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CREATION OF NEW MAGNESIUM-BASED MATERIAL USING DIFFERENT TYPES OF REINFORCEMENTS SYED FIDA HASSAN NATIONAL UNIVERSITY OF SINGAPORE 2006 CREATION OF NEW MAGNESIUM-BASED MATERIAL USING DIFFERENT TYPES OF REINFORCEMENTS SYED FIDA HASSAN (BSc Eng., BUET, Bangladesh, M Eng., NUS, Singapore) A THESIS SUBMITTED FOR THE DEGREE OF DOCTOR OF PHILOSOPHY DEPARTMENT OF MECHANICAL ENGINEERING NATIONAL UNIVERSITY OF SINGAPORE 2006 Preamble Preamble This thesis is submitted for the degree of Doctor of Philosophy in the Department of Mechanical Engineering, National University of Singapore, under the supervision of Associate Professor Manoj Gupta No part of this thesis has been submitted for any degree or diploma at any other Universities or Institution As far as this candidate is aware, all work in this thesis is original unless reference is made to other work Part of this thesis has been published and accepted for publication in the following Journals: Publications: Journals ™ S.F Hassan and M Gupta, “Development of Nano-Y2O3 Containing Magnesium Nanocomposites Using Solidification Processing”, Journal of Alloys and Compounds, 2006 (in Press) ™ S.F Hassan and M Gupta, “Effect of Different Types of Nano-size Oxide Particulates on Microstructural and Mechanical Properties of Elemental Mg”, Journal of Materials Science, 41 (2006) 2229-2236 ™ S.F Hassan and M Gupta, “Effect of Particulate Size of Al2O3 Reinforcement on Microstructure and Mechanical Behavior of Solidification Processed Elemental Mg”, Journal of Alloys and Compounds, 419 (2006) 84-90 ™ S.F Hassan and M Gupta, “Effect of length scale of Al2O3 particulates on microstructural and tensile properties of elemental Mg”, Materials Science and Engineering A, 425 (1-2) (2006) 22-27 ™ S.F Hassan and M Gupta, “Effect of Type of Primary Processing on the Microstructure, CTE and Mechanical Properties of Magnesium/Alumina Nanocomposites”, Composite Structures, 72 (1) (2006) 19-26 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan i Preamble ™ S.F Hassan and M Gupta, “Development of high performance magnesium nano-composites using nano-Al2O3 as reinforcement”, Materials Science and Engineering A, 392 (2005) 163-168 ™ S.F Hassan and M Gupta, “Enhancing Physical and Mechanical Properties of Mg Using Nano-Sized Al2O3 Particulates as Reinforcement”, Metallurgical and Materials Transactions A, 36A (2005) 2253-2258 ™ N Srikanth, Syed Fida Hassan and Manoj Gupta, “Energy Dissipation Studies of Mg Based Nanocomposites “Using an Innovative Circle-fit Approach”, Journal of Composite Materials 38 (22) (2005) 2037-2048 ™ S.F Hassan and M Gupta, “Creation of High Performance Mg Based Composite Containing Nano-size Al2O3 Particulates as Reinforcement”, Journal of Metastable and Nanocrystalline Materials, Vol 23 (2005) pp 151-154 ™ S.F Hassan and M Gupta, “Development of high-performance magnesium nano-composites using solidification processing route”, Materials Science and Technology, 20 (2004) 1383-1388 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan ii Acknowledgement Acknowledgements I would like to thank my supervisor Associate Professor Manoj Gupta for giving me an opportunity to work under him as well as for his priceless guidance, advice, motivation and patience In particular, Associate Professor Manoj Gupta’s recommendations and suggestions have been invaluable for this research work I would like to thank my colleagues for their friendship and valuable suggestions I am grateful to Mr Thomas Tan Bah