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Reactions of Aluminum with Halogen Containing Oxides by Cory Farley

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Reactions of Aluminum with Halogen Containing Oxides by Cory Farley Reactions of Aluminum with Halogen Containing Oxides by Cory Farley, B.S.M.E, M.S.B.M.E. A Dissertation In MECHANICAL ENGINEERING Submitted to the Graduate Faculty of Texas Tech University in Partial Fulfillment of the Requirements for the Degree of DOCTOR OF PHILOSOPHY Approved Michelle Pantoya Chair of Committee Kevin Long Gordon Christopher Jordan Berg Sukalyan Bhattacharya Dominick Casadonte Interim Dean of the Graduate School May 2013 Copyright 2013, Cory Farley Texas Tech University, Cory Farley, May 2013 ACKNOWLEDGEMENTS “For I know the plans I have for you,” declares the Lord, “plans to prosper you and not to harm you, plans to give you hope and a future.” – Jeremiah 29:11. Rarely do we take a direct path to the place God wants us to be, but the destination is worth it. Dr Michelle Pantoya, thank you for the patience you have shown to me over the years as I stumbled my way through. From the time I showed up at your office unannounced and unexpected and you recruited me to the Combustion Lab, you have been a rock on which I could rely. When I was confused on my research, lost in my classes, or panicking on my thesis you were there to guide me back on my path. I only hope that I can portray your professionalism and success as I move forward in my career. To my family, I left for school a long time ago as a scared little kid. However, I have always had your support to do anything, and this was no different. Dad, thank you for instilling a work ethic. Mimi and Papa, thank you for the financial help. I may have eaten ramen noodles for a stretch, but I have no student loans, and there is tremendous peace of mind knowing I will be moving forward debt free. To my beloved wife Stephanie and my son Eli, thank you for providing sanctuary. My home has always been a place of serenity where I am free to love and be loved. Stephanie, you are my soulmate with whom there are no words to describe how powerful my feelings are for you and with Eli, you are my proof that God’s plan for me does indeed give me “hope and a future” Also, I would like to acknowledge Santanu Chaudhuri and Martin Losada at ISP/Applied Sciences Laboratory, Washington State University, WA for their efforts running the quantum mechanical modeling seen in Chapter III. ii Texas Tech University, Cory Farley, May 2013 TABLE OF CONTENTS ACKNOWLEDGEMENTS ....................................................................................................... II LIST OF TABLES ................................................................................................................. IV LIST OF FIGURES ................................................................................................................ V ABSTRACT .......................................................................................................................... VI CHAPTER I: BACKGROUND ................................................................................................ 1 Ignition ............................................................................................................................ 1 Propagation ..................................................................................................................... 5 Flame Speed Measurement ........................................................................................... 12 Conclusion .................................................................................................................... 14 CHAPTER II: REACTION KINETICS OF NANOMETRIC ALUMINUM AND IODINE PENTOXIDE ....................................................................................................................... 15 Introduction ................................................................................................................... 15 Experimental Method.................................................................................................... 16 Results and Discussion ................................................................................................. 17 CHAPTER III: REACTION KINETICS OF NANO-ENERGETICS WITH HALOGEN CONTAINING OXIDES ....................................................................................................... 23 Introduction ................................................................................................................... 23 Methods......................................................................................................................... 24 Near Equilibrium Experiments ............................................................................................... 25 Non-Equilibrium Experiments ................................................................................................ 26 Ab Initio Quantum Chemical Calculations ............................................................................. 29 Solid State Calculations ........................................................................................................ 30 Gas-phase Calculations. ....................................................................................................... 31 Results ........................................................................................................................... 33 Discussion ..................................................................................................................... 39 CHAPTER IV: THE CONTRIBUTION OF ATMOSPHERIC OXYGEN TO ENERGY PROPAGATION IN REACTIVE MATERIALS ....................................................................... 43 Introduction ................................................................................................................... 43 Methods......................................................................................................................... 46 Results ........................................................................................................................... 48 Discussion ..................................................................................................................... 50 Iodine pentoxide .................................................................................................................... 51 Copper oxide ......................................................................................................................... 52 Calcium Iodate....................................................................................................................... 52 Iron oxide ............................................................................................................................... 53 CONCLUSIONS ................................................................................................................... 55 BIBLIOGRAPHY ................................................................................................................. 57 iii Texas Tech University, Cory Farley, May 2013 LIST OF TABLES 1. Powder characteristics .................................................................................................. 16 2. Reactant average particle diameter, supplier and anticipated products from Al reaction with respective oxidizer .................................................................... 25 3. Summary of experimental results. ................................................................................ 36 4. Decomposition of iodine oxide clusters in gas phase for B3LYP, PBE0 and ACM functionals at aug-cc-pVTZ (aVTZ) and aug-cc-pVQZ (aVQZ) levels of theory. The values in the bracket are calculated using spin-orbit (SO) corrections. .......................................................................................... 37 5. The reaction enthalpy and free energy calculated for Al reactions with iodine oxide fragments calculated at aug-cc-pVTZ (aVTZ) and aug-cc- pVQZ (aVQZ) .............................................................................................................. 38 6. Gas production from REAL Code analyses ................................................................. 48 7. Summary of flame speed results in units of m/s. ......................................................... 49 iv Texas Tech University, Cory Farley, May 2013 LIST OF FIGURES 1. Energy changes as an exothermic reaction proceeds .................................................... 2 2. Concept sketch of temperature profile across reaction zone of the heterogeneous composite. ............................................................................................. 6 3. Heat flow and mass loss curves of I2O5; experiments performed in an Ar environment at a heating rate of 10°C/min. ........................................................... 17 4. Heat flow and mass loss curves for Al2O3 and I2O5, experiments performed in an Ar environment at a heating rate of 10°C/min. ................................ 18 5. Heat flow and mass loss curves for micron scale Al and I2O5, experiments performed in an Ar environment at a heating rate of 10°C/min. Note the lack of any exothermic reaction .................................................. 20 6. Nanometer scale Al powder and I2O5 with an equivalence ratio of 0.4, experiments performed in an Ar environment at a heating rate of 10°C/min. .................................................................................................................... 21 7. Schematic of bomb calorimetry experiment. .............................................................. 27 8. Schematic for open tray
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