Appendix A

Sample Title Page

SYNTHESIS OF ZINC SILICATE USING SILICA FROM RICE

HULL ASH (RHA) THROUGH SOLID-STATE REACTION

A TECHNICAL PAPER

Presented to
the Graduate School of
School of Engineering and Architecture
Ateneo de Davao University
E. Jacinto St., Davao City

In Partial Fulfillment
of the Requirements for the Degree of
MASTER OF ENGINEERING
MAJOR IN CHEMICAL ENGINEERING

TENDER P. FEROLIN
October 2013
Industry Practice Guidelines 2

Appendix B
Sample Abstract

ABSTRACT

Successful synthesis of nanocrystalline Zn2SiO4 powders using solid state reaction of the
ZnO powder precipitate and amorphous cristobalite SiO2 powders from processed rice hull ash at
800T1000oC is presented in this study. ZnO powders were grown by chemically reacting
stoichiometric NaOH and ZnSO4. The solid state reacted powders were characterized using
scanning electron microscopy (SEM) with energy dispersive x-ray spectroscopy (EDX), Fourier
transform spectroscopy (FTIR) and x-ray diffraction (XRD). Microscopic analyses of the
annealed powders were consistent with reported morphological structures of Zn2SiO4. FTIR
results indicate the presence of ZnO4 and SiO4 groups corresponding to Zn2SiO4. XRD results
further revealed that Zn2SiO4 powders were synthesized at the reaction temperatures of 900 and
1000oC with onset growth at 800oC. The method used in this study shows that Zn2SiO4 can be
grown at a much lower temperature (800T1000oC) compared to the reported temperature of
synthesizing Zn2SiO4 through solid-state reaction. The Zn2SiO4 powders exhibit dominant a-axis
orientation and the average crystallite size for zinc silicate powders annealed at 1000oC is about
33 nm. The results suggest that the Zn2SiO4 powders are promising materials for phosphor
applications. Using SiO2 from RHA in the synthesis of ZnSiO4 increases the value of rice hulls
and as a result becomes beneficial to rice farmers and that RHA collection and utilization
policies has to be incorporated in local governments.
Industry Practice Guidelines 3

Appendix C
Sample Table of Contents

TABLE OF CONTENTS

Page
TITLE PAGE i
APPROVAL SHEET ii
ABSTRACT iii
ACKNOWLEDGEMENT iv
LIST OF TABLES v
LIST OF FIGURES vi
LIST OF APPENDICES vii
CHAPTER
1 INTRODUCTION 1
1.1 Significance of the Study 5
1.2 Theoretical Framework 5
1.3 Objectives of the Study 8
1.4 Scope and Limitation 10
2 REVIEW OF RELATED LITERATURE 11
2.1 Chemical and Physical Properties 11
2.1.1 Zinc Silicate 11
2.2 Methods of Synthesis 18
2.2.1 Wet Process 18
2.2.2 Solid-State Reaction 19
2.3 Specific Experimental Approaches in Solid-
State Reaction 19
2.3.1 Grinding 19
2.3.3 Drying 20
2.4 Characterization Techniques 22
2.4.1 Scanning Electron Microscopy and Energy
Dispersive X-Ray Spectroscopy 23
2.4.2 Fourier Transform Infrared Spectroscopy 23
2.4.3 X-Ray Diffraction (XRD) 24
3 METHODOLOGY 26
3.1 Raw Materials 26
3.2 Synthesis of Zinc Silicate 27
3.2.1 Preparation of Standard Zinc Silicate 27
3.3 Characterization Techniques 31
3.4 Summary of Process of Synthesis 33
4 RESULTS AND DISCUSSIONS 37
4.1 Synthesis 37
4.2 Characterization 45

5 SUMMARY, CONCLUSIONS AND

RECOMMENDATIONS 80

BIBLIOGRAPHY 87
CURRICULUM VITA 96
Industry Practice Guidelines 4

Appendix D
Sample List of Tables

LIST OF TABLES

Page

Table 2.1 Standard Electromotive Force Series 25

Table 4.1 Elemental Analysis of Synthesized Zinc Silicate Powders 43

Table 4.2 Vibrational Modes on FTIR Spectra of Synthesized Zinc

Silicate Powders 51

Table 4.3 Diffraction Peaks on XRD Patterns of Synthesized Zinc

Silicate Powders 51
Industry Practice Guidelines 5

Appendix E
Sample List of Figures

vi

LIST OF FIGURES

Page

Figure 4.1 FTIR Spectra of Synthesized Zinc Silicate 41

Figure 4.2 SEM Micrographs of Synthesized Zinc Silicate 44

Figure 4.3 XRD Patterns of Synthesized Zinc Silicate 52

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Appendix F
Sample List of Appendices

