Wind power will play a major role in the future energy system in Sweden. Most of the major wind parks are planned to be built in sites where the cold climate and atmospheric icing can cause serious problems. This underlines the importance of addressing these issues. The major cause of these problems is in-cloud icing of the rotor blades due to super cooled liquid droplets of clouds. The droplets freeze upon impact with the rotor blade and form hard rime ice. This rime ice causes disruption in the aerodynamics that leads to production losses, extra loads on the rotor blades and when the ice is shed it poses a safety risk to people in the near environment. This master thesis focuses on how to measure the accretion of ice and the correlation between measured ice and production losses of two wind parks in northern Sweden.   The results show a good correlation between the ice accretion on a stationary sensor and the production loss from a wind turbine. In most icing events the icing of the sensor and large production losses from the wind turbine correlated clearly. Attempts to quantify the production losses at a certain ice rate measured with the stationary sensors was done, however no clear results was produced. The reason for this is that the wind turbines often stop completely during an icing event and that the time series analyzed was too short to be able to quantify the losses at certain wind speed and ice rates.   Recommendations on the type of sensor which should be used was to be produced, however the conclusion was that no single sensor has acted satisfactory and could be recommended to measure ice accretion for wind turbine applications. Due to this, at least two sensors are recommended to increase the redundancy in the measurement system. Modeling ice accretion with standard parameters measured has been done and the results show that the time of icing could be determined quite well when the sensors was ice free, however when the sensors and especially the humidity sensors was iced the time of icing was overestimated.   The main conclusion drawn is that there is a clear relationship between the icing of a stationary sensor and the rotor blade. There is still no which fulfills all demands of measuring ice accretion for wind turbine applications, further it is possible with simple models to roughly determine when icing occurs with standard measurements.

Nowadays, the energy sector is facing a huge demand that needs to be covered. Wind energy is one of the most promising energy resources as it is free from pollution, clean and probably will arise as one of the main energy sources to prevent global warming from happening. Almost 10% of the global energy demand is coming from renewable resources. By 2050 this percentage is expected to grow to 60%. Therefore, efforts on wind turbine technology (i.e. reliability, design…) need to be coped with this growth. Currently, large wind energy projects are usually carried out in higher altitudes and cold climates. This is because almost all of the cold climates worldwide offer profitable wind power resources and great wind energy potential. Operating with wind turbines in cold climates bring interesting advantages as a result of higher air density and consequently stronger winds (wind power is around 10% higher in the Nordic regions). Not only benefits can be obtained but extreme conditions force to follow harsh conditions. Low temperatures and ice accretion present an important issue to solve as can cause several problems in fatigue loads, the balance of the rotor and aerodynamics, safety risks, turbine performance, among others. As wind energy is growing steadily on icy climates is crucial that wind turbines can be managed efficiently and harmlessly during the time they operate. The collected data for the ice detection, de-icing and anti-icing systems parts was obtained through the company Arvato Bertelsmann and is also based on scientific papers. In addition, computer simulations were performed, involving the creation of a wind tunnel under certain conditions in order to be able to carry out the simulations (1st at 0ºC, 2nd at -10ºC) with the turbine blades rotating in cold regions as a standard operation. In this project, Computational Fluids Dynamics (CFD) simulation on a 5MW wind turbine prototype with ice accretion on the blades to study how CL and CD can change, also different measures of ice detection, deicing and anti-icing systems for avoiding ice accumulation will be discussed. Simulation results showed a logical correlation as expected, increasing the drag force about 5.7% and lowering the lift force 17,5% thus worsening the turbine's efficiency.