Chee, Mr Abdul Khalim Bin Abdul, Mr Juraimi Bin Madon, Mr Maung Aye Thein and Mr Ng Hong Wei of the Materials Science Laboratory of NUS for their support and assistance Special thanks to Mrs Zhong Xiang Li for her cordial help in metallography for the new types of nanocomposites I would like to acknowledge financial support for this project provided by the National University of Singapore in the form of Research Scholarship Finally, words alone cannot express the thanks I owe to my parents, siblings and wife for their love, affection and encouragement without which this work would not have been possible I dedicate this work to almighty ALLAH and to his true representatives for their blessings and causeless descending mercy Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan iii Table of Contents Table of Contents Page i Preamble Acknowledgements iii Table of Contents iv Summary ix List of Tables xi List of Figures xiii Chapter Introduction Chapter Literature Survey 2.1 Introduction 2.2 Reinforcement Particulates selection 2.3 Particulates Used In Magnesium-Based Composites 2.3.1 Silicon Carbide (SiC) 2.3.2 Yttria (Y2O3) 2.3.3 Titanium Boraide (TiB2) 2.3.4 Zirconium Boride (ZrB2) 2.3.5 Titanium Carbide (TiC) 10 2.3.6 Boron Carbide (B4C) 10 2.3.7 Zirconia (ZrO2) 10 2.3.8 Alumina (Al2O3) 10 2.3.9 Diamond (C) 11 2.3.10 Copper (Cu) 11 2.3.11 Nickel (Ni) 11 2.3.12 Titanium (Ti) 11 2.4 Fabrication Methods of Magnesium Based MMCs 12 2.4.1 12 Liquid-Phase Processes 2.4.1.1 Conventional Casting 13 2.4.1.2 Infiltration Process 14 2.4.1.3 Squeeze Casting 15 2.4.1.4 In-Situ Process 16 2.4.2 Solid-Phase Process 16 2.4.3 Two-Phase Processes 16 2.4.3.1 Spray Forming 17 2.4.3.2 Disintegrated Melt Deposition 17 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan iv Table of Contents 2.4.3.3 2.6 Compocasting Summary Chapter 17 18 Materials and Methods 3.1 Overview 20 3.2 Materials 20 3.3 Primary Processing 21 3.3.1 Disintegrated Melt Deposition Technique 21 3.3.2 Blend-Press-Sinter Powder Metallurgy Technique 22 3.4 Extrusion 23 3.5 Density Measurement 23 3.6 Microstructural Characterization 23 3.7 Mechanical Characterization 24 3.7.1 Macrohardness 24 3.7.2 Microhardness 24 3.7.3 Tensile Test 25 3.7.4 Fractography 25 Chapter 4.1 4.2 4.3 4.4 Results DMD Processed nano-Al2O3 Reinforced Nanocomposites 26 4.1.1 Macrostructure 26 4.1.2 Density Measurement 26 4.1.3 Microstructural Characterization 26 4.1.4 Mechanical Properties 27 PM Processed nano-Al2O3 Reinforced Nanocomposites 30 4.2.1 Macrostructure 30 4.2.2 Density Measurement 30 4.2.3 Microstructural Characterization 30 4.2.4 Mechanical Properties 31 DMD Processed nano-Y2O3 Reinforced Nanocomposites 33 4.3.1 Macrostructure 33 4.3.2 Density Measurement 33 4.3.3 Microstructural Characterization 33 4.3.4 Mechanical Properties 34 PM Processed nano-Y2O3 Reinforced Nanocomposites 36 4.4.1 Macrostructure 36 4.4.2 Density Measurement 36 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan v Table of Contents 4.5 4.6 4.4.3 Microstructural Characterization 36 4.4.4 Mechanical Properties 37 DMD Processed nano-ZrO2 Reinforced Composites 39 4.5.1 Macrostructure 39 4.5.2 Density Measurement 39 4.5.3 Microstructural Characterization 39 4.5.4 Mechanical Properties 40 PM Processed nano-ZrO2 Reinforced Composites 42 4.6.1 Macrostructure 42 4.6.2 Density Measurement 42 4.6.3 Microstructural Characterization 42 4.6.4 Mechanical Properties 43 4.7 DMD Processed 0.3µm-Al2O3 Reinforced Composites 4.8 4.9 4.7.1 Macrostructure 45 4.7.2 Density Measurement 45 4.7.3 