vii
TABLE OF CONTENTS
CHAPTER
I
TITLE
PAGE
DECLARATION
ii
DEDICATION
iii
ACKNOWLEDGEMENT
iv
ABSTRACT
v
ABSTRAK
vi
TABLE OF CONTENTS
vii
LIST OF TABLES
xi
LIST OF FIGURES
xiii
LIST OF SYMBOLS
xvii
LIST OF ABBREVIATIONS
xix
LIST OF APPENDICES
xx
INTRODUCTION
1.1
Background
1
1.2
Problem Statement
3
1.3
Objectives of the research
4
1.4
Scope of the research
5
1.5
Thesis Plan
6
viii
II
III
LITERATURE REVIEW
2.1
Introduction
7
2.2
Definition of ceramic
8
2.3
Transition element
11
2.4
The structure of TiO2 based ceramic
13
2.5
Lithium (II) Oxide (Li2O)
16
2.6
Nickel Oxide (NiO)
17
2.7
Forming process
18
2.7.1 Dry pressing
18
2.7.2 Sintering process
20
2.8
X-Ray Diffraction (XRD)
23
2.9
Scannning Electron Microscopy (SEM)
25
2.10 Density
28
2.11 Hardness
29
2.12 BET Specific Surface Area
31
2.13 DC Conductivity
37
2.14 Semiconductor
41
2.14.1 Intrinsic semiconductor
41
2.14.2 Extrinsic semiconductor
42
2.14.2(a) n-type material
42
2.14.2(b) p-type material
43
EXPERIMENTAL PROCEDURE
3.1
Introduction
45
3.2
Sample preparation
45
3.3
Measurement and characterization
48
3.3.1 X-Ray Diffraction (XRD)
48
3.3.2 Scanning Electron Microscopy
49
(SEM)
3.3.3 Density
49
ix
3.3.4 Hardness
50
3.3.5 Brunauer Emmett Teller (BET)
51
Specific Surface Area
3.3.6 DC Conductivity
IV
RESULTS AND DISCUSSION
4.1
Introduction
55
4.2
Sample preparation
55
4.3
Crystalline phase analysis
57
4.3.1 Effect of sintering temperature
57
4.3.2 Effect of composition
60
4.4
Surface Analysis (morphology)
62
4.5
Density
64
4.5.1 Effect of sintering temperature
65
4.5.2 Effect of NiO content
66
Hardness
68
4.6.1 Effect of sintering temperature
68
4.6.2 Effect of Li2O content
69
Porosity (BET method)
70
4.7.1 Effect of sintering temperature
71
4.7.2 Effect of Li2O content
72
DC Conductivity
76
4.8.1 Effect of sintering temperature
76
4.8.2 Effect of Li2O content
77
4.6
4.7
4.8
V
52
CONCLUSIONS
5.1
Introduction
79
5.2
Sample Preparation
79
5.3
Crystal Phase and Morphology Analysis
80
x
5.4
Density and Hardness
80
5.5
Surface Area
81
5.6
DC conductivity
81
5.7
Suggestions for future work
81
REFERENCES
83-94
APPENDICES
95-103
xi
LIST OF TABLES
TABLE NO.
TITLE
PAGE
2.1
The stage of sintering.
22
2.2
Pore size classification.
32
2.3
The classification of adsorption isotherms.
35
2.4
The majority and minority charge carriers in
44
semiconductor.
3.1
The sample composition of xLi2O-(50-x)NiO–
46
50TiO2 (0 ≤ x ≤50 mol %).
4.1
The crystallite size of 30Li2O-20NiO-50TiO2
59
ceramic after sintered at different temperature.
4.2
The phase occurrence in 30Li2O-20NiO-
60
50TiO2 ceramic after sintered at different
temperature for nine hours.
4.3
The phase occurrence in xLi2O-(50-x)NiO-
62
50TiO2 ceramic (0  x  50 mol %).
4.4
Density of 30Li2O-50NiO-50TiO2 ceramic
65
sintered at different temperature.
4.5
Density of the xLi2O - (50-x) NiO-50TiO2
ceramic
at
different
NiO
and
67
Li2O
concentration.
4.6
Specific area (m2/g) and particle size (m) of
71
30Li2O-20NiO-50TiO2 ceramic at varies of
sintering temperature (C).
4.7
Specific surface area (m2/g) and particle size
73
xii
(m) of ceramic at difference Li2O level.
xiii
LIST OF FIGURES
FIGURE NO
2.1
TITLE
PAGE
The ionic bond of Na+ and Cl- composition.
10
This is a result of electrostatic (or coulombic)
attraction between oppositely charged ions.
2.2
The covalent bonding.
11
2.3
Blocks within the Periodic Table.
12
2.4
Bulk structures of rutile and anatase. The
14
tetragonal bulk unit cell of cell of rutile has the
dimension,
the
one
and
of
anatase,
. In both structures, slightly distorted
octahedral are the basic building units. The bond
lengths
and
angles
of
the
octahedrally
coordinated Ti atoms are indicated and the
stacking of the octahedral in both structures is
shown on the right side.
2.5
Ball and stick model of rutile crystal structure. It
is composed of slightly distorted octahedral, two
of which are indicated. Along the [1 1 0]
direction these octahedral are stacked with their