Das unerwünschte Aufwachsen oder Anhaften von Eis an z.B. Windenergieanlagen und Wärmetauschern kann zum Funktionsverlust oder zur temporären Stilllegung der gesamten technischen Anlage führen. Bekannte Abwehrmechanismen sind das aktive Beheizen der Oberflächen oder der Einsatz von Enteisungschemikalien. Um den Verbrauch der hierfür benötigten elektrischen Energie oder Enteisungsmittel zu minimieren, werden in zunehmendem Maß passive Oberflächenbeschichtungen zur Gefrierverzögerung und Adhäsionsminimierung entwickelt. Der Einsatz pyroelektrischer Materialien bietet einen Lösungsansatz, der über bisher bekannte Abwehrstrategien hinausgeht. Es wird angenommen, dass pyroelektrisch generierte Oberflächenladungen während der Abkühlung entweder förderlich oder verzögernd auf die Eiskeimbildung wirken können. Dünne Schichten aus pyroelektrischem Poly-(Vinylidenfluorid - co - Trifluorethylen) haben wegen ihrer leichten Verarbeitbarkeit, hohen Flexibilität und pyroelektrischen Eigenschaften Interesse an ihrer Anwendung als funktionelle Beschichtung geweckt. Für eine industrielle Anwendung von P(VDF-TrFE) ist jedoch ein vertieftes Verständnis darüber erforderlich, wie sich der Beschichtungsprozess auf die resultierende Kristallinität, kristallographische Orientierung und Rauheit auswirkt. Die Morphologie teilkristalliner P(VDF-TrFE)-Beschichtungen wurde in dieser Arbeit in Abhängigkeit der Beschichtungsmethode, des Lösungsmittels, der Schichtdicke und der Wärmebehandlung mithilfe von Röntgenweitwinkelstreuung, Röntgenreflektometrie und Infrarot-Reflexions-Absorptions-Spektroskopie untersucht. Mit Hilfe von Rasterkraftmikroskopie- und Kontaktwinkel-Messungen wurden die resultierende Topographie und Rauheit der Schichten überprüft. Auf Grundlage der Ergebnisse dieser Messungen kann die dominierende edge-on Orientierung der P(VDF-TrFE)-Polymerketten entweder mit einem transkristallin-artigen Mechanismus oder Konfinement-Effekten erklärt werden. An den P(VDF-TrFE)-Dünnschichten wurde eine Vielzahl von Vereisungsexperimenten mit aufliegenden Wassertropfen durchgeführt, um den Einfluss der verschiedenen Schichtparameter wie Polarisierungsrichtung, Schichtdicke, verwendetes Lösungsmittel, Beschichtungstechnologie, Substrat und Wärmebehandlung auf die erreichbare Gefrierverzögerung unabhängig voneinander zu ermitteln. Die Rauheit der Schichten sowie substratspezifische Entnetzungserscheinungen veränderten hierbei signifikant die Verteilung der Gefriertemperaturen von Wassertropfen in Kontakt mit den P(VDF-TrFE)-Dünnschichten. Im Gegensatz dazu wurde kein signifikanter Einfluss der Dicke, Morphologie oder des pyroelektrischen Effekts auf die erreichbare Gefrierverzögerung gefunden. Es kann demnach geschlussfolgert werden, dass die heterogene Eiskeimbildung stärker durch lokale Rauheiten im nm-Bereich beeinflusst wird als durch integrale Eigenschaften wie beispielsweise Oberflächenladungen. Die Eisadhäsion auf P(VDF-TrFE) wird hauptsächlich durch Rauheiten im µm-Bereich, die Umgebungstemperatur und den Ionengehalt der flüssigen Phase bestimmt. Auch hier konnte kein signifikanter Einfluss geladener Oberflächen auf die Haftfestigkeit von Eis ausfindig gemacht werden. Statistische Tests ergaben, dass die Verteilung der Gefriertemperaturen unabhängiger Tropfen auf Oberflächen einem Spezialfall der Extremwertstatistik, der so genannten Gumbel-Verteilung, entspricht. Dies ermöglicht die Definition neuartiger Temperaturkennwerte für die Weiterentwicklung und Prüfung von Anti-Eis-Oberflächen.:Inhaltsverzeichnis 1. Einleitung und Motivation 2. Stand der Forschung 2.1. Pyroelektrika 2.1.1. Der pyroelektrische Effekt 2.1.2. Pyroelektrische Werkstoffe 2.1.3. Stabilität pyroelektrischer Materialien in wässrigen Medien 2.1.4. PVDF und P(VDF-TrFE) 2.2. Elektrochemische Doppelschicht 2.2.1. Aufbau und Modelle 2.2.2. Ursachen für Ladungen an Grenzflächen 2.2.3. Isoelektrischer Punkt und Ladungsnullpunkt 2.2.4. Orientierung von Wassermolekülen in der EDL 2.3. Vereisung 2.3.1. Wasser und Eis 2.3.2. Anti-Eis Strategien 2.3.3. Gefrierverzögerung 2.3.4. Eisadhäsion 2.4. Pyroelektrika in wässrigen Medien 2.4.1. Charakterisierungsmöglichkeiten 2.4.2. Anwendungsfelder 3. Materialien und Methoden 3.1. Materialien 3.2. Herstellung pyroelektrischer Beschichtungen 3.3. Schichtcharakterisierung 3.4. Vereisungsneigung 3.5. Statistische Methoden 4. Ergebnisse 4.1. Charakterisierung der P(VDF-TrFE) Beschichtungen 4.1.1. Schichtdicke (Ellipsometrie) und mechanische Eigenschaften 4.1.2. Morphologie (DSC, GIWAXS, XRR, IRRAS) 4.1.3. Elektrische Eigenschaften 4.1.4. Topographie (AFM und Kontaktwinkel) 4.2. Vereisungsneigung von P(VDF-TrFE) 4.2.1. Gefrierverzögerung 4.2.2. Eisadhäsion 4.3. Vergleichsmessungen auf poliertem Aluminium 4.3.1. Kontaktwinkel 4.3.2. Gefrierverzögerung 4.3.3. Eisadhäsion 5. Diskussion 