STRUCTURAL CHARACTERIZATION OF ASYMMETRIC YTTRIA...
Transcript of STRUCTURAL CHARACTERIZATION OF ASYMMETRIC YTTRIA...
STRUCTURAL CHARACTERIZATION OF ASYMMETRIC YTTRIA-
STABILIZED ZIRCONIA HOLLOW FIBRE MEMBRANE
SYAFIKAH HUDA BINTI PAIMAN
UNIVERSITI TEKNOLOGI MALAYSIA
STRUCTURAL CHARACTERIZATION OF ASYMMETRIC YTTRIA-
STABILIZED ZIRCONIA HOLLOW FIBRE MEMBRANE
SYAFIKAH HUDA BINTI PAIMAN
A thesis submitted in fulfilment of the
requirement for the awards of
the degree of Master of Engineering (Gas)
Faculty of Chemical and Energy Engineering
Universiti Teknologi Malaysia
FEBRUARY 2016
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ACKNOWLEDGEMENT
Alhamdulillah. Praised to Allah SWT with His blessed and guidance I got
the opportunity and successfully finished my master study. Deeply thanks to my
parents (Paiman bin Sanusi and Rozi Noriah binti Sukarno), my sister (Nurul Azwa)
and my brother for their constant encouragement, advice and du’a. I truly appreciate
their love, tolerance and understanding.
I would sincerely like to thank my supervisor Dr. Mukhlis bin A Rahman for
his guidance, endless support and du’a throughout my master study and for the
opportunities I have been given to attend conference which give a chance to develop
my presentation skill. I felt very comfortable expressing my opinion at all times and I
am grateful to have benefited from his extensive experience and knowledge not only
in membrane study but also in many other aspects of life as a researcher and as a
slave of Allah in general. I would like to thank Dr. Mohd Hafiz Dzarfan bin Othman
for his excellent advice offered as my co-supervisor.
Special thanks to my friends Miss Halimah, Miss Shuhaida, Miss Fazliana,
Mrs. Iera, Muhazri, Zureen, Azuwa, Azlan and Hilmi Mohamad for their endless
help from the very beginning of instrument installation to the experimental work and
for their kindly help and advice.. Also, thanks to AMTEC’s research officer for help
I have received and everyone in the AMTEC team. Lastly, I am grateful to Ministry
of Science, Technology and Innovation (MOSTI) and Universiti Teknologi Malaysia
(UTM) for financial supports.
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ABSTRACT
Ceramic membrane is proven to overcome a limitation of using polymeric
membrane for applications that requires a high temperature and pressure. In this
study, Yttria-stabilized zirconia (YSZ) was selected as a ceramic material due to its
superior mechanical strength. YSZ hollow fibre membrane was fabricated using
combined dry-wet phase inversion and sintering technique. Four parameters involved
during fabrication process have been varied systematically to study the effect on
YSZ hollow fibre membrane structure and properties. The ceramic loading was
varied from 55 wt.% to 67 wt.% and the YSZ/polyethersulfone (PESf) ratio was
varied from 7 to 10 during YSZ suspension preparations. Then, the air-gap length
was varied from 15 cm to 30 cm during spinning process. Lastly, the sintering
temperature was varied from 1250 oC to 1400
oC during sintering step. The YSZ
hollow fibre membrane produced were characterized in terms of morphology,
mechanical strength, apparent porosity, pure water flux and solute rejection. The
results successfully showed an asymmetric YSZ hollow fibre membranes consist of
finger-like voids and sponge-like voids were produced. The YSZ suspension
viscosity was increased with the increase of YSZ loading and decrease of YSZ/PESf
ratio. High suspension viscosity favored the growth of finger-like voids and limited
the formation of sponge-like region across the membrane. This result was similar to
increase of the air-gap length during spinning. Significant densification occurred at
the sponge-like region during sintering. The formation of isolated voids at 1400 oC
hindered the pure water permeation. However, the mechanical strength increased
with the sintering temperature. From the permeation test, the YSZ hollow fiber
membrane prepared with 65 wt.% loading, ceramic/polymer ratio of 10, spinning at
20 cm air-gap length and sintered at 1300 oC was the most preferable membrane.
This membrane had a pure water flux of 118.4 Lm-².hr
-¹ with a molecular weight cut
off of 50 – 60 kDa and mechanical strength of 224 MPa.
