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Development of Anode Catalysts for Proton Exchange Membrane Water Electrolyser

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Development of Anode Catalysts for Proton Exchange Membrane Water Electrolyser Development of anode catalysts for Proton Exchange Membrane Water Electrolyser A thesis submitted for the degree of Doctor of Philosophy by Vinod Kumar Puthiyapura Supervisor: Prof. Keith Scott School of Chemical Engineering and Advanced Materials, Newcastle University. Newcastle Upon Tyne, United Kingdom. March 2014 Abstract ii Abstract The proton exchange membrane water electrolyser (PEMWE) is a promising technology for the production of hydrogen from water. The oxygen evolution reaction (OER) has a high over potential cf. with the hydrogen evolution reaction and is one of the main reasons for the high energy demand of the electrolyser. RuO2 and IrO2 are the most active catalyst for OER, but are costly, making the electrolyser system expensive. In general, it is important to use stable, active and cheap catalysts in order to make a cost efficient electrolyser system. Supporting the active catalyst on a high surface area conducting support material is one of the approaches to reduce the precious metal loading on the electrode. Antimony tin oxide (ATO) and indium tin oxide (ITO) were studied as possible support materials for IrO2 in the PEMWE anode prepared by the Adams method. The effect of the support material on the surface area, electronic conductivity, particle size and agglomeration were investigated. The IrO2 showed highest conductivity (4.9 S cm-1) and surface area (112 m2 g-1) and decreased with the decrease in the IrO2 loading. Using the catalysts in the membrane electrode assemblies (MEA) with Nafion®-115 membranes, at 80oC showed that the catalyst with better dispersion and conductivity gave better performance. The unsupported IrO2 and 90% IrO2 supported on ATO and ITO showed the best performance among all the catalysts tested, achieving a cell -2 voltage of 1.73 V at 1 A cm . A lower IrO2 loading decreased the conductivity and surface area. The IrO2 particle size and bulk conductivity of the supported catalyst significantly influenced the MEA performance. Overall, it is important to maintain a conductive network of IrO2 on the non-conducting support to maintain the bulk conductivity and thus reduce the Ohmic potential drop. Although RuO2 is the most active catalyst for OER, it lacks stability on long term operation. RuxNb1-xO2 and IrxNb1-xO2 catalysts were synthesized and characterized, to try to develop stable electrodes for PEMWE. However the Adams method of catalyst synthesis formed a sodium–niobium complex making it unsuitable for preparation of Nb based catalysts. In both Adams and hydrolysis methods of synthesis, the addition of Nb2O5 decreased the anodic charge and electronic conductivity of the catalyst due to the dilution of the active RuO2. The RuO2 catalyst showed the best performance in MEA evaluation compared to the bimetallic catalyst (1.62 V and 1.75 V @1 A cm-2 for ii Abstract iii RuO2(A) and RuO2(H) respectively). A higher stability for bimetallic catalyst compared to the monometallic catalysts was obtained from the continuous CV cycling and MEA stability test. iii Acknowledgement iv Acknowledgement It has been a wonderful journey which is reaching an end. There are many without whom this thesis would have never finished. First of all I would like to express my sincere gratitude to my supervisor Prof. Keith Scott for all his guidance and support which helped me to finish the thesis on time. I also express my gratitude to EPSRC for the financial support for my PhD project. I am deeply thankful to Dr. Mohammed Mamlouk (Moodie) for his invaluable help, support and guidance during all these three years. You have been a great mentor all these years. I am also grateful to all fuel cell group members- both past and present members- Dr. Senthil Kumar, Aris (Georgios), Xu Wu, Anca Dumitru, Asier, Ukrit (One), Ryan (Xu Wang), Georgina, Chenxi Xu (Paul), Ravikumar, Lei Xing (Chris), Luke Watkins, Terence (Xiaoteng Liu), Taiwo, Cao and Kemi for being such warm and friendly co-workers. I would also like to express my sincere gratitude to Dr. Sivakumar Pasupathi and Prof. Bruno Pollet (HySA, University of Western Cape, South Africa) for their guidance and support during my stay in South Africa. Thanks to Huaneng Su, BJ Brown, Piotr Bujlo, Basheley and Joris for your help, support and fun at HySA. I cannot forget all the wonderful days in South Africa. I would like to express my sincere thanks and love to Sadiq Ali (Thirumeni), Ramesh Nepalli and Pritesh Sinha for making my stay in South Africa a memorable experience. I would like to express my gratitude to Prof. Basu (IIT Delhi, India) for his supervision during my visit at IIT-Delhi, India. I am thankful to Varagunapandiyan, Pankaj Tiwari, Pawan kumar, Jyothsna Annepu, Rajalekshmi, Shashank sood and Sundar singh for their help and support during my stay at IIT-Delhi. I am also thankful to all the technical and office staff at CEAM for their great support all these years. My special thanks to Maggie and Pauline Carrick for the XRD and SEM analysis. Also, I would like to express my gratitude to all my dear friends in Newcastle who gave me wonderful memories in these 3 years of my life. Thanks Balamurugan, Abhijay Awasthi, Nutthapaon (Tom), Roney Joseph (Thirumeni), Vivek Dodduraj, Vineeth iv Acknowledgement v Thoonoli, Nicolas (Nick), Ela, Simona Tibuloca, Rahul JP and Gayathri (Aishu). Thanks for all the fun! I would also like to express my thanks to my dear friends for their support and for always being with me during the good and bad days. Thanks Jamsad Mannuthodukayyil, Midhun Chandran, Meera Mohan, Tharun Jose and Lishil Silvester (Arnold). Finally, I would like to thank my parents and brother for all their love, support and encouragement during the hard days. v Table of contents vi Table of contents Abstract .................................................................................................................... ii Acknowledgement ................................................................................................... iv Table of contents ..................................................................................................... vi List of Figures ........................................................................................................... x List of Tables .......................................................................................................... xiv Symbols .................................................................................................................. xv Abbreviations ........................................................................................................ xvi 1 Chapter-1. Introduction and objective ............................................................... 1 1.1 Hydrogen economy ..................................................................................................... 1 1.2 Hydrogen production. ................................................................................................. 2 1.2.1 Thermal process of hydrogen production ............................................................... 3 1.2.2 Photolytic hydrogen production ............................................................................. 4 1.2.3 Electrolytic hydrogen production ............................................................................ 4 1.3 History of water electrolysis ........................................................................................ 5 1.4 Theory of water electrolysis ........................................................................................ 7 1.5 Types of water electrolysers ...................................................................................... 11 1.5.1 Alkaline water electrolyser.................................................................................... 11 1.5.2 Solid oxide water electrolyser ............................................................................... 13 1.5.3 Proton exchange membrane water electrolyser .................................................. 14 1.6 Electrocatalysts for PEMWE ...................................................................................... 18 1.6.1 Oxygen evolution reaction (OER) .......................................................................... 18 1.6.2 Hydrogen evolution reaction (HER) ...................................................................... 22 1.7 Objective of the thesis ............................................................................................... 23 2 Chapter-2. Experimental .................................................................................. 25 2.1 Synthesis of the catalyst ............................................................................................ 25 2.1.1 Adams fusion method ........................................................................................... 25 2.1.2 Hydrolysis method ................................................................................................ 27 2.2 Physical Characterization........................................................................................... 28 2.2.1 X-ray diffraction..................................................................................................... 28 2.2.2 X-ray photoelectron spectroscopy (XPS) ............................................................... 31 vi Table of contents vii 2.2.3 Scanning electron microscopy (SEM) .................................................................... 33 2.2.4 Energy dispersive X-ray technique (EDX) .............................................................
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