5.1. Schichtherstellung, -charakterisierung und -eignung 5.1.1. Schichtdicke 5.1.2. Eignung der Charakterisierungsmethoden 5.1.3. Vergleich von Dip- und Spin-Coating 5.1.4. Eignung von P(VDF-TrFE) für Anti-Eis-Beschichtungen 5.2. Anti-Eis-Eigenschaften 5.2.1. Erreichbare Gefrierverzögerung 5.2.2. Eisadhäsion 6. Zusammenfassung und Ausblick Literaturverzeichnis Abbildungsverzeichnis Tabellenverzeichnis Symbol- und Abkürzungsverzeichnis Veröffentlichungen Anhang / Active de-icing of technical surfaces, such as for wind turbines and heat exchangers, currently requires the usage of heat or chemicals. Passive coating strategies that either postpone the freezing of covering water droplets or lower the ice adhesion strength would be beneficial in order to save costs and energy. One hypothesis is that pyroelectric active materials can either delay or promote heterogeneous ice nucleation because of the surface charges generated when these materials are subject to a temperature change. Pyroelectric poly-(vinylidene fluoride - co - trifluoroethylene) P(VDF-TrFE) thin films have created interest in their application because of their easy processibility, high flexibility and ferroelectric properties. The industrial application of P(VDF-TrFE) requires an understanding of the deposition process of films and in particular the resulting crystallinity, crystallographic orientation and roughness. In this work it has been proposed that an interface-mediated crystallization process occurs when P(VDF-TrFE) thin films are deposited from a solvent, resulting in a dominantly edge-on orientation caused either by a transcrystallinity mechanism or confinement effect. The morphology of the semi-crystalline thin film was studied as a function of the deposition method, solvent, film thickness and annealing temperature by grazing incidence wide-angle X-ray scattering, X-ray reflectometry and infrared reflection absorption spectroscopy. Atomic force microscopy measurements were used to examine the resulting topography and contact angle measurements to additionally verify the low roughness of the coatings. Freezing experiments with water droplets subjected to a cooling rate of 1K/min were made on P(VDF-TrFE) coatings in order to separate the effect of the different film parameters such as the poling direction, film thickness, used solvent, deposition process, underlying substrate and annealing temperature on the achievable supercooling. The topography and substrate-specific dewetting effects significantly changed the distribution of freezing temperatures of water droplets in contact with the P(VDF-TrFE) thin films. In contrast, no significant effect of the thickness, morphology or pyroelectric effect of the as-prepared domain-state on the freezing temperatures was found. Statistical tests revealed that the distribution of freezing temperatures of individual droplets deposited on surfaces match a special case of extreme-value statistics, the so-called Gumbel-distribution. This allows for the definition of novel parameters for the development and testing of anti-icing surfaces. The adhesion strength of ice to P(VDF-TrFE) is mainly determined by the topography, temperature and ion-content of the liquid phase. In contrast, surface charges do not significantly influence the ice adhesion strength.:Inhaltsverzeichnis 1. Einleitung und Motivation 2. Stand der Forschung 2.1. Pyroelektrika 2.1.1. Der pyroelektrische Effekt 2.1.2. Pyroelektrische Werkstoffe 2.1.3. Stabilität pyroelektrischer Materialien in wässrigen Medien 2.1.4. PVDF und P(VDF-TrFE) 2.2. Elektrochemische Doppelschicht 2.2.1. Aufbau und Modelle 2.2.2. Ursachen für Ladungen an Grenzflächen 2.2.3. Isoelektrischer Punkt und Ladungsnullpunkt 2.2.4. Orientierung von Wassermolekülen in der EDL 2.3. Vereisung 2.3.1. Wasser und Eis 2.3.2. Anti-Eis Strategien 2.3.3. Gefrierverzögerung 2.3.4. Eisadhäsion 2.4. Pyroelektrika in wässrigen Medien 2.4.1. Charakterisierungsmöglichkeiten 2.4.2. Anwendungsfelder 3. Materialien und Methoden 3.1. Materialien 3.2. Herstellung pyroelektrischer Beschichtungen 3.3. Schichtcharakterisierung 3.4. Vereisungsneigung 3.5. Statistische Methoden 4. Ergebnisse 4.1. Charakterisierung der P(VDF-TrFE) Beschichtungen 4.1.1. Schichtdicke (Ellipsometrie) und mechanische Eigenschaften 4.1.2. Morphologie (DSC, GIWAXS, XRR, IRRAS) 4.1.3. Elektrische Eigenschaften 4.1.4. Topographie (AFM und Kontaktwinkel) 4.2. Vereisungsneigung von P(VDF-TrFE) 4.2.1. Gefrierverzögerung 4.2.2. Eisadhäsion 4.3. Vergleichsmessungen auf poliertem Aluminium 4.3.1. Kontaktwinkel 4.3.2. Gefrierverzögerung 4.3.3. Eisadhäsion 5. Diskussion 5.1. Schichtherstellung, -charakterisierung und -eignung 5.1.1. Schichtdicke 5.1.2. Eignung der Charakterisierungsmethoden 5.1.3. Vergleich von Dip- und Spin-Coating 5.1.4. Eignung von P(VDF-TrFE) für Anti-Eis-Beschichtungen 5.2. Anti-Eis-Eigenschaften 5.2.1. Erreichbare Gefrierverzögerung 5.2.2. Eisadhäsion 6. Zusammenfassung und Ausblick Literaturverzeichnis Abbildungsverzeichnis Tabellenverzeichnis Symbol- und Abkürzungsverzeichnis Veröffentlichungen Anhang