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ABSTRAK
Membran seramik terbukti boleh mengatasi masalah penggunaan membran
polimer untuk aplikasi yang memerlukan suhu dan tekanan yang tinggi. Yttria-stabil
zirkonia (YSZ) telah dipilih sebagai bahan seramik dalam kajian ini kerana kekuatan
mekanikal yang tinggi. Membran asimetrik gentian gerongga YSZ telah dihasilkan
menggunakan gabungan teknik penyongsangan fasa kering dan pensinteran. Empat
parameter yang terlibat telah diubah semasa proses penghasilan untuk mengkaji
kesan terhadap struktur dan sifat membran gentian gerongga YSZ. Kandungan
seramik diubah dari 55 % jisim hingga 67 % jisim dan nisbah YSZ/polietersulfon
(PESf) telah diubah dari 7 hingga 10 semasa penghasilan larutan YSZ. Selain itu,
panjang sela udara semasa proses pemejaman diubah daripada 15 cm hingga 30 cm.
Akhir sekali, suhu ketika proses pembakaran dinaikkan dari 1250 oC hingga 1400
oC.
Membran gentian gerongga YSZ yang terhasil dicirikan dari segi morfologi,
kekuatan mekanikal, keliangan ketara, kebolehtelapan air tulen dan penolakan bahan
larut. Keputusan menunjukkan membran asimetrik gentian gerongga YSZ terdiri
daripada lompang seperti jari dan lompang seperti span berjaya dihasilkan. Kelikatan
larutan YSZ meningkat dengan peningkatan kandungan YSZ dan pengurangan
nisbah YSZ/PESf. Kelikatan yang tinggi, kadar pertumbuhan lompang seperti jari
adalah tinggi dan menyekat pertumbuhan lompang seperti span dalam membran.
Keputusan ini sama dengan kesan peningkatan jarak sela udara semasa proses
pemejaman. Peningkatan suhu pembakaran menyebabkan pemadatan pada bahagian
struktur-mikro dan mengurangkan keliangan. Pembentukan lompang terpencil pada
suhu 1400 oC telah menghalang penelapan air tulen. Namun, peningkatan suhu
pembakaran telah meningkatkan kekuatan mekanikal. Ujian penelapan menunjukkan,
membran gentian gerongga YSZ yang dihasilkan dengan kandungan 65 % jisim,
nisbah seramik/polimer 10, panjang sela udara 20 cm dan disinter pada suhu 1300 oC
menghasilkan fluks air tulen sebanyak 118.4 Lm-².hr
-¹ dengan berat molekul terputus
sebanyak 50 hingga 60 kDa dan kekuatan mekanikal 224 MPa.
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TABLE OF CONTENT
CHAPTER TITLE PAGE
TITLE PAGE i
DECLARATION ii
ACKNOWLEDGEMENT iii
ABSTRACT iv
ABSTRAK v
TABLE OF CONTENT v
LIST OF TABLES ix
LIST OF FIGURES xi
LIST OF ABBREVIATIONS xv
LIST OF SYMBOLS xvii
LIST OF APPENDICES xxvix
1 INTRODUCTION 1
1.1 Background of Study 1
1.2 Problem Statement 4
1.3 Objective 5
1.4 Scope of Study 6
1.5 Significant of Study 7
1.6 Thesis Structure 7
2 LITERATURE REVIEW 9
2.1 Introduction of Ceramic Membrane 9
2.2 The Configuration of Ceramic Membrane 13
2.3 Fabrication Method of Ceramic Membrane 15
2.3.1 Slip Casting 16
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2.3.2 Tape Casting 17
2.3.3 Dip Coating 18
2.3.4 Extrusion 20
2.4 Ceramic Hollow Fibre through Combined Phase Inversion
and Sintering Process 21
2.4.1 Ceramic Suspension 23
2.4.2 Spinning 27
2.4.3 Sintering 32
2.5 Applications 36
2.5.1 Membrane Filtration 36
2.5.2 Catalyst Substrate for Microreactor 40
3 RESEARCH METHODOLOGY 42
3.1 Introduction 42
3.2 Materials 44
3.2.1 Zirconia 45
3.3 Fabrication of Ceramic Hollow Fibre Membrane 47
3.3.1 Preparation of Ceramic Suspension Solution 48
3.3.2 Spinning Process 50
3.3.3 Sintering Process 52
3.4 Characterization 54
3.4.1 Scanning Electron Microscopy 54
3.4.2 Three Point Bending Test 55
3.4.3 X-Ray Diffraction 56
3.4.4 Atomic Force Microscopy 56
3.4.5 Viscosity 56
3.4.6 Apparent Porosity 57
3.4.7 Pure Water Permeation 57
3.4.8 Solute Rejection 59
4 RESULTS AND DISCUSSIONS 61
4.1 The Effect of Ceramic Loading on the YSZ Hollow Fibre
Membrane 62
4.1.1 Rheology of Ceramic Suspension 62
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4.1.2 Morphology 64