Microstructural Characterization 45 4.7.4 Mechanical Properties 46 PM Processed 0.3µm-Al2O3 Reinforced Composites 48 4.8.1 Macrostructure 48 4.8.2 Density Measurement 48 4.8.3 Microstructural Characterization 48 4.8.4 Mechanical Properties 49 DMD Processed 1µm-Al2O3 Reinforced Composites 51 4.9.1 Macrostructure 51 4.9.2 Density Measurement 51 4.9.3 Microstructural Characterization 51 4.9.4 Mechanical Properties 52 4.10 PM Processed 1µm-Al2O3 Reinforced Composites 54 4.10.1 Macrostructure 54 4.10.2 Density Measurement 54 4.10.3 Microstructural Characterization 54 4.10.4 Mechanical Properties 55 Chapter 5.1 45 Discussion DMD Processed nano-Al2O3 Reinforced Nanocomposites 58 5.1.1 58 Synthesis of Mg and Mg/Al2O3 Materials Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan vi Table of Contents 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 5.1.2 Microstructural Behavior 58 5.1.3 Mechanical Properties 60 PM Processed nano-Al2O3 Reinforced Nanocomposites 64 5.2.1 Microstructural Behavior 64 5.2.2 Mechanical Properties 65 DMD Processed nano-Y2O3 Reinforced Nanocomposites 69 5.3.1 Synthesis of Mg and Mg/Y2O3 Materials 69 5.3.2 Microstructural Behavior 69 5.3.3 Mechanical Properties 71 PM Processed nano-Y2O3 Reinforced Nanocomposites 76 5.4.1 Microstructural Behavior 76 5.4.2 Mechanical Properties 77 DMD Processed nano-ZrO2 Reinforced Nanocomposites 81 5.5.1 Synthesis of Mg and Mg/ZrO2 Materials 81 5.5.2 Microstructural Behavior 81 5.5.3 Mechanical Properties 83 PM Processed nano-ZrO2 Reinforced Nanocomposites 86 5.6.1 Microstructural Behavior 86 5.6.2 Mechanical Properties 87 DMD Processed 0.3µm-Al2O3 Reinforced Nanocomposites 91 5.7.1 Synthesis of Mg and Mg/Al2O3 Materials 91 5.7.2 Microstructural Behavior 91 5.7.3 Mechanical Properties 93 PM Processed 0.3µm-Al2O3 Reinforced Nanocomposites 98 5.8.1 Microstructural Behavior 98 5.8.2 Mechanical Properties 99 DMD Processed 1µm-Al2O3 Reinforced Nanocomposites 104 5.9.1 Synthesis of Mg and Mg/Al2O3 Materials 104 5.9.2 Microstructural Behavior 104 5.9.3 Mechanical Properties 106 5.10 PM Processed 1µm-Al2O3 Reinforced Nanocomposites 5.10.1 Microstructural Behavior 111 5.10.2 Mechanical Properties 112 Chapter 6.1 111 Conclusions and Recommendations Conclusions: Types of Materials 117 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan vii Table of Contents 6.1.1 DMD Processed nano-Al2O3 Reinforced Nanocomposites 117 6.1.2 PM Processed nano-Al2O3 Reinforced Nanocomposites 117 6.1.3 DMD Processed nano-Y2O3 Reinforced Nanocomposites 118 6.1.4 PM Processed nano-Y2O3 Reinforced Nanocomposites 119 6.1.5 DMD Processed nano-ZrO2 Reinforced Nanocomposites 120 6.1.6 PM Processed nano-ZrO2 Reinforced Nanocomposites 120 6.1.7 DMD Processed 0.3µm-Al2O3 Reinforced Composites 121 6.1.8 PM Processed 0.3µm-Al2O3 Reinforced Composites 122 6.1.9 DMD Processed 1µm-Al2O3 Reinforced Composites 123 6.1.10 PM Processed 1µm-Al2O3 Reinforced Composites 123 6.2 Conclusions: Comparative on Reinforcements and Processing 125 6.3 Recommendations for Future Work 127 References 128 Appendix Appendix A DMD Log Book 138 Appendix B Coefficient of Thermal Expansion 154 Appendix C Density 156 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan viii Appendix A: DMD Log Book Table A-5: Process log sheet for DMD processed nanocomposite with 1.11-vol%of 29nm-size Y2O3 Process Log Sheet for yttria Reinforced Magnesium Process Number SFH-29nm Y-1 Date 12/10/2004 Type of Ingot Mg/Y2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Material Type/Weight Mode of Mixing Matrix