Icing on materials surface causes operational failures as well as technical and safety issues. Furthermore, it reduces the energy efficiency of the power supply and passenger/freight transportation systems. Conventional active deicing methods are widely used to remove ice, but are often associated with uneconomically high energy consumption and high maintenance costs, often not being aware of their environmental impact. Instead, passive anti-icing methods are being sought to prevent or delay ice formation by means of physico-chemical surface treatment. Pyroelectric materials can be used as possible anti-icing surfaces after their ability to inhibit ice nucleation has been experimentally demonstrated. This makes use of the effect of the pyroelectrically induced surface charge, which changes with the ambient temperature and thus, hypothetically, exerts an influence on the dipole orientation of the water molecules at the surface. This is expected to affect the hydrogen bonding network of the interfacial water in the supercooled liquid phase, depending on the sign of surface charge. However, the Classical Nucleation Theory predicts an increased nucleation rate with increasing electric field strength of the pyroelectric surface charge irrespective of its polarity, as confirmed by many experiments. This raises the question of what exactly influences the ice nucleation. The main purpose of this thesis is to find a relationship between the pyroelectricity and the ice nucleation rate. Various theoretical and experimental investigation methods have been used to examine which of the possible influencing factors related to the pyroelectric material surface plays a major role in promoting or inhibiting ice nucleation.:Contents Abstract i List of figures xi List of tables xv 1 Introduction 1 1.1 Motivation 1 1.2 Objective and Tasks 4 1.3 Structure of the thesis 6 2 Basics 7 2.1 Pyroelectric materials 7 2.1.1 Fundamental properties 7 2.1.2 Lithium niobate, LiNbO3 14 2.2 Ice nucleation and water freezing 21 2.2.1 Thermodynamics of ice nucleation 21 2.2.2 Factors influencing ice nucleation 26 3 Materials and Methods 29 3.1 Sample materials used for the investigation 29 3.2 Theoretical methods 31 3.2.1 Theoretical background of computational quantum mechanical modeling 31 3.2.2 LiNbO3 model system 38 3.2.3 DFT implementation in CP2K 41 3.3 Experimental methods 42 3.3.1 Optical and vibrational spectroscopy 43 3.3.2 X-ray spectroscopy 47 3.3.3 Atomic force microscopy 48 3.3.4 Environmental scanning electron spectroscopy 51 3.3.5 Pyroelectric measurement 52 3.3.6 Contact angle measurement 53 3.3.7 Icing temperature measurement 54 3.4 Tabular overview of the different methods 57 ix4 Results and Discussion 59 4.1 Results 59 4.1.1 Several results of DFT calculations 59 4.1.2 MD simulations of interfacial water 75 4.1.3 Results of optical and vibrational spectroscopy 80 4.1.4 X-ray spectroscopy on LiNbO3 surfaces 96 4.1.5 Extended treatment of the Classical Nucleation Theory 100 4.1.6 Results of atomic force microscopy 108 4.1.7 ESEM images of ice crystals grown on LiNbO3 116 4.1.8 Results of pyroelectric measurements 122 4.1.9 Results of contact angle measurements 124 4.1.10 Results of icing temperature measurements 126 4.2 Discussion 135 4.2.1 Surface charge 135 4.2.2 Surface structure 144 4.2.3 Surface reactivity 149 4.3 Conclusion of the findings and remarks 151 5 Summary and Outlook 157 5.1 Conclusion of the thesis 157 5.2 Recommendations for further investigations 161 5.3 Outlook 164 Appendix 167 A.1 Additional information to the DFT calculations 167 A.2 Background spectrum for ATR spectroscopy 175 A.3 Additional information to SFG/SHG spectroscopy 176 A.4 Additional information to the XPS results 181 A.5 Additional information to the AFM measurement 182 A.6 ESEM images of ice accretion in the sample system 187 A.7 FEM simulation of local temperature and flow velocity distribution 190 A.8 Additional information to the icing temperature measurement 203 A.9 Temperature-dependent pH variation of water at LiNbO3 surface 207 List of abbreviations and symbols 213 References 217 Publications 276 Acknowledgements 277 Erklärung 281 / Vereisung auf Werkstoffoberflächen führt einerseits zu Betriebsausfällen und andererseits zur Reduzierung der Energieeffizienz von Energieversorgungs- sowie Personen- und Gütertransportsystemen. Sie stellt nicht selten ein sicherheitstechnisches und gesundheitliches Risiko dar. Da die konventionellen aktiven Enteisungsmethoden mit hohem Energieaufwand und hohen Wartungskosten verbunden sind, wird nach passiven