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Thesis Has Been Carried out Under the Microcat Funding As Part of the Scientific Programme of the French National Research Agency (ANR) UvA-DARE (Digital Academic Repository) Development of catalytic microreactors by plasma processes: application to wastewater treatment Da Silva, B.T. Publication date 2015 Document Version Final published version License Other Link to publication Citation for published version (APA): Da Silva, B. T. (2015). Development of catalytic microreactors by plasma processes: application to wastewater treatment. General rights It is not permitted to download or to forward/distribute the text or part of it without the consent of the author(s) and/or copyright holder(s), other than for strictly personal, individual use, unless the work is under an open content license (like Creative Commons). Disclaimer/Complaints regulations If you believe that digital publication of certain material infringes any of your rights or (privacy) interests, please let the Library know, stating your reasons. In case of a legitimate complaint, the Library will make the material inaccessible and/or remove it from the website. Please Ask the Library: https://uba.uva.nl/en/contact, or a letter to: Library of the University of Amsterdam, Secretariat, Singel 425, 1012 WP Amsterdam, The Netherlands. You will be contacted as soon as possible. UvA-DARE is a service provided by the library of the University of Amsterdam (https://dare.uva.nl) Download date:28 Sep 2021 Development of catalytic microreactors by plasma processes: application to wastewater treatment Bradley Da Silva Development of catalytic microreactors by plasma processes: application to wastewater treatment © Bradley Timothy Da Silva. All rights reserved. The author can be reached at [email protected] The research reported in this thesis has been carried out under the MicroCat funding as part of the scientific programme of the French National Research Agency (ANR). Development of catalytic microreactors by plasma processes: application to wastewater treatment ACADEMISCH PROEFSCHRIFT ter verkrijging van de graad van doctor aan de Universiteit van Amsterdam en Université Pierre et Marie Curie op gezag van de Rector Magnificus prof. dr. D.C. van den Boom ten overstaan van een door het College voor Promoties ingestelde commissie, in het openbaar te verdedigen in de Agnietenkapel op woensdag 18 november 2015, te 16:00 uur door Bradley Timothy Da Silva geboren te Panjim, Goa, India Promotiecommissie: Promotores: Prof. dr. D. Bonn Universiteit van Amsterdam Prof.dr. M. Tatoulian Université Pierre et Marie Curie Overige leden: Prof.dr. P. Da Costa Université Pierre et Marie Curie Prof. dr. B. de Bruin Universiteit van Amsterdam Dr. R. Sprik Universiteit van Amsterdam Dr. N. F. Shahidzadeh Universiteit van Amsterdam Prof. Dr. T. Roques-Carmes Université de Nancy Faculteit der Natuurwetenschappen, Wiskunde en Informatica To my father, Froilano Da Silva Contents Contents ACKNOWLEDGMENTS ................................................................................. 11 ABSTRACT ....................................................................................................... 15 SAMENVATTING ............................................................................................ 17 RÉSUMÉ ............................................................................................................ 19 GENERAL INTRODUCTION ......................................................................... 21 CHAPTER 1: LITERATURE REVIEW ......................................................... 25 1. INTRODUCTION ........................................................................................ 25 2. MICROFLUIDIC MATERIALS, PROPERTIES AND FABRICATION TECHNIQUES ..................................................................................................... 25 2.1 Glass microreactors ....................................................................... 25 2.2 Silicon microsystems ...................................................................... 26 2.3 Polymer-based microreactors ........................................................ 27 2.4 Metal and ceramic-based microsystems ........................................ 30 3. ADVANCED OXIDATION PROCESSES ........................................................ 33 4. CATALYTIC MICROREACTORS ................................................................. 40 5. CATALYST DEPOSITION TECHNIQUES ....................................................... 43 6. CONCLUSION ........................................................................................... 46 CHAPTER 2: MATERIALS AND METHODS ............................................. 47 1. INTRODUCTION ........................................................................................ 47 2. MICROFLUIDIC MATERIALS ..................................................................... 47 3. METAL-ORGANIC PLASMA ENHANCED CHEMICAL VAPOUR DEPOSITION PROCESS ...................................................................................... 48 3.1 Description of the reactor .............................................................. 48 3.2 General procedure for the silica-like deposition ........................... 49 3.3 General procedure for the catalyst deposition ............................... 50 4. CATALYTIC OZONATION PROCESS ........................................................... 50 5. ANALYTICAL METHODS ........................................................................... 51 5.1 Surface characterizations .............................................................. 51 5.1.1 FTIR-ATR ................................................................................. 51 5.1.2 Water contact angle measurements ........................................... 52 5.1.3 X-Ray diffraction....................................................................... 54 5.2 X-ray photoelectron spectroscopy ............................................. 55 5.2.1 Scanning Electron Microscopy .................................................. 57 5.2.2 Transmission Electron Microscopy ........................................... 58 5.2.3 Specific surface area measurements .......................................... 59 5.3 Analytical methods used for the liquid phases ............................... 61 5.3.1 High Performance Liquid Chromatography .............................. 61 7 Contents 5.3.2 Flame Atomic Absorption Spectroscopy ................................... 63 5.3.3 pH-metry ................................................................................... 64 CHAPTER 3: STUDY OF THE STABILITY AND HYDROPHILICITY OF PLASMA-MODIFIED MICROFLUIDIC MATERIALS ....................... 65 1. INTRODUCTION ........................................................................................ 65 2. Materials and methods ....................................................................... 68 2.1 Chemicals .................................................................................. 68 2.2 Materials .................................................................................... 68 3. GENERAL PROCEDURE FOR THE SILICA-LIKE DEPOSITION USING PLASMA PROCESSES.......................................................................................... 69 3.1 Sputtered silica-like thin film deposition ................................... 69 3.2 Deposition of SiO2-like layer by PECVD.................................. 70 4. RESULTS AND DISCUSSION ...................................................................... 71 4.1 Aging of silica-like coated substrates using water contact angle measurements .............................................................................................. 71 4.1.1 Effect of the Ar/O2 plasma pre-treatment step ........................... 71 4.1.2 Effect of the silica-like coating .................................................. 73 4.2 Chemical composition of the silica-like modified substrates ......... 82 4.2.1 FTIR spectroscopy..................................................................... 82 4.2.2 XPS measurements .................................................................... 86 5. CONCLUSION ........................................................................................... 93 CHAPTER 4: DEVELOPMENT OF CATALYTIC MICROREACTORS: COMPARISON OF THE PERFORMANCE OF PLASMA-DEPOSITED IRON AND COBALT OXIDES IN CATALYTIC OZONATION ............................................................................ 95 1. INTRODUCTION ........................................................................................ 95 2. EXPERIMENTAL ....................................................................................... 99 2.1 Elaboration of the COC microchannels ......................................... 99 2.2 Catalysts preparation................................................................... 100 2.3 Thin films characterization .......................................................... 104 2.4 Chip Assembly.............................................................................. 106 2.5 Adsorption and catalytic activity ................................................. 106 2.6 Catalytic ozonation apparatus ..................................................... 107 2.7 HPLC and FAAS Measurements .................................................. 108 3. RESULTS AND DISCUSSION .................................................................... 109 3.1 Water stability of deposited catalysts ........................................... 109 3.2 Deposition of the cobalt oxide catalyst ........................................ 109 3.3 Deposition of the
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