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The Pennsylvania State University The Pennsylvania State University The Graduate School College of Earth and Mineral Sciences METAL ORGANIC CHEMICAL VAPOR DEPOSITION OF ENVIRONMENTAL BARRIER COATINGS FOR THE INHIBITION OF SOLID DEPOSIT FORMATION FROM HEATED JET FUEL A Dissertation in Energy and Geo-Environmental Engineering by Arun Ram Mohan ©2011 Arun Ram Mohan Submitted in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy May 2011 The dissertation of Arun Ram Mohan was reviewed and approved* by the following: Semih Eser Professor of Energy and Geo-Environmental Engineering Dissertation Advisor Chair of Committee Ljubisa R. Radovic Professor of Energy and Mineral Engineering André L. Boehman Professor of Fuel Science and Materials Science and Engineering Coray M. Colina Corning Faculty Fellow Associate Professor of Materials Science and Engineering Yaw D. Yeboah Professor and Department Head of Energy and Mineral Engineering *Signatures are in file in the Graduate School ii ABSTRACT Solid deposit formation from jet fuel compromises the fuel handling system of an aviation turbine engine and increases the maintenance downtime of an aircraft. The deposit formation process depends upon the composition of the fuel, the nature of metal surfaces that come in contact with the heated fuel and the operating conditions of the engine. The objective of the study is to investigate the effect of substrate surfaces on the amount and nature of solid deposits in the intermediate regime where both autoxidation and pyrolysis play an important role in deposit formation. A particular focus has been directed to examining the effectiveness of barrier coatings produced by metal organic chemical vapor deposition (MOCVD) on metal surfaces for inhibiting the solid deposit formation from jet fuel degradation. In the first part of the experimental study, a commercial Jet-A sample was stressed in a flow reactor on seven different metal surfaces: AISI316, AISI 321, AISI 304, AISI 347, Inconel 600, Inconel 718, Inconel 750X and FecrAlloy. Examination of deposits by thermal and microscopic analysis shows that the solid deposit formation is influenced by the interaction of organosulfur compounds and autoxidation products with the metal surfaces. The nature of metal sulfides was predicted by Fe-Ni-S ternary phase diagram. Thermal stressing on uncoated surfaces produced coke deposits with varying degree of structural order. They are hydrogen-rich and structurally disordered deposits, spherulitic deposits, small carbon particles with relatively ordered structures and large platelets of ordered carbon structures formed by metal catalysis. In the second part of the study, environmental barrier coatings were deposited on tube surfaces to inhibit solid deposit formation from the heated fuel. A new CVD system was configured by the proper choice of components for mass flow, pressure and temperature control in the reactor. A bubbler was designed to deliver the precursor into the reactor for the deposition iii of metal and metal oxide functional coatings by MOCVD. Alumina was chosen as a candidate for metal oxide coating because of its thermal and phase stability. Platinum was chosen as a candidate to utilize the oxygen spillover process to maintain a self-cleaning surface by oxidizing the deposits formed during thermal stressing. Two metal organic precursors, aluminum trisecondary butoxide and aluminum acetylacetonate, were used as precursors to coat tubes of varying diameters. The morphology and uniformity of the coatings were characterized by electron microscopy and energy-dispersive x-ray spectroscopy. The coating was characterized by x-ray photoelectron spectroscopy to obtain the surface chemical composition. This is the first study conducted to examine the application of MOCVD to coat internal surfaces of tubes with varying diameters. In the third part of the study, the metal oxide coatings, alumina from aluminum acetylacetonate, alumina from aluminum trisecondary butoxide, zirconia from zirconium acetylacetonate, tantalum oxide from tantalum pentaethoxide and the metal coating, platinum from platinum acetylacetonate were deposited by MOCVD on AISI304. The chemical composition and the surface acidity of the coatings were characterized by x-ray photoelectron spectroscopy. The morphology of the coatings was characterized by electron microscopy. The coated substrates were tested in the presence of heated Jet-A in a flow reactor to evaluate their effectiveness in inhibiting the solid deposit formation. All coatings inhibited the formation of metal sulfides and the carbonaceous solid deposits formed by metal catalysis. The coatings also delayed the accumulation of solid carbonaceous deposits. In particular, it has been confirmed that the surface acidity of the metal oxide coatings affects the formation of carbonaceous deposits. Bimolecular