DESIGN, ASSEMBLY AND CHARACTERIZATION OF COMPOSITE ...

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4.1. Introduction CHAPTER 4 AQUEOUS NICKEL INK Colloidal inks used in solid freeform fabrication have limited material selections with respect to metals due to two major reasons: 1) many metals oxidize readily on exposure to air and may be pyrophoric if finely divided, and 2) the size of particles that are often used in processes such as powder metallurgy, laser engineered net shaping (LENS), Selective Laser Sintering, and electron beam melting (EBM) are relatively large and pose a significant challenge to use in an extrusion system for colloidal inks. Nonetheless, the ability to use metals in a solid freeform fabrication process is highly attractive because of mechanical and electrical properties. Additionally, the use of metal and ceramic inks in combination suggests ceramic-metal composite devices and metal- ceramic joints with graded composition. Examples of the use of metal inks includes various metal particle filled aqueous and organic inks used in micropen, 123, 124 fused deposition modeling, 125, 126 and other similar direct-write processes. 127-130 Robocasting has used aqueous colloidal ceramic inks, such as alumina for photonic band gap, 30 calcium phosphates for biomedical, 33 and PZT 6 and barium titanate 105 for ferroelectric purposes. A tungsten based ink has been used in Robocasting for functional graded materials 131 and biocompatible scaffolds. 132 However, no other 112
metal inks have been reported for Robocasting and this is likely due to lack of a readily available powder source and difficulty in sintering. This thesis project seeks to assemble BaTiO3-Ni composite structures using an aqueous BaTiO3 ink and requires development of an aqueous colloidal ink of Ni to serve as the metal phase. Of critical importance is matching the flow behavior of the inks, the amount of shrinkage during drying, the rate and amount of shrinkage during sintering, and the chemical stability of both species during the sintering operation. Ni has outstanding corrosion resistance and relatively low cost. Commercial production of Ni powder usually involves hydrothermal reduction of Ni salt 140 or decomposition of nickel carbonyl (Mond Process), 141 through which particles as small as 100 nm with controlled shape and morphology may be synthesized. In electronics industry, Ni powder has generally been used with organic solvents or polymeric binders for screen printing, tape casting, or conductive trace printing. At room temperature in air, Ni spontaneously develops a NiO surface layer of several atoms thick in air 133, 134 and this layer is electrically conductive. After equilibrium in water, Ni particles present a stable surface chemistry of NiO and is relatively stable in basic condition. 135 This suggests that Ni powder may be processed via aqueous colloidal route and should possess an amphoteric surface chemistry typical of most metal oxides. Aqueous Ni suspensions have been studied with the use of various polymeric dispersants 136-139 for fabrication of Ni objects through injection molding or slip casting to achieve up to 97% of theoretical density after sintering. 136 Here, an aqueous colloidal Ni gel is developed for use in the Robocasting process. Complex nickel structures are printed and pressureless sintered to achieve >99.0% 113
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DESIGN, ASSEMBLY AND CHARACTERIZATI
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ACKNOWLEDGEMENTS First and foremost
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CHAPTER 5 BARIUM TITANATE NICKEL CO
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Table 6.1 Formulations of aqueous c
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Figure 2.12 Schematic illustrations
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Figure 2.35 Schematic of the SHS pr
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Figure 4.9 Sintered nickel lattices
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Figure 6.12 Optical image of the cr
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1.1. Motivation CHAPTER 1 INTRODUCT
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and characterizing rheological prop
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2.1. Materials System CHAPTER 2 BAC
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2.2. Reentrant Structures and Ceram
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devices would provide self-sustaini
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a) b) Figure 2.4 Schematic illustra
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production of concept models, injec
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Fused Deposition Modeling (FDM) was
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Laser Engineered Net Shaping (LENS)
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Inkjet printing (IP) 27 is based on
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Table 2.1 Comparisons of various SF
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Figure 2.11 Processing steps involv
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2.4.1 Colloidal Inks The printing i
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Robocasting has lacked a well-desig
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Table 2.2 Example polymers that dep
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2.6. Sintering In robocasting, sint
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Figure 2.15 Sphere and plate model
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where
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2.5.3 Solid State Sintering In this
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Figure 2.18 Illustration of neck gr
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2.5.3.4 Final Stage During this sta
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Figure 2.23 Schematic diagram of th
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2.5.4.2 Rearrangement With the form
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2.5.4.6 Spreading of Sintering Aid
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Driven by reduction of free energy,
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2.5.5 Sintering Atmosphere Sinterin
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2.7. Composite Materials In this re
