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University of Southampton Research Repository Eprints Soton University of Southampton Research Repository ePrints Soton Copyright © and Moral Rights for this thesis are retained by the author and/or other copyright owners. A copy can be downloaded for personal non-commercial research or study, without prior permission or charge. This thesis cannot be reproduced or quoted extensively from without first obtaining permission in writing from the copyright holder/s. The content must not be changed in any way or sold commercially in any format or medium without the formal permission of the copyright holders. When referring to this work, full bibliographic details including the author, title, awarding institution and date of the thesis must be given e.g. AUTHOR (year of submission) "Full thesis title", University of Southampton, name of the University School or Department, PhD Thesis, pagination http://eprints.soton.ac.uk CCoonnttrroolllleedd EElleeccttrrooddeeppoossiittiioonn ooff MMeettaall NNaannoocceennttrreess FFoorr CCaattaallyyssiiss by Hartini Haji Mohd. Yasin A thesis submitted for the degree of Doctor of Philosophy November 2010 UNIVERSITY OF SOUTHAMPTON ABSTRACT FACULTY OF NATURAL AND ENVIRONMENTAL SCIENCES SCHOOL OF CHEMISTRY Doctor of Philosophy Controlled Electrodeposition of Metal Nanocentres For Catalysis by Hartini Haji Mohd Yasin In this research, electrodeposition was used with the aim of preparing surfaces with controlled dispersion and uniform small centre size to enhance the catalytic performance. Nanoparticle catalyst centres are designed to minimize the amount of expensive metal components loaded onto a cheaper substrate but with optimum catalytic activity. The electrodeposition of platinum and gold nanocentres have been investigated by varying the deposition parameters in hydrogen hexachloroplatinate(IV) acid and hydrogen tetrachloroaurate(III) hydrate respectively. Various substrates such as microdisc, microband and microwire electrodes were used for the study of controlled electrodeposition. Their smaller surface area provides a better tool for the study of nucleation and growth of nuclei. The effect of mass transport was studied with microdisc and rotating disc electrodes. The mechanism for the reduction of hydrogen hexachloroplatinate(IV) in hydrochloric acid was investigated. Voltammograms show two reduction waves and both waves lead to the deposition of platinum(0). At high overpotential, the reaction becomes diffusion controlled. No dissolution of platinum is observed on the reverse scan. In contrast, the reduction of hydrogen tetrachloroaurate(III) hydrate in acidic media produces a simple mass transfer controlled three-electron reduction wave with a stripping peak of gold observed on the backward scan. Several approaches, such as cyclic voltammetry, single potential step and double- pulse potential step deposition were used to electrodeposit platinum and gold nanocentres. Isolated and hemispherical nanocentres of platinum and gold were successfully electrodeposited onto carbon surfaces. In contrast, the electrodeposition of platinum onto a gold substrate quickly leads to complete layers when observed with a scanning electron microscope. The platinum and gold nanocentres were characterized by means of cyclic voltammetry in acid solution, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDXS). The electrodeposition of platinum from a lyotropic liquid crystalline mixture, specifically from a micellar solution, produced platinum deposits with higher specific catalyst area than those deposited in aqueous solution. The nanostructured i platinum was not observable with the scanning electron microscope, even at high magnification; however the presence of nanostructured platinum was confirmed by cyclic voltammetry in sulphuric acid. On gold electrodes, the nanostructured platinum showed good catalytic response for hydrogen evolution and oxygen reduction reactions. This study has shown that a surface with small centres and high nuclei number density could be produced by electrodeposition at high overpotentials. A smooth surface with small centres deposited at low charge density will produce low roughness factor, and this makes it difficult to be confirmed with cyclic voltammetry in sulphuric acid. In addition, small centres of less than 50 nm cannot be observed using scanning electron microscopy. However, small centres are believed to be present on the surface as they lead to the centres observed at higher charge densities when deposited at very negative potentials. ii DECLARATION OF AUTHORSHIP I, Hartini Haji Mohd Yasin declare that the thesis entitled Controlled Electrodeposition of Metal Nanocentres For Catalysis and the work presented in the thesis are both my own, and have been generated by me as the result