Development of PVD-coated and nanostructured reactive multilayer films. Seema Sen

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1 Development of PVD-coated and nanostructured reactive multilayer films Seema Sen Universitätsverlag Ilmenau 2018

2 Impressum Bibliografische Information der Deutschen Nationalbibliothek Die Deutsche Nationalbibliothek verzeichnet diese Publikation in der Deutschen Nationalbibliografie; detaillierte bibliografische Angaben sind im Internet über abrufbar. Diese Arbeit hat der Fakultät für Elektrotechnik und Informationstechnik der Technischen Universität Ilmenau als Dissertation vorgelegen. Tag der Einreichung: 14. November Gutachter: Univ.-Prof. Dr. rer. nat. habil. Dr h.c. Peter Schaaf (Technische Universität Ilmenau) 2. Gutachter: Univ.-Prof. Dr.-Ing. habil. Jean Pierre Bergmann (Technische Universität Ilmenau) 3. Gutachter: Prof. Dr.-Ing. Markus K. Lake (Hochschule Niederrhein, Krefeld) Tag der Verteidigung: 6. Juli 2018 Technische Universität Ilmenau/Universitätsbibliothek Universitätsverlag Ilmenau Postfach Ilmenau readbox unipress in der readbox publishing GmbH Am Hawerkamp Münster ISSN ISBN URN (Druckausgabe) (Druckausgabe) urn:nbn:de:gbv:ilm Cover Image: Left: SEM image of freestanding ternary Ti/Si/Ti/Al reactive multilayer film. / Middle: Colored TEM image of Zr/Al binary reactive film. / Right: High speed photographic image of steady state reaction propagation in Ti/Si/Ti/Al reactive film (top) and unsteady propagation in Ti/3Al reactive film (bottom).

3 Danksagung... VII Kurzfassung... IX Abstract... XIII... XV 1 Introduction Motivation and goals State of the art Self-propagating exothermic reaction Reactive material systems Nanoscale effects and diffusion phenomenon Exothermic reaction properties and kinetics Manufacturing process Ignition methods for multilayers Potential fields of application Materials and experimental methods Selection of reactant combinations for RMFs Magnetron Sputter Ion Plating (MSIP) method Synthesis of freestanding RMFs Characterization techniques Microstructural analysis Phase identification by XRD Electrical resistivity measurement Differential scanning calorimetry Measurement of reaction propagation and temperature Reactive joining process Thermodynamic and numerical CFD simulation... 36

4 XVI Results and Discussions Simulation Thermodynamic simulation Ti-Al binary system Zr-Al binary system Ti-Si binary system Computational Fluid Dynamics (CFD) Numerical modelling Concentration profile during reaction Simulated temperature flow during exothermic reaction Ti/Al reactive multilayer film Synthesis of Ti/Al RMFs with different molar ratios Microstructural analysis of as-deposited RMFs Reaction products identification by XRD Exothermic reaction properties of Ti/Al RMFs Transformation heat and phase change temperature by DSC Reaction front velocity of Ti/Al RMFs Reaction temperature evaluation High temperature oxidation during self-propagating reaction Reaction propagation mode and its effects on reaction properties Characterization of reacted Ti/Al films Zr/Al reactive multilayer film Synthesis and characterization of Zr/Al RMFs Reaction products identification by XRD Exothermic reaction properties Evaluation of phase change temperature and heat flows Reaction front velocity of Zr/Al RMFs Reaction temperature in Zr/Al RMFs Oxidation effects during reaction in Zr/Al RMFs Microstructural analysis of reacted Zr/Al films... 96

5 XVII 8 Ternary reactive films of Ti, Si and Al reactants Investigation of Si/Ti/Al/Si and Ti/Si/Ti/nAl RMFs Characterization of unreacted ternary RMFs Reaction products identification by XRD Exothermic reaction properties of ternary RMFs Phase change temperature and transformation heat Reaction front velocity Reaction temperature in ternary RMFs Microstructural analysis of reacted ternary films Comparative analysis on reaction properties in developed RMFs Certain considerations for synthesis and uses Process development for large sized freestanding film synthesis Stability and handling Expanded applications of developed reactive films Developed ternary RMFs for reactive joining Conclusions and outlook References List of figures List of tables List of abbreviations List of symbols List of own publications in reviewed international journals Conferences Scientific presentations Patent registration Lectureship and teaching

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