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Figure 2.29 Types of composite mate
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Table 2.6 Examples of composite mat
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Table 2.7 Examples of FGM applicati
Page 77 and 78: 2.7.3 Processing For the fabricatio
Page 79 and 80: prepared discrete layers of uniform
Page 81 and 82: Powder densification processes gene
Page 83 and 84: The specific volume fraction beyond
Page 85 and 86: a) b) Figure 2.34 a) Volume fractio
Page 87 and 88: When the powders are densified in s
Page 89 and 90: Various FGM coating processes are a
Page 91 and 92: of FGMs, such as partially reactive
Page 93 and 94: leading to a characteristic time τ
Page 95 and 96: 3.1 Introduction CHAPTER 3 AQUEOUS
Page 97 and 98: occurs in a multi-step process: fir
Page 99 and 100: a) b) Figure 3.1 a) SEM image of as
Page 101 and 102: 3.2.3 Preparation of Carbon Black C
Page 103 and 104: 3.2.5 Drying Shrinkage Characteriza
Page 105 and 106: the optimized surfactant concentrat
Page 107 and 108: The storage modulus of a colloidal
Page 109 and 110: For HA ink, yield stress
Page 111 and 112: In the case of the aqueous carbon b
Page 113 and 114: PPO units of Pluronic F-127 may ads
Page 115 and 116: a) b) Figure 3.6 A carbon black lat
Page 117 and 118: a) b) Figure 3.7 SEM images of a) c
Page 119 and 120: TGA plot is in agreement with previ
Page 121 and 122: a) b) Figure 3.9 Thermogravimetric
Page 123 and 124: 3.3.8 Fabrication of Complex Cerami
Page 125 and 126: c) d) 109
Page 127: 3.4 Conclusion A fugitive support m
Page 131 and 132: Midland, MI) 5% by weight stock sol
Page 133 and 134: 4.2.5. Thermal Degradation of Binde
Page 135 and 136: 4.3. Results and Discussion 4.3.1.
Page 137 and 138: 4.3.2. Preparation of Nickel Ink Su
Page 139 and 140: 260 °C for 8 hours, the residual c
Page 141 and 142: Table 4.1 Calculated residual carbo
Page 143 and 144: a) b) Figure 4.6 Sintered Ni struct
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Page 147 and 148: Figure 4.8 Scanning electron microg
Page 149 and 150: c) Figure 4.9 Sintered nickel latti
Page 151 and 152: 5.1. Introduction CHAPTER 5 BARIUM
Page 153 and 154: materials within the overall struct
Page 155 and 156: 40:60, 60:40, 80:20 are separately
Page 157 and 158: 5.2.3. Rheological Characterization
Page 159 and 160: 5.2.5. Co-sintering and Re-oxidatio
Page 161 and 162: mixing, BT and Ni phases appear uni
Page 163 and 164: The combined use of PAA and PAA-90K
Page 165 and 166: To quantify this difference in sint
Page 167 and 168: As the BT and Ni particles used in
Page 169 and 170: The reducing atmosphere used in the
Page 171 and 172: Figure 5.7 Vickers hardness number
Page 173 and 174: 5.3.6. Fabrication of BT-Ni composi
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Page 177 and 178: a) b) Figure 5.10 Co-sintered compo
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5.4. Conclusions Freeform fabricati
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Liquid phase sintering involves usi
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(pH=4.4, 31.5% by weight) (Adva Flo
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concentration of 7 mg/mL in the aqu
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Table 6.1 Formulations of aqueous c
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thickness. Each layer of the struct
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6.2.6. Hardness Test Microindentati
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micrographs for these two powders.
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Second, the added LiAC∙2H2O is am
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Figure 6.3 Oscillatory behavior for
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a) b) Figure 6.4 Sintering strain c
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mass transport in LFBT network. 167
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The above discussion is mainly focu
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Figure 6.8 shows the bowtie-shaped
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Figure 6.10 A NPR composite of para
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etween BT and Ni phases. But Zn ele
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Figure 6.13 Scanning electron micro
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Figure 6.15 shows the mapping of Ti
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Figure 6.17 and Figure 6.18 show el
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Figure 6.19 shows element mapping f
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6.3.7. Piezoelectricity and Dielect
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6.4. Conclusions Aqueous colloidal
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geometric features, including non-s
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3. Development of aqueous colloidal
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7.2. Recommendations In the context
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gelation behavior. κ-carrageenan i
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REFERENCES 1. Larsson 9301647, 1993
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29. Simchi, A.; Petzoldt, F.; Pohl,
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61. Bouvard, D., Acta Metallurgica
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92. Morissette, S. L.; Lewis, J. A.
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120. Boehm, H. P., Some Aspects of
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150. Atkinson, A., Growth of Nio an
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APPENDICES A. Mathematical Modeling
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and
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conditions: Equation A.12 is solved
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and with
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a) b) Figure B.1 a) Freeze-dried st
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a) Figure C.1 Cr-Ni lattices of 5Cr
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E. Binary Phase Diagram of ZnO-B2O3
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References A.1. Du, Z., Sarofim, A.
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Name: Jian Xu Date of Degree: May,
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