Reinforcement Magnesium Material Yttria Turnings/700 gm Type/ Weight Powder/22.62gm Arranged as layer of reinforcement in Mg turning in crucible Furnace Thermocouple Stirrer Coating Stirring Duration Resistance K tpye Zirtex 2.5 minutes Equipments Used Crucible Stirrer Type Stirrer Position Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 661.82gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 142 Appendix A: DMD Log Book Table A-6: Process log sheet for DMD processed nanocomposite with 0.66-vol%of 29nm-size Y2O3 Process Log Sheet for yttria Reinforced Magnesium Process Number SFH-29nm Y-2 Date 19/10/2004 Type of Ingot Mg/Y2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Matrix Reinforcement Material Magnesium Material Yttria Type/Weight Turnings/700 gm Type/ Weight Powder/13.39gm Mode of Mixing Arranged as layer of reinforcement in Mg turning in crucible Furnace Thermocouple Stirrer Coating Stirring Duration Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 450 rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 650.49gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 143 Appendix A: DMD Log Book Table A-7: Process log sheet for DMD processed nanocomposite with 0.22-vol%of 29nm-size Y2O3 Process Log Sheet for yttria Reinforced Magnesium Process Number SFH-29nm Y-3 Date 20/10/2004 Type of Ingot Mg/Y2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Matrix Reinforcement Material Magnesium Material Yttria Type/Weight Turnings/700 gm Type/ Weight Powder/4.44gm Mode of Mixing Arranged as layer of reinforcement in Mg turning in crucible Furnace Thermocouple Stirrer Coating Stirring Duration Disintegration Gas Number of Jet Disintegration Flight Distance Crucible Bottom Opening Temp (°C) 800 Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 450 rpm Disintegrated and Melt Deposition Parameters Argon Gas Jet Gas Flow Rate 25.0 L/min Disintegration Time sec 2, each of φ 4mm 500 mm Total Flight 765 mm Distance 10 mm Mold Type Cylindrical Stainless Steel, φ 40 mm Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1440 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 300gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 144 Appendix A: DMD Log Book Table A-8: Process log sheet for DMD processed nanocomposite with 0.22-vol%of 29-68nm-size ZrO2 Process Log Sheet for zirconia Reinforced Magnesium Process Number SFH-29-56nm Zr-1 Date 08/06/2005 Type of Ingot Mg/ZrO2 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Matrix Reinforcement Material Magnesium Material Zirconia Type/Weight Turnings/700 gm Type/ Weight Powder/5.22gm Mode of Mixing Arranged as layer of reinforcement in Mg turning in crucible Furnace Thermocouple Stirrer Coating Stirring Duration Disintegration Gas Number of Jet Disintegration Flight Distance Crucible Bottom Opening Temp (°C) 800 Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Argon Gas Jet Gas Flow Rate 25.0 L/min Disintegration Time sec 2, each of φ 4mm 500 mm Total Flight 765 mm Distance 10 mm Mold Type Cylindrical Stainless Steel, φ 40 mm Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 641.27gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 145 Appendix A: DMD Log Book Table A-9: Process log sheet for DMD processed nanocomposite with 0.66-vol%of 29-68nm-size ZrO2 Process Log Sheet for zirconia Reinforced Magnesium Process Number SFH-29-56nm Zr-2 Date 10/06/2005 Type of Ingot Mg/ZrO2 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Material Type/Weight Mode of Mixing Matrix Reinforcement Magnesium Material Zirconia