long axes alternating by 90o. Open channel are
visible along the [0 0 1] direction. The dashed
lines A and B enclose a charge-neutral repeat
unit without a dipole moment perpendicular to
15
xiv
the [1 1 0]-direction.
2.6
The bulk structure of Lithium (II) Oxide.
16
2.7
The bulk structure of Nickel (II) Oxide.
17
2.8
The stages of dry pressing.
19
2.9
Schematic diagram showing the stage of granule
compaction.
2.10
Changes that occur during the initial stage of
20
sintering (a) starting particles (b) rearrangement
(c) neck formation.
2.11
Changes that occur during the second stage of
21
sintering (a) Neck growth and volume shrinkage
(b) lengthening of grain boundaries, and (c)
continued neck growth and grain boundary
lengthening,
volume
shrinkage
and
grain
growth.
2.12
Changes that occur during the final stage of
22
sintering. (a) Grain growth with discontinuous
pore phase. (b) Grain growth with porosity
reduction (c) grain growth with porosity
elimination.
2.13
SEM micrographs of AH90 powder sintered at
23
different sintering temperature. (a) 1100C (b)
1150C (c) 1200C (d) 1250C ; respectively.
2.14
Deriving Bragg's Law using the reflection
24
geometry and applying trigonometry. The lower
beam must travel the extra distance (AB + BC)
to continue travelling parallel and adjacent to
the top beam (Bengisu, 2001).
2.15
Schematic diagram of the scanning electron
27
microscope (Goldstein et al., 1981).
2.16
The diamond pyramid shape of Vickers indenter
having an angle of 136° between opposite
pyramid faces.
31
xv
2.17
IUPAC classification of adsorption isotherms.
33
2.18
Collinear four point probe showing current flow
38
and voltage measurement.
2.19
Conductivities of the various classes of material:
39
shading indicates the range of values at room
temperature.
2.20
The energy band for different materials: (a)
41
insulator (b) semiconductor (c) conductor.
2.21
A structure of silicon crystal which contains a
43
donor atom.
2.22
A structure of silicon crystal that contains an
44
acceptor.
3.1
Preparation of Li2O-NiO-TiO2 ceramic.
47
3.2
X-Ray Diffractor used in this experiment.
48
3.3
The SEM used in this experiment.
49
3.4
Density measurement by the Archimedes’
50
method.
3.5
Vickers Hardness Instrument used to measure
51
the hardness of the sample.
3.6
Autosorb Micromeritic (Model ASAP 2010)
52
used for BET analysis.
3.7
Probe configuration in contact with the surface
53
for dc conductivity measurement.
3.8
Instruments setup for obtaining sheet resistance
53
value.
3.9
Illustration of the probe array displacement on
54
the sample surface from aerial view.
4.1
The appearance of xLi2O-(50-x)NiO-50TiO2
56
ceramic with different compositions (a) 50NiO50TiO2 (b) 10Li2O-40NiO-50TiO2 (c) 20Li2O30NiO-50TiO2 (d) 30Li2O-20NiO-50TiO2 (e)
40Li2O-10NiO-50TiO2 (f) 50Li2O-50TiO2.
4.2
XRD pattern of 30Li2O-20NiO-50TiO2 ceramic
58
xvi
sintered at different temperature for 9 hours.
4.3
XRD pattern of xLi2O-(50-x)NiO-50TiO2 (0  x
61
50 mol %) sintered at 1100 C. Diffractograms
show the plot of intensity (I) against Bragg
angle (2).
4.4
SEM micrographs of 30Li2O-20NiO-50TiO2
63
ceramic sintered at different temperature (a)
700C (b) 800C (c) 900C (d) 1000C
(e)1100C.
4.5
The
variation
temperature
of
density
for
with
sintering
66
30Li2O-20NiO-50TiO2
ceramics.
4.6
Density () against NiO content (mol %)
67
sintered at 1100C.
4.7
Graph of hardness for 30Li2O-20NiO-50TiO2
69
ceramic against sintering temperature of the
sample.
4.8
Graph of hardness against mol % of Li2O
70
sintered at 1100C.
4.9
The surface area and particle size as a function
72
of sintering temperature.
4.10
Specific surface area and particle size versus
74
Li2O level sintered at 1100C.
4.11
Adsorption/desorption curve from BET analysis
75
4.12
Relationship between dc conductivity and
76
sintering temperature (C) for 30Li2O-20NiO50TiO2.
4.13
Relationship between the conductivity () and
Li2O content (mol %).
78
xvii
LIST OF SYMBOLS
A
-
Area of a material
Å
-
Angstroms