4.1.3 Mechanical Properties 66
4.2 The Effect of Air-gap Length on the YSZ Hollow Fibre
Membrane 68
4.2.1 Morphology 68
4.2.2 Mechanical Properties 71
4.3 The Effect of Ceramic/Polymer Ratio on the YSZ Hollow
Fibre Membrane 73
4.3.1 Rheology of Ceramic Suspension 73
4.3.2 Morphology 74
4.3.3 Mechanical Properties 77
4.4 The Effect of Sintering Temperature on the YSZ Hollow
Fibre Membrane 78
4.4.1 Morphology 78
4.4.2 Mechanical Properties 85
4.4.3 Apparent Porosity 86
4.4.4 XRD Pattern 87
4.4.5 Pure Water Flux 88
4.4.6 PEG Rejection 90
5 CONCLUSION AND RECOMMENDATION 92
5.1 Conclusion 92
5.2 Recommendation 94
REFERENCES 96
APPENDIX A 105
APPENDIX B 106
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LIST OF TABLES
TABLE NO. TITLE PAGE
2.1 The general comparison of ceramic, metal and polymer 10
2.2 The applications for the porous ceramic membrane 12
2.3 The applications for the dense ceramic membrane 12
2.4 The comparison between hollow fibre, tubular and flat
sheet membrane configuration 15
2.5 The list of dip-coating method 20
2.6 The factors that affecting the suspension solution
preparation 25
2.7 The spinning condition involves during spinning process 28
2.8 Microstructural changes observed during sintering
process 35
2.9 The sintering conditions that effect the final membrane
formation 36
2.10 The type and characteristic of membrane filtration 38
3.1 Mechanical properties of stabilized zirconia 47
3.2 The composition of YSZ suspension solution with
different ceramic loading 49
3.3 The composition of YSZ suspension solution with
different ceramic: polymer ratio 50
3.4 The spinning condition for ceramic hollow fibre
membranes 52
4.1 The wall thickness of YSZ hollow fibre membrane wall
thickness prepared at different ceramic loading and
sintered at 1400 oC 67
4.2 The wall thickness of YSZ hollow fibre membrane wall
thickness at different air-gap length and prepared at 65
wt. % ceramic loading 71
x
4.3 The wall thickness of YSZ hollow fibre membrane
prepared at different ceramic/polymer ratio and sintered
at 1400 oC 78
4.4 The wall thickness of YSZ hollow fibre membrane wall
thickness at different sintering temperature and prepared
at 65 wt. % YSZ loading 86
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LIST OF FIGURES
FIGURE NO. TITLE PAGE
1.1 The simple mechanism of membrane process 2
1.2 Polymer and ceramic membrane timeline 3
2.1 The a) asymmetric and b) symmetric ceramic hollow
fibre membrane structure 11
2.2 Flat sheet membrane configuration i.e. a) flat sheet
membrane and b) the process 13
2.3 Hollow fibre membrane configuration i.e. a) different
type of tubular membrane and b) the process 14
2.4 Tubular membrane configuration i.e. a) hollow fibre
membrane and b) the process 15
2.5 The general step of fabricating ceramic membrane 16
2.6 Slip casting 17
2.7 The illustration of tape casting method 18
2.8 The illustration of dip-coating method 19
2.9 The illustration of extrusion method 21
2.10 Surface morphology of YSZ hollow fibre membrane
sintered at 1200 oC and prepared at (a) 0.1 μm and (b)
0.1 μm/20 nm 26
2.11 The illustration of tube-in-orifice spinneret from the
bottom side 27
2.12 The asymmetric structure of ceramic membrane i.e. a)
finger-like void (microstructure) and b) sponge-like
void (macrostructure) 28
2.13 The asymmetric Al2O3 hollow fibre membrane
prepared at different ceramic suspension viscosity; a)
18.5 Pa.s and b) 45 Pa.s 29
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2.14 The sandwich structure of ceramic hollow fibre
membrane 30
2.15 The schematic diagram of spinning process for ceramic
hollow fibre membrane 30
2.16 The sintering profile 33
2.17 Mechanism for grain growth of sintering model: (a)
two particles are in contact; (b) neck growth between
the particles by surface diffusion; (c) grain growth 34
