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Titanium Dioxide Coatings Obtained by Thermal Spray Technologies and Their Functional Application

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Titanium Dioxide Coatings Obtained by Thermal Spray Technologies and Their Functional Application Ciència i Tecnologia dels Materials Titanium Dioxide coatings obtained by Thermal Spray technologies and their functional application by Marc Gardon Ramos Prof. Josep Maria Guilemany i Casadamon. Centre de Projecció Tèrmica, Universitat de Barcelona, c/Martí i Franquès 1, 08028, Barcelona. Submitted to the Department of Ciència dels Materials i Enginyeria Metal·lúrgica in Partial Fulfillment of the Requirements for the Degree of Doctor at the Universiat de Barcelona. Index 0. Motivation and scope 1 1. Summary 2 2. Objectives of the thesis 8 3. Relation of papers 10 4. Introduction 14 4.1 State-of-the-art 16 4.1.1 Paper 1: 17 M. Gardon, J. M. Guilemany. Milestones in functional titanium dioxide thermal spray coatings, Journal of Thermal Spray Technology. 4.2 Metal oxide gas sensors 59 4.2.1 Paper 2: 60 M. Gardon, J. M. Guilemany. A review on fabrication, sensing mechanisms and performance of metal oxide gas sensors, Journal of Materials Science: Materials in Electronics. 5. Experimental procedures 73 5.1 Technologies 73 5.1.1 Atmospheric Plasma Spray 73 5.1.2 Cold Gas Spray 75 5.2 Characterization techniques 80 5.2.1 Characterization of powders and coatings 80 5.2.2 Factorial design of experiments 81 5.2.3 Analysis of functional coatings 82 6. Results and partial discussion 83 6.1 Atmospheric Plasma Spray 83 6.1.1 Detailed background 83 a) Irreversible transformations 83 b) Titanium sub-oxide coatings 85 6.1.2 Electrodes 89 a) Paper 3: 90 M. Gardon, J. M. Guilemany. The influence of Titanium sub-oxides in thermal sprayed coatings, International Thermal Spray Conference, Proceedings 2012. b) Paper 4: 96 M. Gardon, S. Dosta, J. M. Guilemany, M. Kourasi, B. Mellor, R. G. A. Wills. Improved, high conductivity titanium sub-oxide coated electrodes obtained by Atmospheric Plasma Spray, Journal of Power Sources. c) Paper 5: 102 M. Gardon, S. Dosta, J. M. Guilemany, M. Kourasi, B. Mellor, R. G. A. Wills. Enhanced performance of common electrodes by means of Thermal Spray coatings. 6.1.3. Gas sensors 121 a) Paper 6: 122 M. Gardon, O. Monereo, S. Dosta, G. Vescio, A. Cirera, J. M. Guilemany. New procedures for building-up the active layer of gas sensors on flexible polymers. 6.2 Cold Gas Spray 140 6.2.1 Detailed background 140 a) Starting scenario in CGS nano -TiO2 coatings 140 b )TiO2-based feedstock blends 142 6.2.2 Photocatalysts 143 a) Paper 7: 144 M. Gardon, C. Fernandez, M. Torrell, S. Dosta, J. M. Guilemany. Developing photocatalytic Copper/nano-Anatase coatings by Cold Gas Spray. b) Paper 8: 162 M. Gardon, C. Fernández, M. Torrell, S. Dosta, J. M. Guilemany. Improved photocatalytic nanostructured anatase coatings obtained by Cold Gas Spray. 6.2.3 Biomedical applications 179 a) Paper 9: 180 M. Gardon, A.Latorre, M. Torrell, S. Dosta, J. Fernández, J. M. Guilemany. Cold Gas Spray Titanium coatings onto a biocompatible polymer, Materials Letters. b) Paper 10: 184 M. Gardon, H. Melero, S. Dosta, J. M. Guilemany. Enhancing the bioactivity of polymeric implants by means of Cold Gas Spray coatings. 7. Overall discussion 206 7.1 Starting considerations 206 7.2 Atmospheric Plasma Spray 208 7.2.1 Electrodes 208 a) Coating development 208 b) Key-properties evaluation 215 c) Functional application 217 7.2.2 Flexible sensors 219 a) Coating development 219 b) Key-properties evaluation 221 c) Functional application 2 22 7.3 Cold Gas Spray 225 7.3.1 Photocatalysts 226 a) Coating development 226 b) Key-properties evaluation 231 c) Functional application 2 33 7.3.2 Biomedical applications 235 a) Coating development 235 b) Key-properties evaluation 237 c) Functional application 2 39 8. Conclusions 241 8.1 With regard to TiO2-x APS coatings 241 8 .2 With regard to CGS coatings 242 8.3 With regard to general juncture 244 9. Future trends 245 1 0. Acknowledge ments 247 11. References 248 1 1.1 Specific references 248 1 1.2 General references 250 1 2. Appendix 251 Resum 256 0. Motivation and scope Contribute to Materials Science with an intense engineering point of view is the leitmotif of this Thesis. In order to reach this challenge, it must be entailed an abiding correlation among materials involved, selected technologies and final application of the obtained product. Therefore, for undertaking this commitment and from the kick-off of this doctorate, a permanent quest of coatings that will take a functional key role in a device has nurtured the motivation of the project. Reminding that an initial problem may be solved by means of distinct alternatives; in this survey, real concerns in the industry and in our society are treated with the aim of finding straightforward and worthy solutions using Thermal Spray technologies and Titanium Dioxide feedstock. This text has been considered with the purpose that the reader will depart and land among publications but always correlated around the same concept: get profit of Thermal Spray processes and have a say in the deposition of Titanium Dioxide active layers. 