addition reactions promoted by the Brønsted acid sites appear to lead to the formation of carbonaceous solid deposits depending on the surface acidity of the coatings. iv In the last part of the study, the residual carbon was incorporated in the zirconia coating by deposition with and without oxygen. As carbon surface is less active towards coke deposition, presence of residual carbon in the coating was expected to reduce its activity towards carbon deposition. The residual carbon in the coating was characterized by Raman spectroscopy and thermal analysis. However, it has been observed that residual carbon in the coating beyond a certain concentration compromises the integrity of the coating during the process of cooling the substrate from deposition temperature to room temperature. It has been found that residual carbon in the zirconia coating does not appear to affect the activity of the surface towards carbon deposition. v Table of Contents List of Tables ix List of Figures x Acknowledgements xv Chapter 1. Introduction 1 1.1 Background 1 1.1.1 Liquid phase autoxidation of hydrocarbons 1 1.1.2 Deposit formation during autoxidation of hydrocarbons 4 1.1.2.1 Effects of hydrocarbon structure 4 1.1.2.2 Effects of dissolved oxygen 7 1.1.2.3 Effects of sulfur compounds 8 1.1.2.4 Effects of nitrogen- and oxygen-containing compounds 9 1.1.2.5 Effects of antioxidants 9 1.1.2.6 Synergism between natural and synthetic antioxidants 10 1.1.2.7 Effects of natural antioxidants in autoxidation of neat and blended fuels 12 1.1.2.8 Effects of surface catalysis on the liquid phase autoxidation of hydrocarbons 13 1.1.2.8a Effects of metals 13 1.1.2.8b Effects of metal oxides 15 1.1.2.9 Autoxidation of jet fuels and deposit formation 16 1.1.3 Factors affecting deposits under pyrolytic conditions 20 1.1.4 Solid deposit formation from jet fuel under pyrolytic conditions 21 1.1.4.1 Carbonaceous mesophase 21 1.1.4.2 Filamentous carbon 23 1.1.4.3 Spherulitic deposits 24 1.1.4.4 Pyrolytic carbon 25 1.1.4.5 Metal sulfides 25 1.2 Objectives of the thesis 27 1.3 Organization of the thesis 28 1.4 References 29 Chapter 2. Analysis of Carbonaceous Solid Deposits from Thermal Oxidative Stressing of Jet-A Fuel on Iron and Nickel-based Alloy Surfaces 34 2.1 Abstract 34 2.2 Introduction 34 2.3 Experimental Section 36 2.3.1 Thermal stressing experiments 36 2.3.2 Characterization of carbon deposits 37 2.4 Results and Discussion 38 2.4.1 Amount of solid carbon deposited on different metal substrates 39 2.4.2 TPO and FESEM analysis of deposits on various substrates 40 2.5 Conclusions 48 2.6 References 50 vi Chapter 3. Environmental Barrier Coatings by MOCVD on Tube Surfaces to Inhibit Carbon Deposition 61 3.1 Background 61 3.2 Coating process for EBCs 63 3.2.1 Plasma spray deposition 63 3.2.2 Electron beam physical vapor deposition 66 3.2.3 Electrodeposition process 68 3.2.4 Chemical vapor deposition 70 3.2.5 Effect of process variables on MOCVD and properties of coatings 71 3.2.6 Influence of process parameters in the stress induced in coatings 73 3.2.7 Coating precursors 74 3.2.8 Configuration of the MOCVD experimental set-up for coating tubes 75 3.3 Experimental Procedure 76 3.4 Results and Discussion 77 3.4.1 Characterization of alumina coatings from aluminum trisecondary butoxide 77 3.4.2 Characterization of alumina coatings from aluminum acetylacetonate 84 3.4.3 Temperature-Programmed Oxidation of residual carbon in alumina coatings 88 3.4.4 Characterization of platinum deposited on alumina coating 89 3.5 Conclusions 91 3.6 References 93 Chapter 4. Effectiveness of Low-Pressure MOCVD Coatings on Metal Surfaces for the Mitigation of Fouling from Heated Jet Fuel 112 4.1 Abstract 112 4.2 Introduction 113 4.3 Experimental section 114 4.3.1 MOCVD experimental set-up for foil coatings 114 4.3.2 Thermal stressing experiments 116 4.3.3 Characterization of coatings and carbon deposits 117 4.4 Results and Discussion 120 4.4.1 Morphology and spectroscopic characterization of coated substrates 120 4.4.2 Analysis of Jet-A sample and TPO of the deposits on coated & uncoated substrates 125 4.5 Conclusions 132 4.6 References 134 Chapter 5. Characterization of Zirconia Coatings Deposited by MOCVD and Their Effectiveness in Inhibiting Solid Deposition from Jet Fuel 150 5.1 Abstract 150 5.2 Introduction 150 5.3 Experimental section 151 5.3.1 MOCVD experimental set-up for zirconia coating 151 5.3.2 Thermal stressing experiments 152 5.3.3 Characterization of coatings and carbon deposits 153 vii 5.4 Results and Discussion 155 5.4.1 Morphology of zirconia coating 155 5.4.2 Raman spectra of zirconia coatings 156 5.4.3 Infrared spectrum of zirconia coatings 157 5.4.4 X-ray photoelectron spectroscopy of residual carbon in the zirconia coating 159 5.4.5 Temperature–Programmed Oxidation 160 5.5 Conclusions 162 5.6 References 163 Chapter 6.
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