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Titanium Diboride Metal Matrix Hybrid Nanocomposite Afsaneh Dorri Moghdam University of Wisconsin-Milwaukee

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Titanium Diboride Metal Matrix Hybrid Nanocomposite Afsaneh Dorri Moghdam University of Wisconsin-Milwaukee University of Wisconsin Milwaukee UWM Digital Commons Theses and Dissertations May 2016 In-Situ Synthesis of Aluminum- Titanium Diboride Metal Matrix Hybrid Nanocomposite Afsaneh Dorri Moghdam University of Wisconsin-Milwaukee Follow this and additional works at: https://dc.uwm.edu/etd Part of the Materials Science and Engineering Commons Recommended Citation Dorri Moghdam, Afsaneh, "In-Situ Synthesis of Aluminum- Titanium Diboride Metal Matrix Hybrid Nanocomposite" (2016). Theses and Dissertations. 1137. https://dc.uwm.edu/etd/1137 This Dissertation is brought to you for free and open access by UWM Digital Commons. It has been accepted for inclusion in Theses and Dissertations by an authorized administrator of UWM Digital Commons. For more information, please contact [email protected]. IN-SITU SYNTHESIS OF ALUMINUM- TITANIUM DIBORIDE METAL MATRIX HYBRID NANOCOMPOSITE by Afsaneh Dorri Moghadam A Dissertation Submitted in Partial Fulfillment of the Requirements for the degree of Doctor of Philosophy in Engineering at The University of Wisconsin-Milwaukee May 2016 ABSTRACT IN-SITU SYNTHESIS OF ALUMINUM- TITANIUM DIBORIDE METAL MATRIX HYBRID NANOCOMPOSITE by Afsaneh Dorri Moghadam The University of Wisconsin-Milwaukee, 2016 Under the Supervision of Professor Pradeep K. Rohatgi Metal matrix nanocomposites (MMNC’s) are reported to have improved mechanical, thermal and electrical properties as compared to their respective base alloys. To date, these materials have been synthesized mainly by powder metallurgy or deformation processing. Solidification synthesis of MMNCs is a promising method, capable of economically producing large and complex shapes, however technical challenges including nanoparticle agglomeration, and poor interfacial strength have hindered the adoption of this technology. In-situ processing methods, in which the reinforcements are synthesized in liquid metals, typically via exothermic reactions offer the potential for improved dispersion and interfacial bonding between the reinforcement and the matrix, however this technique has been largely unexplored in the literature for metal matrix nanocomposites. The objectives of this research were to examine the feasibility of synthesizing nano or sub-micron size particulates in liquid aluminum using in-situ stir mixing and squeeze casting. An exothermic reaction was designed to synthesize Al2O3 and TiB2 from TiO2 particles and elemental boron in an aluminum melt. This dissertation investigates (i) the mechanism of aluminothermic and borothermic reduction of titanium oxide in the presence of molten aluminum and boron, ii (ii) in situ synthesis of micron and nano sized particles via solidification processing, and (iii) the effects of processing variables on the physical, microstructural, mechanical and tribological properties of in-situ MMNCs. Microstructural examination and theoretical analysis indicates that the reaction to form TiB2 and Al2O3 proceeds through several complex non-equilibrium reactions. A multi-stage reaction model is proposed to describe the process by which the TiO2 surface is reduced to form Al2O3 and TiB2. The effects of the powder particle size on the formation of reinforcing phases and microstructural evolution have been investigated and it was found that nanosized TiO2 powder promoted the formation of smaller size reinforcing phases. Furthermore, a solidification route has been designed to fabricate in-situ aluminum composites reinforced with submicron Al2O3 and TiB2 particulates. Experimental and theoretical analysis is presented that shows that the particle size and refining power of nanoparticles is controlled by the viscosity of the melt, rather than precipitation and growth. In addition, it was found that increasing the weight percentage of nanoparticles of TiO2 resulted in an increase in elastic modulus with good agreement to analytical models. Increasing the weight percentage of reinforcement up to 4 wt% resulted in an increase in the hardness greater than that predicted by the rule of mixtures or the Hall Petch relationship. iii © Copyright by Afsaneh Dorri Moghadam, 2016 All Rights Reserved iv I dedicate this research work to EMAD FOR HIS UNCONDITIONAL LOVE. I LOVE YOU. And also To my parents, my brother, and my sister for their endless love, support, and encouragements. v TABLE OF CONTENTS TABLE OF CONTENTS ------------------------------------------------------------------------------ vi LIST OF FIGURES ---------------------------------------------------------------------------------- viii LIST OF TABLES ------------------------------------------------------------------------------------ xiii