2.18 The changes in microstructure of SCYb hollow fibre
membrane over sintering process; a) before sintering
and b) sintering at 1400 oC 36
2.19 The type of membrane filtration with the type of filtrate 37
2.20 The membrane filtration mode. (a) dead-end filtration
and (b) crossflow filtration 39
2.21 Asymmetric hollow fibre: (a) sponge-like region and
(b) finger-like region with catalyst deposition 40
2.22 Four different features of incorporated catalyst in
ceramic hollow fibre membrane 41
3.1 The flow chart of experimental work 44
3.2 Three crystalline forms in zirconia structure 46
3.3 The general procedure of fabrication of ceramic hollow
fibre membranes 47
3.4 The preparation steps of ceramic suspension solution 49
3.5 The schematic diagram of degassing system 50
3.6 The schematic diagram of spinning system for ceramic
hollow fibre fabrication 51
3.7 The spinneret used during experiment with dimension
of outer diameter/ internal diameter of 2.8 mm/0.5 mm 52
3.8 The sintering profile of sintering process 53
3.9 The schematic diagram preparation of hollow fibre
membrane for SEM characterization 54
3.10 The schematic diagram of three point bending strength
test 55
3.11 The schematic diagram of ceramic hollow fibre
membrane module 58
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3.12 The schematic diagram of hollow fibre membrane
filtration system 59
4.1 The rheological behavior of YSZ/NMP/PESf/Arlacel
suspension solution prepared with different ceramic
loading 63
4.2 Photographic image of YSZ hollow fibre membrane
prepared with 55 wt. % YSZ loading and sintered at
1400 oC 64
4.3 The overall morphology (i) and cross-sectional
structure (ii) of YSZ hollow fibre membrane, extruded
at 10 ml/min, bore fluid rate at 7 ml/min, 15 cm air-gap
and sintered at 1400 oC with different ceramic loading:
(a) 62 wt. %, (b) 65 wt. % and (c) 67 wt. % 65
4.4 The mechanical strength of YSZ hollow fibre
membranes prepared with different ceramic loading; 62
wt. %, 65 wt. % and 67 wt. % and sintered at constant
sintering temperature; 1400 oC 66
4.5 The illustration of ceramic loading 67
4.6 The overall morphology (i) and cross-sectional
structure (ii) of YSZ hollow fibre membrane prepared
with 65 wt. % of ceramic loading, extruded at 10
ml/min bore fluid rate, 7 ml/min extrusion and varying
air-gap length; (a) 15 cm, (b) 20 cm and (c) 30 cm and
sintered at 1400 oC 70
4.7 The mechanical strength of YSZ hollow fibre
membrane prepared at ceramic loading 65 wt. %
ceramic loading at varying air-gap length and sintered
at 1400 oC 72
4.8 The rheological behavior of YSZ/NMP/PESf/Arlacel
suspension solution prepared with different ceramic:
polymer ratio 74
4.9 The overall morphology (i) and cross-sectional
structure (ii) of 65 wt. % YSZ hollow fibre membrane,
extruded at 10 ml/min, bore fluid rate at 7 ml/min, 15
cm air-gap and sintered at 1400 oC with different
ceramic/polymer ratio; (a) 10/1, (b) 9/1, (c) 8/1 and (d)
7/1 76
4.10 The mechanical strength of YSZ hollow fibre
membrane sintered at 1400 oC, prepared different
ceramic/polymer ratio, extruded at 10 ml/min, bore
fluid rate of 7 ml/min and air-gap length of 15 cm 77
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4.11 The overall morphology structure (i) and cross-
sectional structure (ii) of YSZ hollow fibre membranes
sintered at different sintering temperature; (a) 1250 oC,
(b) 1300 oC, (c) 1350
oC and (d) 1400
oC 80
4.12 The sponge-like region structure (microstructure) of
YSZ hollow fibre membranes sintered at different
sintering temperature; (a) 1250 oC, (b) 1300
oC, (c)
1350 oC and (d) 1400
oC 82
4.13 The SEM images (i) and AFM images (ii) of surface
morphology structure of YSZ hollow fibre membranes
sintered at different sintering temperature; a) 1250 oC,
b) 1300 oC, c) 1350
oC and d) 1400
oC 84