-
Full Width Half Maximum
e
-
Electron
F
-
Force
h
-
Planck constant
-
Hardness
I
-
Current
L
-
Probe distance from the edge
Ls
-
Sample length
l
-
Length of the material
n
-
Negative
p
-
Positive
P
-
Load
P’
-
Porosity
-
Partial pressure of oxygen
p
-
Partial pressure
R
-
Electrical resistance
Rs
-
Sheet resistance
R’
-
Particle size
S
-
Specific surface area
s
-
Probe spacing
s1
-
Probe spacing between probe (1) and probe
(2)
s2
-
Probe spacing between probe (2) and probe
xviii
(3)
s3
-
Probe spacing between probe (3) and probe
(4)
T
-
Temperature
t
-
Sample thickness
V
-
Voltage
Vin
-
Input voltage
V2
-
Voltage at probe 2
V3
-
Voltage at probe 3
V23
-
Voltage between probe (2) and probe (3)
Ws
-
Sample width
w
-
Width of a material
W1
-
Weight in air
W2
-
Weight in toluene
x
-
Probe position from the edge of the sample
<d>
-
Crystallite Size

-
Electrical conductivity

-
Electrical resistivity

-
Density
λ
-
Wavelength of X-Ray radiation

-
Pi = 3.14159

-
Diffraction angle
xix
LIST OF ABBREVIATIONS
Al2O3
-
Alumina
BET
-
Brunauer-Emmett-Teller
BJH
-
Barrett-Joyner-Halenda
DC
-
Direct Current
EDAX
-
Energy Dispersive X-Ray Analysis
Fe3O4
-
Magnetite
Li2O
-
Lithium (II) Oxide
MRI
-
Magnetic Resonance Imaging
NiO
-
Nickel Oxide
NMR
-
Nuclear Magnetic Resonance
ReO3
-
Rhenium Trioxide
SEM
-
Scanning Electron Microscopy
TiO
-
Titanium Oxide
TiO2
-
Titanium (IV) Dioxide
UV
-
Ultraviolet
VO
-
Vanadium Oxide
XRD
-
X-Ray Diffraction
xx
LIST OF APPENDICES
APPENDIX
TITLE
PAGE
A
The Sample Calculation
95
B
Periodic Table
98
C
BET graph
99