Anti-icing-Methoden als vorbeugende Maßnahmen zur Vermeidung/Verzögerung von Eisbildung auf physikalisch-chemisch behandelten Oberflächen gesucht. Der Einsatz dieser Werkstoffoberflächen senkt nicht nur den Energieverbrauch, sondern soll auch die Umwelt schonen. Pyroelektrische Materialien kommen als passive Anti-icing-Oberflächen in Frage, nachdem ihre eiskeimbildungshemmende Fähigkeit experimentell nachgewiesen wurde. Dabei wird der Effekt der pyroelektrisch induzierten Oberflächenladung ausgenutzt, die sich mit der Umgebungstemperatur ändert und somit, hypothetisch gesehen, einen Einfluss auf die Dipolorientierung der Wassermoleküle an der Oberfläche ausübt. Das hat je nach Vorzeichen der Oberflächenladung Auswirkungen auf das Wassermolekülbindungsnetzwerk des Grenzflächenwassers in der unterkühlten flüssigen Phase. Da die klassische Keimbildungstheorie jedoch eine erhöhte Keimbildungswahrscheinlichkeit mit zunehmender Stärke des elektrischen Feldes der pyroelektrischen Oberflächenladung unabhängig von ihrem Vorzeichen voraussagt, wie es ebenfalls in vielen Experimenten nachgewiesen wurde, stellt sich die Frage, was genau die Eiskeimbildung beeinflusst. Das Hauptanliegen dieser Arbeit ist, einen Zusammenhang zwischen der Pyroelektrizität der Oberfläche und der Eiskeimbildungsrate zu finden. Mithilfe einer Vielzahl von verschiedenen theoretischen und experimentellen Methoden wird untersucht, welcher der möglichen Einflussfaktoren im Zusammenhang mit der pyroelektrischen Materialoberfläche eine große Rolle bei der Eiskeimbildung spielt.:Contents Abstract i List of figures xi List of tables xv 1 Introduction 1 1.1 Motivation 1 1.2 Objective and Tasks 4 1.3 Structure of the thesis 6 2 Basics 7 2.1 Pyroelectric materials 7 2.1.1 Fundamental properties 7 2.1.2 Lithium niobate, LiNbO3 14 2.2 Ice nucleation and water freezing 21 2.2.1 Thermodynamics of ice nucleation 21 2.2.2 Factors influencing ice nucleation 26 3 Materials and Methods 29 3.1 Sample materials used for the investigation 29 3.2 Theoretical methods 31 3.2.1 Theoretical background of computational quantum mechanical modeling 31 3.2.2 LiNbO3 model system 38 3.2.3 DFT implementation in CP2K 41 3.3 Experimental methods 42 3.3.1 Optical and vibrational spectroscopy 43 3.3.2 X-ray spectroscopy 47 3.3.3 Atomic force microscopy 48 3.3.4 Environmental scanning electron spectroscopy 51 3.3.5 Pyroelectric measurement 52 3.3.6 Contact angle measurement 53 3.3.7 Icing temperature measurement 54 3.4 Tabular overview of the different methods 57 ix4 Results and Discussion 59 4.1 Results 59 4.1.1 Several results of DFT calculations 59 4.1.2 MD simulations of interfacial water 75 4.1.3 Results of optical and vibrational spectroscopy 80 4.1.4 X-ray spectroscopy on LiNbO3 surfaces 96 4.1.5 Extended treatment of the Classical Nucleation Theory 100 4.1.6 Results of atomic force microscopy 108 4.1.7 ESEM images of ice crystals grown on LiNbO3 116 4.1.8 Results of pyroelectric measurements 122 4.1.9 Results of contact angle measurements 124 4.1.10 Results of icing temperature measurements 126 4.2 Discussion 135 4.2.1 Surface charge 135 4.2.2 Surface structure 144 4.2.3 Surface reactivity 149 4.3 Conclusion of the findings and remarks 151 5 Summary and Outlook 157 5.1 Conclusion of the thesis 157 5.2 Recommendations for further investigations 161 5.3 Outlook 164 Appendix 167 A.1 Additional information to the DFT calculations 167 A.2 Background spectrum for ATR spectroscopy 175 A.3 Additional information to SFG/SHG spectroscopy 176 A.4 Additional information to the XPS results 181 A.5 Additional information to the AFM measurement 182 A.6 ESEM images of ice accretion in the sample system 187 A.7 FEM simulation of local temperature and flow velocity distribution 190 A.8 Additional information to the icing temperature measurement 203 A.9 Temperature-dependent pH variation of water at LiNbO3 surface 207 List of abbreviations and symbols 213 References 217 Publications 276 Acknowledgements 277 Erklärung 281

This study aims to develop coatings which show wear resistant behaviour along with multiple functions such as improved ice adhesion, better freezing delay etc which help in improving the effectiveness of the wind turbine efficiency. The significance of anti-icing/de-icing solutions for wind turbines is emphasized since ice accretion can cause serious issues in generation of power and might lead to damage of blades. The use of active and passive anti-icing/de-icing technologies in wind turbine blade applications is reviewed. The discrepancy between passive anti-icing, which depends on surface treatment, coatings, de-icing fluids and active anti-icing, which uses heating devices, sensors such as actuators, transducers, is explored along with the current challenges in industry. In this study we’ve developed interesting methods