4.14 The mechanical strength of YSZ hollow fibre
membrane prepared using 65 wt. % ceramic loading
with 20 cm air-gap length and sintered at different
sintering temperature 85
4.15 The apparent porosities of YSZ hollow fibre membrane
prepared using 65 wt. % ceramic loading with 20 cm
air-gap length and sintered at different sintering
temperature 87
4.16 The XRD patterns of YSZ powder and YSZ hollow
fibre membrane sintered at different sintering
temperature 88
4.17 The pure water flux and apparent porosity of YSZ
hollow fibre membrane at different sintering
temperature; 1250 oC, 1300
oC, 1350
oC and 1400
oC 89
4.18 The morphology of YSZ hollow fibre membranes
sintered at 1400 oC; a) microstructure region and b)
surface 89
4.19 The 3P strength and pure water flux of YSZ hollow
fibre membrane at different sintering temperature 90
4.20 The solute rejection of YSZ hollow fibre membrane
using PEG with different molecular weight at different
sintering temperature 91
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LIST OF ABBREVIATIONS
YSZ - Yttria-stabilized zirconia
SEM - Scanning electron microscopy
AFM - Atomic force microscopy
XRD - X-ray diffraction
Al2O3 - Aluminum oxide
ZrO2 - Zirconia
TiO2 - Titanium dioxide
UF - Ultrafiltration
Pd - Palladium
HFMR - Hollow fibre micro reactor
CHFMR - Ceramic hollow fibre micro reactor
CHFMMR - Ceramic hollow fibre membrane micro reactor
WGS - Water gas shift
DRM - Dry reforming of methanol
MSR - Methanol steam reforming
LSCF - Lanthanum-strontium-cobalt-ferric
SOFC - Solid oxide fuel cell
NiO2 - Nickel oxide
TIPS - Thermally induced phase separation
DIPS - Diffusion induced phase separation
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NMP - N-Methylpyrrolidone
NaOH - Sodium hydroxide
Na2ZrO3 - Sodium zirconate
Na2SiO3 - Sodium silicate
Zr(OH)4 - Zirconium hydroxide
ZrSiO4 - Zirconium silicate
Y2O3 - Yttria
MgO - Magnesium oxide
CaO - Calcium oxide
CuO - Copper oxide
MF - Microfiltration
NF - Nanofiltration
RO - Reverse osmosis
H2 - Hydrogen
ESR - Ethanol steam reforming
CeO2 - Cerium oxide
PESf - Polyethersulfone
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LIST OF SYMBOLS
A - Area of hollow fibre
BF - Bending strength
cm - Centimeter
D - Dry weight
d - Thickness
Di - Inner diameter
DO - Outer diameter
g - Gram
L - Length
L - Length of hollow fibre
m - Meter
min - Minute
N - Load
M - Saturated weight
S - Suspended weight
T - Temperature
t - Time
W - Watt
wt - Weight
°C - Degree Celsius
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% - Percent
µm - Micrometer
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LIST OF APPENDICES
APPENDIX TITLE PAGE
A Publication and presentation 105
B Calculation for the percentage distribution length of
finger-like voids and sponge-like region 106
CHAPTER 1
INTRODUCTION
1.1 Background of Study
Membrane can be defined as a semipermeable barrier between two phases
that selectively separate some components from others. In detail, membrane will only
allow a selective component to permeate through it and reject the permeation of other
components. Figure 1.1 illustrates the membrane process. The basic principles of
membrane which is simple in concept and operation, low energy consumption,
environmental friendly and more flexible as it is easy to scale-up made it well suited
for large-scale operations in various applications. The key pillar in membrane
technology is producing a membrane with a structure that have a high selectivity and
permeability. The desired membrane structure may be different based on the
applications. In addition to the selectivity and permeability, the membrane life time
and the durability are another important character which should be taken into
consideration to ensure the feasibility of the membrane in particular application and
economically viable.