of my own original research. I confirm that: · this work was done wholly or mainly while in candidature for a research degree at this University; · where any part of this thesis has previously been submitted for a degree or any other qualification at this University or any other institution, this has been clearly stated; · where I have consulted the published work of others, this is always clearly attributed; · where I have quoted from the work of others, the source is always given. With the exception of such quotations, this thesis is entirely my own work; · I have acknowledged all main sources of help; · where the thesis is based on work done by myself jointly with others, I have made clear exactly what was done by others and what I have contributed myself; · parts of this work have been published as: Ø H. M. Yasin, G. Denuault, D. Pletcher, Journal of Electroanalytical Chemistry, 633 (2009) 327. Signed: ……………………………………………………………………….. Date:……………………………………………………………………………. iii iv ACKNOWLEDGEMENTS Syukur Alhamdulilah, thank you to Allah for giving me patience and enthusiasm in achieving my wish to continue my study in the field I like most. I would like to express my sincere gratitude to my co-supervisors, Professor Derek Pletcher and Dr. Guy Denuault for their supervision, guidance, constant support and encouragement throughout my electrochemical studies in Southampton. Without their motivation and encouragement, I would not be able to finish this thesis. Special thanks to my beloved parents, Haji Mohd Yasin Bin Haji Tengah and Hajah Masnah Binti Dato Paduka Haji Abdul Wahab, for their prayers, encouragement and having confidence in whatever I do. I would like to thank my siblings, Masyati, Dr. Haji Mohd Yusni, Dr. Harliza, Dr. Nur Azri and Nur Qutrul A’ini for their motivation and moral support throughout the year. With this accomplishment, I hope I can make them proud. I also like to acknowledge the financial support received from the Brunei Government throughout the period of this work, and the help and understanding of staff at the In-service Training Department, Brunei High Commissioner and the University of Brunei Darussalam. Thank you to all my group mates; Laila, Kelly, Mohammad Aziz, Ihsin, Alicja and Jacek for being supportive in any kinds of discussions, compromising with sharing equipments and also the cooperation given in managing the lab in order to make it a welcoming place to do work. Also I should not forget to mention those who have left the group; Clélia, Maria and Jin for all their help, moral support and advice throughout this project. I also would like to thank the Bartlett and Russell groups; v Thomas, Magda, David, Maciej, Ahmet, Rob, Mohammad Ghanem, Summet, Prabalini and Gael for the friendship and the helping hands offered when needed. And not forgetting Alistair for the SEM training and providing me tips in using the SEM, and also the indirect involvement of the glassblowers in my research (especially in the fabrication of the microelectrodes). Finally, thank you to my friends, Sharina, Faizah, Dr. Ena Kartina, Hajah Sarawati and Haji Muhd Arpan for their understanding and time in listening when I need a friend to talk to. Not forgetting, Dr Hajah Noor Maya and family for their kindness and great companion whenever I feel homesick. And to those friends back home who I did not mention, my big thank you!! vi TABLE OF CONTENTS 1 Introduction ____________________________________________________ 2 1.1. Small metal centres _______________________________________________ 2 1.1.1. Applications of small centres _____________________________________________ 3 1.1.2. Effects of small size centres and distribution _________________________________ 4 1.1.3. Effects of substrate _____________________________________________________ 8 1.1.4. Various methods of preparation _________________________________________ 11 1.2. Lyotropic liquid crystals (LLC)_______________________________________ 13 1.2.1. Formation of liquid crystals _____________________________________________ 14 1.2.2. Phases of lyotropic liquid crystals _________________________________________ 16 1.2.2.1. Hexagonal phase _________________________________________________ 16 1.2.2.2. Lamellar phase ___________________________________________________ 17 1.2.2.3. Cubic phase _____________________________________________________ 18 1.2.3. Phase diagrams of the octaethylenegylcol monohexadecyl ether in water ________ 19 1.2.4. Formation of LLC template ______________________________________________ 20 1.2.5. Advantages and applications of mesoporous template _______________________ 22 1.3. Electrochemistry of noble metals ___________________________________ 23 1.3.1. Platinum ____________________________________________________________ 23 1.3.1.1. Chemistry
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