ACKNOWLEDGEMENTS ------------------------------------------------------------------------- xiv CHAPTER 1. INTRODUCTION ------------------------------------------------------------------- 1 1.1 Introduction to Metal Matrix Nanocomposites --------------------------------------------- 1 1.2 Research Objectives ----------------------------------------------------------------------------- 6 CHAPTER 2. LITERATURE REVIEW ----------------------------------------------------------- 8 2.1 Introduction ----------------------------------------------------------------------------------------- 8 2.2 In-situ Al/TiB2 composites --------------------------------------------------------------------- 12 2.2.1 Mixed salt reaction or flux assisted synthesis (FAS) --------------------------------- 13 2.2.2 Liquid Mixing Synthesis --------------------------------------------------------------------- 16 2.2.3 Self-propagating high temperature synthesis (SHS) -------------------------------- 18 2.3 In-situ Al/TiB2 nanocomposites -------------------------------------------------------------- 19 2.4 Ultrasonic Cavitation–Based Solidification Processing -------------------------------- 21 2.5 Summary and Conclusion -------------------------------------------------------------------- 25 CHAPTER 3. REACTION MECHANISM [137] ---------------------------------------------- 28 3.1 Thermodynamic Considerations ------------------------------------------------------------ 28 3.2 Materials and Experimental ------------------------------------------------------------------ 30 3.3 Results and Discussion ----------------------------------------------------------------------- 33 3.4 Summary ------------------------------------------------------------------------------------------ 51 CHAPTER 4. PROCESSING/STRUCTURE RELATIONSHIPS ----------------------- 53 4.1 Introduction --------------------------------------------------------------------------------------- 53 4.2 Materials and Experimental ------------------------------------------------------------------ 53 4.2.1 Materials ---------------------------------------------------------------------------------------- 53 4.2.2 Composite fabrication----------------------------------------------------------------------- 54 4.2.3 Characterization of Composites ---------------------------------------------------------- 58 4.3 Results and Discussion ----------------------------------------------------------------------- 64 4.3.1 Synthesis of composites starting with micron size TiO2 --------------------------- 64 4.3.2 Synthesis of composites starting with nano size TiO2 ----------------------------- 69 4.3.3 Comparison of mechanical properties of micro and nanocomposites --------- 76 4.3.4 Variation of mechanical properties with reinforcement content ------------------ 84 4.3.5 Variation of properties with processing parameters -------------------------------- 89 4.3.6 Variation of tribological properties with processing parameters [145] ---------- 99 4.3.7 Summary -------------------------------------------------------------------------------------- 107 CHAPTER 5. CONCLUSION ------------------------------------------------------------------- 109 vi CHAPTER 6. FUTURE WORK ----------------------------------------------------------------- 114 CHAPTER 7. REFERENCES ------------------------------------------------------------------- 116 Appendix I (Corrosion and Wetting of Al/ (TiB2-Al2O3) Micro- and Nanocomposites) ----------------------------------------------------------------------------------- 124 vii LIST OF FIGURES Figure 1 Optical micrographs of a dissolving TiAl3 particle obtained through video frames during hot stage observations [119]. .......................................................................... 17 Figure 2 Generation of an acoustic bubble .......................................................................... 22 Figure 3 Schematic of cavitation bubble collapse ................................................................ 23 Figure 4 The cavitated bubble collapse and interparticle collisions lead to erosion, surface cleaning and wetting of the particles and particle size reduction .............................. 24 Figure 5 A simplified model for two SiC nanoparticles in aluminum alloy melt and the forces keep these particles together ................................................................................... 25 Figure 6 The temperature dependence of Gibbs free energy change (ΔG0)........................ 29 Figure 7 comparing free energy changes by temperature of different possible compounds in Al-Ti-B system ......................................................................................................... 30 Figure 8 Schematic showing DSC/TGA chamber equipped with Controlled back filled atmosphere. ...........................................................................................................
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