Back in the 18th
century, the emergence development of membrane
technology has been started from the phenomenon of water permeation through a pig
bladder used to store alcohol which has been noticed by Jean-Antoine Nollet, a
physicist. He was probably the first to recognize the relation between a
semipermeable membrane and the osmotic pressure. Later, more studies on
semipermeable membrane and osmotic pressure were conducted by Thomas Graham
on the diffusion of gasses through different media [1]. Then, a rapid advancement of
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membrane technology in following decades is also aided by Fick and van t’Hoff who
explained the diffusion of solutes in liquid media. It can be seen, the early stage of
membrane technology is focusing more on theoretical explanation of membrane
process. Besides, most of the early studies on membrane permeation were carried out
with natural material such as animal bladder.
Figure 1.1 The simple mechanism of membrane process
Early twentieth century, membrane science and technology entered a new
phase of producing an artificial membrane. A fabrication method that is popularly
known as phase inversion and invented by Loeb and Sourirajan [2] gives a new
phenomenon in producing artificial membrane. The flat sheet membrane produced is
in asymmetric structure with a dense skin at the surface which determined the
membrane selectivity and permeation flux while the porous structure provided the
mechanical strength. Then, progress in polymer science contributed to the fabrication
of polymeric membrane using this method. It is seen in dominating the membrane
markets as being used in spanning number of applications includes; filtration [3,4]
and gas separation [5]. Subjected to the medical applications, polymeric membrane
also found to be used for hemodialysis.
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The nature of ceramic materials which were mechanically, thermally and
chemically resistance had gather an interest to use it for ceramic membrane
fabrication. The ceramic membrane was successfully widening the membranes
applications range to membrane reactor [6–8] and fuel cell application [9,10].
Besides, ceramic membrane may even replace the polymeric membrane application
in microfiltration [11–13], ultrafiltration [14], nanofiltration [15], reverse osmosis
[16] and gas separation [17,18]. Here, the development of membrane technology
keep expanding as it moves from the natural material to polymer membrane and then
towards ceramic membrane. Figure 1.2 shows the timeline of the development in
membrane technology.
Figure 1.2 Polymer and ceramic membrane timeline [19]
Concerning on the issue of water related problem, treating and/or purifying
the contaminated water before channeled for usage is vitality important. Even though
water is the most abundance natural resources, only less than 1 % of it is available
for human consumption. As man uses water as one of the main resources for daily
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activities together with the rapid developments of industrial, agricultural and
domestic activities, it brings about to the broadening of water related problems. The
conventional treating method for water and wastewater includes one or more of the
processes; chemical addition, coagulation, flocculation, sedimentation, filtration,
adsorption and disinfection. However, the rising technology in membrane area has
gathered an interest to replace the conventional process with membrane process. The
ability to remove a wide range of components, ranging from suspended solids to
small organic compounds and ions have made membrane such a promising technique
for water and wastewater treatment. Yet, the renowned ceramic membrane over
polymeric membrane encourages of using ceramic membrane for filtration
applications.
1.2 Problem Statement
Phase inversion method introduced by Loeb and Sourirajan in fabricating
cellulose acetate membrane (polymeric membrane) have become the most common
method used in membrane fabrication. However, due to the differences between
polymeric and ceramic systems, particularly in dope solution preparation limits the
use of the phase inversion information in polymeric systems for ceramic membrane
fabrication. In polymeric system, the phase inversion process involved the interaction
between polymer, solvent and non-solvent. The solvent was diffused out from the
polymer solution while non-solvent was diffused into the dope solution. The solvent
and non-solvent exchanged results in solidification of polymer solution and
formation of polymeric membrane. Different in ceramic system; the solidification of
ceramic suspension solution involves in the movement of ceramic particles during
the solvent and non-solvent exchanged. Moreover, low polymer content and high
ceramic content in ceramic suspension solution influenced the phase inversion
process for ceramic membrane.
Ceramic membranes have been reported to have a number of advantages in
various applications. However, ceramic membranes have their own respective
desired morphology depending on the ceramic membranes’ applications. From the
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aforementioned literature, it can be deduced that different ceramic materials used for
membrane fabrication produced a hollow fibre membrane with different structures
and properties. In this study, yttria-stabalized zirconia (YSZ) was selected as a
ceramic membrane material. However, limited research have been focused on the
structural study of YSZ hollow fibre membrane through phase inversion method
drives an interest to study the process conditions effects towards the structure and
properties.