Turnings/700 gm Type/ Weight Powder/15.74gm Arranged as layer of reinforcement in Mg turning in crucible Furnace Thermocouple Stirrer Coating Stirring Duration Resistance K tpye Zirtex 2.5 minutes Equipments Used Crucible Stirrer Type Stirrer Position Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1000 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1155 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 615.35gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 146 Appendix A: DMD Log Book Table A-10: Process log sheet for DMD processed nanocomposite with 1.11-vol%of 29-68nm-size ZrO2 Process Log Sheet for zirconia Reinforced Magnesium Process Number SFH-29-56nm Zr-3 Date 10/06/2005 Type of Ingot Mg/ZrO2 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Material Type/Weight Mode of Mixing Matrix Reinforcement Magnesium Material Zirconia Turnings/600 gm Type/ Weight Powder/22.80gm Arranged as layer of reinforcement in Mg turning in crucible Furnace Thermocouple Stirrer Coating Stirring Duration Resistance K tpye Zirtex 2.5 minutes Equipments Used Crucible Stirrer Type Stirrer Position Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1000 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1155 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 463.02gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 147 Appendix A: DMD Log Book Table A-11: Process log sheet for DMD processed composite with 2.49-vol%of 0.3µm-size Al2O3 Process Log Sheet for alumina Reinforced Magnesium Process Number SFH-0.3µm Al-1 Date 06/10/2004 Type of Ingot Mg/Al2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Material Type/Weight Mode of Mixing Matrix Reinforcement Magnesium Material Alumina Turnings/700 gm Type/ Weight Powder/40.85gm Al2O3 powder inserted in Mg-turnings in three Al tube of 1.16gm Furnace Thermocouple Stirrer Coating Stirring Duration Disintegration Gas Number of Jet Disintegration Flight Distance Crucible Bottom Opening Temp (°C) 800 Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Argon Gas Jet Gas Flow Rate 25.0 L/min Disintegration Time sec 2, each of φ 4mm 500 mm Total Flight 765 mm Distance 10 mm Mold Type Cylindrical Stainless Steel, φ 40 mm Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 617.27gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 148 Appendix A: DMD Log Book Table A-12: Process log sheet for DMD processed composite with 1.11-vol%of 0.3µm-size Al2O3 Process Log Sheet for alumina Reinforced Magnesium Process Number SFH-0.3µm Al-2 Date 21/08/2003 Type of Ingot Mg/Al2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Matrix Reinforcement Material Magnesium Material Alumina Type/Weight Turnings/780 gm Type/ Weight Powder/20gm Mode of Mixing Al2O3 powder inserted in Mg-turnings in two Al tube of 1.00gm Furnace Thermocouple Stirrer Coating Stirring Duration Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 715.2gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 149 Appendix A: DMD Log Book Table A-13: Process log sheet for DMD processed composite with 0.66-vol%of 0.3µm-size Al2O3 Process Log Sheet for alumina Reinforced Magnesium Process Number SFH-0.3µm Al-3 Date 26/08/2003 Type of Ingot Mg/Al2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Material Type/Weight Mode of Mixing Matrix Reinforcement Magnesium Material Alumina Turnings/788 gm Type/ Weight Powder/12gm Al2O3 powder inserted in Mg-turnings in two Al tube of 0.50gm Furnace Thermocouple Stirrer Coating Stirring Duration Resistance K tpye Zirtex 2.5 minutes Equipments Used