1 1. Summary The main subject of this thesis is the fabrication of functional titanium dioxide coatings by means of Atmospheric Plasma Spray (APS) and Cold Gas Spray (CGS). Functional role may be understood as the capacity of TiO2 surfaces to respond in a determined way under certain conditions. This involved both the understanding of distinct technologies and the real application of the active layers in several fields. In order to gain a better comprehension about bonding mechanisms on different substrates, the interaction of this metal oxide with plasma jets, combustion flames or nitrogen streams was studied. Most significant achievements in functional Thermal Spray (TS) TiO2 coatings were reviewed so as to identify new opportunities in recognized lines of research in the last decade and revise detailed technical considerations. It was perceived remarkable occasions regarding APS titanium dioxide coatings in electrochemical applications. Moreover, depositing homogeneous nanostructured anatase layers obtained by CGS would be highly interesting for the photocatalytic degradation of contaminants and also as surface for being used in the biomedical field. The starting purpose of the doctorate consisted on developing a metal oxide gas sensor based on titanium dioxide using APS. Firstly, conventional coating processes, sensing mechanisms and overall efficiencies were deeply studied. As regards to experimental results, it was observed that H2 contained in the plasma mixture could reduce TiO2 towards non stoichiometric or stoichiometric compounds such as titanium sub-oxides (TiO2-x) or Magnéli Phases (TinO2n-1) respectively during the in-flight of the particles. Large accumulation of oxygen vacancies in the crystal lattice of rutile led to a donor level to the conduction band. Therefore, a corrosion-resistant ceramic material with a low electrical resistivity was obtained on ceramic tiles. This unexpected procedure led to deposit APS TiO2-x / TinO2n-1 coatings on stainless steel and apply them in electrochemical bi-polar batteries (Engineering and the Environment, University of Southampton). Then, from the created feedback thin stainless steel and aluminium films, carbon-polymer composites or nickel foams as common standard electrode materials were selected and coated. 2 1. Summary In all cases, coatings were well-bonded and coated pieces had an increased potential range of operation than uncoated ones. Besides, electric conductivity was boosted, which would decrease the overpotential for electrodeposition and dissolution in lead batteries. Produce the active layer of a metal oxide gas sensor using APS fed by TiO2 was still a target to be accomplished. With the aim of offering more innovation to conventional metal oxide sensors, it was determined to build-up the sensing layer on a thin polymeric flexible substrate. It was possible to reach certain spraying conditions that avoided thermal degradation of the polymer. Furthermore, heterogeneous disposition of the coating, where some areas were coated and certain spots uncoated provided electric contact between the electrodes and structure that eased elastic deformation of the film. Satisfactory performances were obtained testing the response of the device in front of a target gas (Group MIND, Universitat de Barcelona). The device had also suitable response as radiation sensor. Thenceforth, transition to thermally less-aggressive technologies was carried out. Despite some interesting possibilities raised in High Velocity Oxygen Fuel (HVOF), it was decided to focus the efforts on CGS, which does not require melting the material for being deposited. Subsequently, nanostructured anatase was used as feedstock in order to achieve photocatalytic layers with large specific surfaces for applying them in the degradation of different contaminants. It was used a powder able to create chemical bonds with the substrate and among the particles at the impact. Unfortunately, feeding system was repeatedly clogged because of the high agglomerating capacity of the powder. Blends were prepared with copper and microstructured TiO2 that flowed appropriately so as to avoid the obstruction of the pipelines. First, Cu/nano-TiO2 coatings were deposited using spraying conditions that favoured the deposition of nanostructured anatase at the top surface, which assured the development of the photocatalytic process. Samples successfully degraded toluene in gaseous phase (Universidad de Las Palmas de Gran Canaria). On the other hand, micro- TiO2/nano-TiO2 blend was not suitably deposited onto steel. Ceramic particles may not deform plastically. Thus, chemical bonds with the substrate and among particles had to be boosted for building-up the coatings. Substrate surface 3 1. Summary based on APS TiO2-x with controlled roughness provided composition, hardness and required geometry for adhering nano-TiO2 particles. In this way, CGS nano- TiO2 coatings were tested for degrading phenol and formic acid in liquid phase. The obtained results equalized or even improved the performance of sol-gel ® coatings (commercial standard P25 nano-TiO2).
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