The fabrication of ceramic membrane through this phase inversion method
composed of three main steps and in every step, the process conditions were
contributed to the structure formation. Aforementioned study reported that the
ceramic loading and the ceramic/polymer ratio influenced the structure formation for
alumina oxide (Al2O3) membrane. However, no study was reported on these
parameters for YSZ hollow fibre membrane structure formation. Besides, the air-gap
lengths during spinning process were reported to give a significant effect for Al2O3
hollow fibre membrane structure formation. This gathers an attention to study the
effect air-gap length on the YSZ hollow fibre membrane prior to the selection of
membrane for certain applications. Lastly, the sintering process gave impact
particularly in term of the surface morphology, microstructure, grain growth and pore
evaluation or elimination. Thus, this stage played an important role to determine the
final properties of ceramic membrane. The sintering temperature must be controlled
subjected to the feasibility of YSZ membrane for water purification application as
using YSZ membrane for this application is still new.
1.3 Objective
Referring to the problems stated in 1.2, the aim of this research study is to
fabricate a ceramic hollow fibre membrane made from Yttria-stabilized zirconia by
using combined phase inversion method and sintering process. This study involves
the preparation of ceramic suspension solution, spinning and sintering process. In
each process, there having parameters that gives influenced on the structure of
ceramic hollow fibre membrane. Thus, a morphological study of YSZ hollow fibre
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membrane is important as it may be a guideline for the fabrication of YSZ hollow
fibre membrane for a specific application. In order to achieve this aim, the following
objectives were carried out:
1) To study the effect of ceramic loading and ceramic/polymer ratio
during suspension preparation on the morphology structure and the
properties of YSZ hollow fibre membrane
2) To study the effect of air-gap length during spinning process on the
morphology structure and the properties of YSZ hollow fibre
membrane
3) To study the effect of sintering temperature on the microstructure and
the properties of YSZ hollow fibre membrane for water purification
application
1.4 Scope of Study
The following scope of work is carried out to achieve objectives stated in
1.3:
1) Preparing the ceramic suspensions for spinning process using
planetary ball mill at different ceramic loadings and ceramic/polymer
ratios
2) Measuring the viscosities of ceramic suspensions using viscometer
3) Fabricating the ceramic hollow fibre precursor by dry-wet phase
inversion at different air-gap length
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4) Sintering the ceramic hollow fibre precursors at different sintering
temperature using high temperature furnace
5) Characterizing the effect of ceramic loading, ceramic/polymer ratio,
air-gap length and sintering temperature on the morphology structure
and properties of ceramic hollow fibre membrane by using scanning
electron microscopy (SEM), atomic force microscopy (AFM), three
point bending test, X-ray diffraction (XRD), apparent porosity, pure
water permeation tests and solute rejection tests
1.5 Significant of Study
A structural study related to YSZ hollow fibre membrane was not well
studied yet. This research will give an overview on the effect of the process
conditions during membrane fabrication on the morphology of YSZ hollow fibre
membrane produced. Besides, it gives a guideline for the future study to prepare YSZ
membrane with a desired structure base on the application. Moreover, the
development of ceramic hollow fibre membrane through combined phase inversion
and sintering process are promising in reducing the production cost together with the
simple technology concept that can reduce the time consumed. Other than that, this
study discovers the feasibility of YSZ hollow fibre membrane to be used in water
separation applications.
1.6 Thesis Structure
This report consists of five chapters. In the first chapter, a brief description
on the research backgrounds, research problems, research objectives and scopes were
presented. In Chapter 2, the literature review discussed on the development of
ceramic membrane, the advantages of ceramic membrane over polymeric membrane,
the fabrication method of ceramic membrane and the application of ceramic
membrane were presented. In Chapter 3, the research methodology included the
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materials, the analytical procedures and the characterization involves during study is
presented. Chapter 4 presents the results and discussions to answer the objectives
stated above. It discusses the changes occur over varying the parameters during YSZ
hollow fibre membrane fabrication onto the structure and the properties. Lastly, the
conclusion of whole study was presented in Chapter 5. Besides, few
recommendations are also listed for future study and enhancement.
96
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