Crucible Stirrer Type Stirrer Position Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1440 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 715.2gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 150 Appendix A: DMD Log Book Table A-14: Process log sheet for DMD processed composite with 2.49-vol%of 1µm-size Al2O3 Process Log Sheet for alumina Reinforced Magnesium Process Number SFH-1µm Al-1 Date 08/10/2004 Type of Ingot Mg/Al2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Matrix Reinforcement Material Magnesium Material Alumina Type/Weight Turnings/700 gm Type/ Weight Powder/40.85gm Mode of Mixing Al2O3 powder inserted in Mg-turnings in three Al tube of 1.16gm Furnace Thermocouple Stirrer Coating Stirring Duration Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 460 rpm Disintegrated and Melt Deposition Parameters Disintegration Gas Argon Gas Jet Gas Flow Rate 25.0 L/min Number of Jet Disintegration Time sec 2, each of φ 4mm Disintegration 500 mm Total Flight 765 mm Flight Distance Distance Crucible Bottom 10 mm Mold Type Cylindrical Stainless Opening Steel, φ 40 mm Temp (°C) 800 Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 669.07gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 151 Appendix A: DMD Log Book Table A-15: Process log sheet for DMD processed composite with 1.11-vol%of 1µm-size Al2O3 Process Log Sheet for alumina Reinforced Magnesium Process Number SFH-1µm Al-2 Date 11/10/2004 Type of Ingot Mg/Al2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Material Type/Weight Mode of Mixing Matrix Reinforcement Magnesium Material Alumina Turnings/700 gm Type/ Weight Powder/17.88gm Al2O3 powder inserted in Mg-turnings in two Al tube of 0.63gm Furnace Thermocouple Stirrer Coating Stirring Duration Disintegration Gas Number of Jet Disintegration Flight Distance Crucible Bottom Opening Temp (°C) 800 Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 450 rpm Disintegrated and Melt Deposition Parameters Argon Gas Jet Gas Flow Rate 25.0 L/min Disintegration Time sec 2, each of φ 4mm 500 mm Total Flight 765 mm Distance 10 mm Mold Type Cylindrical Stainless Steel, φ 40 mm Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1320 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 668.10gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 152 Appendix A: DMD Log Book Table A-16: Process log sheet for DMD processed composite with 0.66-vol%of 1µm-size Al2O3 Process Log Sheet for alumina Reinforced Magnesium Process Number SFH-1µm Al-3 Date 11/10/2004 Type of Ingot Mg/Al2O3 Status Successful Processing Technique Disintegrated Melt Deposition Materials Used Matrix Reinforcement Material Magnesium Material Alumina Type/Weight Turnings/700 gm Type/ Weight Powder/10.58gm Mode of Mixing Al2O3 powder inserted in Mg-turnings in two Al tube of 0.52gm Furnace Thermocouple Stirrer Coating Stirring Duration Disintegration Gas Number of Jet Disintegration Flight Distance Crucible Bottom Opening Temp (°C) 800 Equipments Used Resistance Crucible K tpye Stirrer Type Zirtex Stirrer Position 2.5 minutes Stirring Speed Graphite Twin Blade Impeller ~20 mm from bottom ~ 450 rpm Disintegrated and Melt Deposition Parameters Argon Gas Jet Gas Flow Rate 25.0 L/min Disintegration Time sec 2, each of φ 4mm 500 mm Total Flight 765 mm Distance 10 mm Mold Type Cylindrical Stainless Steel, φ 40 mm Heating Profile 400 0 Start Time Initial Temperature Inert Atmosphere 50 1440 hrs 25 0C Argon 100 Time (min) 150 Heating Profile End Time Final Temperature Flow Rate 200 1510 hrs 750 0C