types of materials which is brittle,
ductile and ceramic in nature for testing purpose . From our first 30 minutes test, we were
able to gain some size reduction of the particle but not a fine powder. In order to get the fine
powder we have to run the 3D ball milling attachment more than 3 hours. At the end of the
testing process the size reduction of aluminium oxide which is brittle in nature is more when
compared to the size reduction of remaining two materials i.e., egg shells and Al powder
which are ceramic and ductile in nature. Further, the variation of time of milling is measured
and reported under constant container speed, stirrer speed and feed rate. Average particle
size reduces as milling time increases.
Throughout our project, we found out that determining all the variables before fabrication
is essential. By knowing the required parameter, fabricating become easier as no huge
changing of design is required. And also it is difficult to clean the container after operation.

73
CHAPTER 10
 FUTURE SCOPE

This project can be further carried out to get more results. Some of the future scopes of this
project includes:-
 Feed rate which is not given automatically shall be a further scope for improvement
in getting the fine powders within less duration.
 There is a difficulty faced by the project members after completing the operation to
clean the container.
 Milling parameter can be varied such as atmosphere, milling speed etc.

74
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