for improving the anti-icing/de-icing capabilities of wind turbine blades by using gelcoat coatings in which are filler particles (boron nitride and graphene) and oils (vegetable and paraffin oil) are incorporated. Evaluating the impacts of type of fillers, oils, their concentrations on anti-icing efficacy, as well as the prospects for this technique to enhance wind energy production's reliability and productivity will be explored. In summary, this study aims to develop multi-functional polymer coatings for anti-icing/de-icing application in wind turbine blades. The coatings with boron-nitride and graphene showed an increase in the surface roughness and contact angles, while there’s no change in the chemical composition in comparison with pure gelcoat. The thermal conductivity of the coatings was increased with addition of fillers. For the wear test, the operating parameters chosen are a load of 5N and 1Hz frequency of slider, which is run for a duration of 10 min. The COF for both the coatings is lesser than baseline coatings whereas graphene provided better wear resistance. The hardness was increased for boron-nitride coatings and it remained almost same for graphene coatings. The ice adhesion strength, freezing delay and thermal analysis (TGA) for these coatings showed better performance than pure gelcoat. Whereas for coatings with vegetable and paraffin oils, the contact angles were increased and surface roughness was increased in case of paraffin oil coatings whereas it reduced for vegetable oil coatings. Both the coatings offered better wear resistance and reduced COF, whereas the hardness was reduced. The ice adhesion strength and freezing delay improved drastically and are much better than both pure gelcoat as well as coatings with boron-nitride and graphene. There is slight increase in the glass transition temperature than pure gelcoat coating.

No description available.

Icing severely affects society, especially in the Nordic countries. Iceaccumulation can result in critical performance problems and safetyconcerns for instance in road, air and sea transportation, transmissionlines, marine and offshore structures, wind turbines and heat exchangers.Present active ice-combating approaches possess environmental,efficiency and cost drawbacks. Thus, fabricating icephobic surfaces orcoatings impeding ice formation (anti-icing), but facilitating ice removal(de-icing) is desired. However, different conditions in the environmentduring ice formation and growth add to the complexity of the problem.An icephobic surface that works for a certain application might not be agood candidate for another. These surfaces and the challenges are infocus in this thesis.Wetting properties are important for ice formation on surfaces fromthe liquid phase (often supercooled water), where the water repellency ofthe surfaces could enhance their anti-icing effect. Considering this,different hydrophobic and superhydrophobic surfaces with differentchemistry, morphology and roughness scale were prepared. Since anyinduced wetting state hysteresis on hydrophobic surfaces could influencetheir performance, the wetting stability was investigated. In particulardynamic wetting studies of the hydrophobic surfaces revealed whatsurface characteristics benefit a stable wetting performance. Further, theeffect of temperature, particularly sub-zero temperatures, on the wettingstate of flat and nanostructured hydrophobic surfaces was investigated.This was complemented with studies of the wetting stability of sessilewater droplets on flat to micro- and multi-scale (micro-nano) roughhydrophobic samples in a freeze-thaw cycle. To be consistent with mostapplications, all temperature-controlled experiments were performed inan environmental condition facilitating frost formation. Further, antiicingproperties of hydrophobic surfaces with different topography butsimilar chemistry were studied by freezing delay measurements.A dynamic wetting study using hydrophobic samples with similarchemistry but different topography revealed that multi-scale roughnesscould benefit the wetting stability. However, when these surfaces areutilized at low temperatures the wetting hysteresis observed during acooling/heating cycle is significant. Such a temperature-inducedhysteresis is also significant on superhydrophobic surfaces. I attributethis to condensation followed by frost formation facilitating spreading of  the supercooled water droplet. The freezing delay measurementsdemonstrate no significant effect of surface topography on anti-icingproperties of hydrophobic surfaces, however the flat surfaces showed thelongest delay. These findings are in agreement with heterogeneous icenucleation theory, suggesting preferential ice nucleation in concave sites,provided they are wetted.In the second part of this thesis, I consider