lit/min Observations Continuous flows of magnesium melt from the crucible Ingot weighed 576.56gm Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 153 Appendix B: Coefficient of Thermal Expansion Appendix B: Thermal Analysis Coefficient of thermal expansion (CTE) of monolithic and composite materials was determined using an automated SETARAM 92-16/18 thermomechanical analyzer Displacement of monolithic and composite materials was measured as a function of temperature (in the range of 50°-400°C) using an alumina probe under argon atmosphere and was subsequently used to determine the coefficient of thermal expansion The heating rate of the samples was maintained at 5°C/min while the argon gas flow rate was maintained at 1.2 lit/min A sample length of ~15 mm was used in all of the tests The results shows reinforcements used in this study has very little effect in improving dimensional stability of pure magnesium matrix and thus not included in main content of the thesis Table B-1: Results of Coefficient of Thermal Expansion (CTE) measurements of DMD processed Materials Materials Pure Mg Mg/0.22Al2O3 Mg/0.66Al2O3 Mg/1.11Al2O3 Mg/0.22Y2O3 Mg/0.66Y2O3 Mg/1.11Y2O3 Mg/0.22ZrO2 Mg/0.66ZrO2 Mg/1.11ZrO2 Mg/0.66Al2O3 Mg/1.11Al2O3 Mg/2.49Al2O3 Mg/0.66Al2O3 Mg/1.11Al2O3 Mg/2.49Al2O3 Reinforcement size 50-nm 50-nm 50-nm 29-nm 29-nm 29-nm 29-58-nm 29-58-nm 29-58-nm 0.3-µm 0.3-µm 0.3-µm 1-µm 1-µm 1-µm weight percentage CTE (x10-6/°k) 0.5 1.5 2.5 0.6 1.9 3.1 0.7 2.2 3.7 1.5 2.5 5.5 1.5 2.5 5.5 28.4 ± 0.3 27.5 ± 0.1 28.0 ± 0.9 25.1 ± 0.3 27.2 ±0.3 28.8 ± 0.5 26.0 ± 1.4 27.9 ± 0.6 26.4 ± 1.8 26.1 ± 0.9 28.2 ± 0.7 27.4 ± 1.3 26.8 ± 0.4 29.0 ± 0.3 26.1 ± 1.8 28.2 ± 0.2 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 154 Appendix B: Coefficient of Thermal Expansion Table B-2: Results of Coefficient of Thermal Expansion (CTE) measurements of PM processed Materials Materials Pure Mg Mg/0.22Al2O3 Mg/0.66Al2O3 Mg/1.11Al2O3 Mg/0.22Y2O3 Mg/0.66Y2O3 Mg/1.11Y2O3 Mg/0.22ZrO2 Mg/0.66ZrO2 Mg/1.11ZrO2 Mg/0.66Al2O3 Mg/1.11Al2O3 Mg/2.49Al2O3 Mg/0.66Al2O3 Mg/1.11Al2O3 Mg/2.49Al2O3 Reinforcement size 50-nm 50-nm 50-nm 29-nm 29-nm 29-nm 29-58-nm 29-58-nm 29-58-nm 0.3-µm 0.3-µm 0.3-µm 1-µm 1-µm 1-µm weight percentage CTE (x10-6/°k) 0.5 1.5 2.5 0.6 1.9 3.1 0.7 2.2 3.7 1.5 2.5 5.5 1.5 2.5 5.5 29.4 ± 0.3 29.0 ± 0.2 28.2 ± 1.1 28.4 ± 0.7 28.8 ±0.1 28.6 ± 0.1 21.6 ± 1.6 30.1 ± 0.1 27.2 ± 0.9 21.7 ± 1.1 28.3 ± 0.7 29.3 ± 0.4 29.2 ± 0.5 29.0 ± 0.1 28.4 ± 0.5 28.4 ± 0.4 Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 155 Appendix C: Density Appendix C: Density Calculation Equations in Density and Porosity Calculation ™ ™ Wa × ρ w − Ww × ρ a Wa − Ww Where, ρe = Experimental density; Ww = Weight of the specimen in water; Wa = Weight of the specimen in air; ρa = Density of air = 0.001225g/cc; ρw = Density of water = g/cc Experimental density was given by the equation; ρ e = Theoretical density was given by equation of Rule-of-Mixture (ROM); ρth = (1-Vr) ρm + Vr ρr Where, ρth = Theoretical density; Vr = Volume fraction of reinforcement; ρm = Density of matrix material; ρr = Density of reinforcing material Density of matrix material i.e., magnesium [74] is 1.74 gm/cm3 Density of reinforcement materials [75] are: Al2O3 = 3.96 gm/cm3, Y2O3 = 5.01 gm/cm3, and ZrO2 = 5.89 gm/cm3, respectively ™ Porosity of the developed materials were calculated using the equation Porosity = ρ th − ρ e and Percentage porosity = Porosity × 100 ρ th − ρ a Creation of New Mg-Based Material Using Different Types of Reinforcements by S Fida Hassan 156