vii

LIST OF APPENDICES

Page

A Elemental Analyses of Synthesized Zinc Silicate 86

B FTIR Spectra of Synthesized Zinc Silicate 91

C Diffraction Peaks of Synthesized Zinc Silicate 96

D Micrographs of Synthesized Zinc Silicate 101

Industry Practice Guidelines 7

Appendix G
Sample Chapter

CHAPTER 1
INTRODUCTION

Doped zinc silicate (Zn2SiO4) is utilized in various electronic applications such as

cathode ray tubes [1], plasma display panels [2], electroluminescent equipment [3] and imaging
devices for mammographic applications [4]. Zn2SiO4 is used as host matrix for doping ions such
as europium (Eu3+), terbium (Tb3+), nickel (Ni2+) and manganese (Mn2+) [5,6]. However,
despite the importance of zinc silicate in electronics industry, the Philippines is unable to
produce zinc silicate that can largely attribute to the following: (1) the existing processes used in
the synthesis of zinc silicate powders requires acquisition of modern and expensive equipment,
(2) the present methods used require high working temperatures between 1200 and 3250oC, and
(3) the technique used in the synthesis of zinc silicate requires chemical reagents which have
working conditions that are uneconomical in tropical countries, expensive and need to be
imported. Thus, with the current economic and energy crisis that the country is experiencing, it is
imperative to explore other process of synthesis addressing the concerns cited. Hence, this study
is undertaken to synthesize zinc silicate using locally available precursors, readily available
equipment, lower temperature requirement for synthesis and manufacture of high-grade zinc
silicate in the country that can be utilized for significant uses in the electronics industry.

The current production of zinc silicate utilizes inorganic precursors such as zinc oxide
[7], Zn(NO3)2 [8] and Zn(OOCCH3)2 [9] as Zn source and tetraethylorthosilicate (TEOS)
[10,11], quartz SiO2 [12] and hexamethyldisoloxane (HMDSO) [13] as source for SiO2. Zinc
acetate, on the other hand, is usually used as the precursor source of [14,15,16]. Other methods
make use of zinc oxide and silicon dioxide powders as the precursors [18]. However, the
precursors used such as TEOS and HMDSO have unfavorable characteristics. For instance,
TEOS has a ash point of 52oC [19]. Its use is a setback in tropical countries like the Philippines
where ambient temperature is 33oC but can be higher during summer months. On the other hand,
Industry Practice Guidelines 8

Appendix H
Labeling of Equations, Figures and Tables

Label for Equations:

Volume = Area of Base (Height) Equation 4.1

Label for Figures:

Figure 4.5. Micrographs of Zinc Silicate

Label for Tables:

Table 4.4 Elemental Analysis of Galvanized Iron Taken Every Ten (10) Days
Day 0 Day 10 Day 20 Day 30
Element
Atom%
Oxygen xx.xx xx.xx xx.xx xx.xx
Iron xx.xx xx.xx xx.xx xx.xx
Zinc xx.xx xx.xx xx.xx xx.xx
Industry Practice Guidelines 9

Appendix I
Sample Bibliography

87

BIBLIOGRAPHY

[1] Tani T., et al., Emulsion Combustion and Flame Spray Synthesis of Zinc Oxide/Silica
Particles, J. Nanopart Res 5 (2003) 39-46.

[2] Zeng J.H., et.al., Precursor, base concentration and solvent behavior on the formation of zinc
silicate, Mater Res Bull 44 (2009) 1106-1110.

[3] Inoue Y., et al., Photoacoustic spectra on Mn-doped zinc silicate powders by evacuated
sealed silica, J. Mater Sci 43 (2008) 378-383.

[4] TEOS. 2010. Online. 9 March 2011. www.chemilink.com/msds/78-10-4 243.pdf.

[5] Hexamethyldisoloxane. 2010. Online. 9 March 2011.

www.sciencelab.com/msds.php?msdsId=992429.

[6] Natarajan V., et. al., Photoluminiscence investigation of Zn2SiO4 codoped with Eu3+and T
b3+ions, Solid State Communications 134 (2005) 261-264.

[7] Maloney, J.O. Perrys Chemical Engineers Handbook 8th ed. (McGraw- Hill, 2008) 2-15,
2-18, 2-24, 2-27.

[8] Zinc and compounds: Health effects. Online. 19 January 2010. http://www.npi.gov.au/
substances/zinc/health.html

[9] Lou T.J., et al. A facile synthesis to Zn2SiO4:Mn2+phosphor with controllable size and
morphology at low temperature, J. Colloid Interf Sci 314 (2007) 510513.

[10] Barin I. and O. Knacke Thermochemical Properties of Inorganic Substances (Berlin:

Springer, 1973) 891.

[11] Zinc Silicate. 2009. Online. 1 August 2009.

http://www.pesticideinfo.org/Detail_Chemical.jsp?Rec_Id=PC38348.

[12] Callister, William D.Materials Science and Engineering: An Introduction, 6th ed. (Wiley &
Sons Inc., 2003) 84,575.
Industry Practice Guidelines 10

Appendix J
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