the findings from theprevious part illustrating the limitations of (super)hydrophobic surfaces.The de-icing properties of hydrophilic surfaces with a hydration waterlayer, hypothesized to lubricate the interface with ice, were studied. Heretemperature-controlled shear ice adhesion measurements, down to -25oC, were performed on an adsorbed layer of a polymer, either bottle-brushstructured poly(ethylene oxide) or linear poly(ethylene oxide). The iceadhesion strength was reduced significantly on the bottle-brushstructured polymer layer, specifically at temperatures above -15 oC,whereas less adhesion reduction was observed on the layer formed by thelinear polymer. These findings are consistent with differential scanningcalorimetry (DSC) data, demonstrating that the hydration water, boundto the bottle-brush structured polymer, is in the liquid state at thetemperatures where de-icing benefit is observed. Further, continuingwith the hypothesis of the advantage of surfaces with a natural lubricantlayer for de-icing targets, I studied shear ice adhesion on the molecularlyflat basal plane of hydrophilic mica down to -35 oC. Interestingly, ultralowice adhesion strength was measured on this surface. I relate this to theproposed distinct structure of the first ice-like but fluid water layer onmica, with no free OH groups, followed by more bulk liquid-like layers.This combined with the molecularly smooth nature of mica results in aperfect plane for ice sliding. / Isbildning har en stark inverkan på samhället, speciellt i de nordiskaländerna. Isuppbyggnad kan resultera i kritiska prestandaproblem ochsäkerhetsrisker inom t.ex. väg-, luft-, och sjötransport, kraftledningar,marina- och offshorestrukturer, vindkraftverk och värmeväxlare.Nuvarande aktiva isbekämpningsmetoder uppvisar brister i avseende påmiljö, effektivitet och kostnad. Det finns därmed ett behov av attframställa ytor eller ytbeläggningar som förhindrar isbildning (antiisning)eller underlättar borttagandet av redan bildad is (avisning). Dockkompliceras problemet av de många olika förhållanden under vilka is kanbildas. En beläggning som fungerar för en viss tillämpning behöver intenödvändigtvis vara en bra kandidat för en annan. Dessa ytor ochutmaningar relaterade till dem är i fokus i denna avhandling.Vätningsegenskaper är viktiga för isbildning på ytor från vätskefas(ofta underkylt vatten), och det har visats att vattenavstötande ytor i vissasammanhang kan motverka isbildning. Med detta i åtanke framställdesolika hydrofoba och superhydrofoba ytor, med varierande kemi,morfologi och ytråhet. Eftersom en förändring i de hydrofoba ytornasvätningsegenskaper kan påverka deras funktion studerades vätningsstabilitetenför dessa ytor. I synnerhet dynamiska vätningsstudier av dehydrofoba ytorna avslöjade vilka ytegenskaper som är fördelaktiga förvätningsstabiliteten. Vidare studerades hur temperaturen, särskilt undernoll grader, påverkar vätningstillståndet på släta och nanostruktureradehydrofoba ytor. Arbetet kompletterades med studier av vätningsstabilitetenför vattendroppar på släta samt mikro- och multistrukturerade(mikro-nano) hydrofoba ytor under flera frysningsupptiningscykler.För att vara i linje med de flesta tillämpningar, utfördesalla temperaturkontrollerade mätningar i en miljö där frost kunde bildaspå ytorna. Anti-isegenskaperna hos de hydrofoba ytorna med varierandetopografi men samma kemi studerades vidare genom att studera hur långtid det dröjde innan en vattendroppe på ytan fryste vid en visstemperatur.De dynamiska vätningsstudierna på hydrofoba ytor med samma kemimen olika topografi avslöjade att en ytråhet på flera längdskalor kan haen positiv inverkan på vätningsstabiliteten. När dessa ytor är exponeradeför låga temperaturer är dock vätningshysteresen under en nedkylnings-/uppvärmnings-cykel significant. Den temperatur-inducerade hysteresenär också betydande för superhydrofoba ytor. Detta tillskriver jag  kondensation på ytan som följs av frostbildning, vilket i sin tur möjliggörspridning av den underkylda vattendroppen på ytan. Mätning avfördröjningen i frysningsförloppet påvisade ingen betydande effekt avyttopografin för hydrofoba ytor, men släta hydrofoba ytor uppvisade denlängsta fördröjningen. Dessa resultat är i överensstämmelse med rådandeheterogen iskärnbildningsteori, som visar på fördelaktig iskärnbildningpå konkava delar av ytan, förutsatt att dessa väts.I den andra delen av avhandlingen utnyttjar jag observationerna frånden första delen vilka illustrerade begränsningarna för superhydrofobaytor, och söker en annan lösning. Avisningsegenskaper för hydrofilastarkt hydratiserade ytor studerades, med hypotesen att hydratiseringkan smörja gränsskiktet med is. Temperatur-kontrolleradeisadhesionsmätningar ned till -25 °C utfördes på adsorberade skikt av enpolymer med många sidokedjor av polyetylenoxid (”bottle-brush”), såvälsom på ett skikt av linjär polyetylenoxid. Isadhesionen blev kraftigtreducerad på ”bottle-brush”-polymeren, speciellt vid temperaturer högreän -15°C. Däremot kunde knappast ingen minskad isadhesion observerasför den linjära polymeren. Dessa observationer överensstämmer meddifferentialskanningskalorimetri (DSC) data, som visar att dethydratiserade vattenskiktet, vilket är bundet till ”bottle-brush”-polymeren, är i vätskeform vid de temperaturer där avisningsfördelar ärobserverade. För att vidare undersöka hypotesen att det vore fördelaktigtmed ett naturligt smörjande skikt på ytan för att uppnå godaavisningsegenskaper, utförde jag isadhesionsmätningar på molekylärtsläta glimmerytor ner till -35 °C. Intressant nog uppmättes extremt lågisadhesion på denna yta. Detta relaterar jag till den föreslagna utprägladehydratiseringsstrukturen, bestående av ett första is-liknande vattenskiktutan fria OH-grupper, följt av ett mer bulkliknande skikt. Detta ikombination med den molekylärt släta naturen hos glimmer resulterar iett perfekt plan för isen att glida på. / <p>QC 20160504</p> / TopNano

Les études, menées en collaboration entre la société VALEOL et le laboratoire IMS, proposent des solutions pour optimiser la production et le fonctionnement d'une éolienne. Il s’agit de travailler sur les lois de commande du système ou des sous-systèmes en utilisant la commande CRONE, répondant à un besoin de robustesse. Chaque étude met en avant des aspects de modélisation, d’identification et de synthèse de lois de commande avant mises en application au travers de simulations ou d’essais sur modèles réduits et taille réelle.Le chapitre 1 donne une vision d’ensemble des problématiques traitées dans ce manuscrit, à l’aide d’états de l’art et de remise dans le contexte économique et industriel de 2013.Le chapitre 2 introduit la commande CRONE pour la synthèse de régulateurs robustes. Cette méthodologie est utilisée pour réaliser l’asservissement de la vitesse de rotation d’une éolienne à vitesse variable, présentant une architecture innovante avec un variateur de vitesse mécanique et génératrice synchrone.Le chapitre 3 établit la comparaison de trois nouveaux critères d’optimisation pour la méthodologie CRONE. Le but est de réduire sa complexité et de faciliter sa manipulation par tout utilisateur. Les résultats sur les différents critères sont obtenus par simulations sur un exemple académique, puis sur un modèle d’éolienne de type MADA.Le chapitre 4 porte sur la réduction des charges structurelles transmises par le vent à l’éolienne. Il est question d’une amélioration du contrôle de l’angle de pitch par action indépendante sur chaque pale en fonction de la position du rotor ou encore des perturbations liées au ventLe chapitre 5 est consacré à la conception d’un système d’antigivrage et dégivrage d’une pale dans le cadre d’un projet Aquitain. Après modélisation et identification du procédé, la commande CRONE est utilisée pour réguler la température d’une peinture polymère chauffante sous alimentation électrique disposée sur les pales. L’étude est complétée par la mise en place d’un observateur pour la détection de présence de givre. / The research studies, in collaboration with VALEOL and IMS laboratory, propose several solutions to optimize the production and the efficiency of a wind turbine. The general theme of the work is based on control laws of the system or subsystems using the CRONE robust design. Each part highlights aspects of modeling, system identification and design before simulations or tests of scale and full size models. Chapter 1 provides an overview of the issues discussed in this manuscript, using states of the art and precisions on the industrial and economic context of 2013.Chapter 2 introduces the CRONE command for robust design. It is used to achieve the control of the rotation speed of a variable speed wind turbine, with an innovative architecture - mechanical variable speed solution and synchronous generator.Chapter 3 makes a comparison of three new optimization criteria for CRONE design. The aim is to reduce the methodology complexity and to facilitate handling by any user. The results are obtained through simulations on an academic example, then with a DFIG wind turbine model. Chapter 4 focuses on the reduction of structural loads transmitted by the wind on the turbine. It is about better control of the pitch angle by individual pitch control, depending on the rotor position or wind disturbances.Chapter 5 deals with the design of an anti-icing/de-icing system for blades. After the modeling and identification steps, the CRONE design is used to control the temperature of a heating coating disposed on the blades. An observer is finally designed to detect the presence of ice.

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