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- All Subjects: Materials Science
- Genre: Masters Thesis
Description
Gold-silver alloy nanoparticles (NPs) capped with adenosine 5'-triphosphate were synthesized by borohydride reduction of dilute aqueous metal precursors. High-resolution transmission electron microscopy showed the as-synthesized particles to be spherical with average diameters ~4 nm. Optical properties were measured by UV-Visible spectroscopy (UV-Vis), and the formation of alloy NPs was verified across all gold:silver ratios by a linear shift in the plasmon band maxima against alloy composition. The molar absorptivities of the NPs decreased non-linearly with increasing gold content from 2.0 x 108 M-1 cm-1 (fÉmax = 404 nm) for pure silver to 4.1 x 107 M-1 cm-1 (fÉmax = 511 nm) for pure gold. The NPs were immobilized onto transparent indium-tin oxide composite electrodes using layer-by-layer (LbL) deposition with poly(diallyldimethylammonium) acting as a cationic binder. The UV-Vis absorbance of the LbL film was used to calculate the surface coverage of alloy NPs on the electrode. Typical preparations had average NP surface coverages of 2.8 x 10-13 mol NPs/cm2 (~5% of cubic closest packing) with saturated films reaching ~20% of ccp for single-layer preparations (1.0 ~ 10-12 mol NPs/cm2). X-ray photoelectron spectroscopy confirmed the presence of alloy NPs in the LbL film and showed silver enrichment of the NP surfaces by ~9%. Irreversible oxidative dissolution (dealloying) of the less noble silver atoms from the NPs on LbL electrodes was performed by cyclic voltammetry (CV) in sulfuric acid. Alloy NPs with higher gold content required larger overpotentials for silver dealloying. Dealloying of the more-noble gold atoms from the alloy NPs was also achieved by CV in sodium chloride. The silver was oxidized first to cohesive silver chloride, and then gold dealloyed to soluble HAuCl4- at higher potentials. Silver oxidation was inhibited during the first oxidative scan, but subsequent cycles showed typical, reversible silver-to-silver chloride voltammetry. The potentials for both silver oxidation and gold dealloying also shifted to more oxidizing potentials with increasing gold content, and both processes converged for alloy NPs with >60% gold content. Charge-mediated electrochemistry of silver NPs immobilized in LbL films, using Fc(meOH) as the charge carrier, showed that 67% of the NPs were electrochemically inactive.
ContributorsStarr, Christopher A (Author) / Buttry, Daniel A (Thesis advisor) / Petuskey, William (Committee member) / Jones, Anne (Committee member) / Arizona State University (Publisher)
Created2014
Description
Alkali treated aluminosilicate (geopolymer) was functionalized by surfactant to increase the hydrophobicity for making Pickering emulsion for the first part of this work. In the first part of this study, alkali treated metakaolin was functionalized with cetyltrimethylammonium bromide ((C16H33)N(CH3)3Br, CTAB). The electrostatic interaction between this quaternary ammonium and the surface of the aluminosilicate which has negative charge has taken place. The particles then were used to prepare Pickering emulsion. The resulting stable dispersions, obtained very fast at very simple conditions with low ratio of aluminosilicate to liquid phase. In the second part, the interaction between geopolymer and glycerol was studied to see the covalent grafting of the geopolymer for making geopolymer composite. The composite material would be the basis material to be used as support catalyst, thin coating reagent and flame retardant material and so on, Variety of techniques, Thermogravimetric (TGA), Particle-induced X-ray emission (PIXE), FTIR, Solid state NMR, Powder X-ray diffraction (PXRD), BET surface area, Elemental analysis (CHN), TEM, SEM and Optical microscopy were used to characterize the functionalized geopolymer.
ContributorsMesgar, Milad (Author) / Seo, Dong-Kuyn (Thesis advisor) / Petuskey, William (Committee member) / Gould, Ian (Committee member) / Arizona State University (Publisher)
Created2012
Description
The microstructure development of Inconel alloy 718 (IN718) during conventional processing has been extensively studied and much has been discovered as to the mechanisms behind the exceptional creep resistance that the alloy exhibits. More recently with the development of large scale 3D printing of alloys such as IN718 a new dimension of complexity has emerged in the understanding of alloy microstructure development, hence, potential alloy development opportunity for IN718.
This study is a broad stroke at discovering possible alternate microstructures developing in Direct-Metal-Laser-Sintering (DMLS) processed IN718 compared to those in conventional wrought IN718. The main inspiration for this study came from creep test results from several DMLS IN718 samples at Honeywell that showed a significant
improvement in creep capabilities for DMLS718 compared to cast and wrought IN718 (Honeywell).
From this data the steady-state creep rates were evaluated and fitted to current creep models in order to identify active creep mechanisms in conventional and DMLS IN718 and illuminate the potential factors responsible for the improved creep behavior in DMSL processed IN718.
Because rapid heating and cooling can introduce high internal stress and impact microstructural development, such as gamma double prime formations (Oblak et al.), leading to differences in material behavior, DMLS and conventional IN718 materials are studied using SEM and TEM characterization to investigate sub-micron and/or nano-scale
microstructural differences developed in the DMLS samples as a result of their complex thermal history and internal stress.
The preliminary analysis presented in this body of work is an attempt to better understand the effect of DMLS processing in quest for development of optimization techniques for DMLS as a whole. A historical sketch of nickel alloys and the development of IN718 is given. A literature review detailing the microstructure of IN718 is presented. Creep data analysis and identification of active creep mechanisms are evaluated. High-resolution microstructural characterization of DMLS and wrought IN718 are discussed in detail throughout various chapters of this thesis. Finally, an initial effort in developing a processing model that would allow for parameter optimization is presented.
This study is a broad stroke at discovering possible alternate microstructures developing in Direct-Metal-Laser-Sintering (DMLS) processed IN718 compared to those in conventional wrought IN718. The main inspiration for this study came from creep test results from several DMLS IN718 samples at Honeywell that showed a significant
improvement in creep capabilities for DMLS718 compared to cast and wrought IN718 (Honeywell).
From this data the steady-state creep rates were evaluated and fitted to current creep models in order to identify active creep mechanisms in conventional and DMLS IN718 and illuminate the potential factors responsible for the improved creep behavior in DMSL processed IN718.
Because rapid heating and cooling can introduce high internal stress and impact microstructural development, such as gamma double prime formations (Oblak et al.), leading to differences in material behavior, DMLS and conventional IN718 materials are studied using SEM and TEM characterization to investigate sub-micron and/or nano-scale
microstructural differences developed in the DMLS samples as a result of their complex thermal history and internal stress.
The preliminary analysis presented in this body of work is an attempt to better understand the effect of DMLS processing in quest for development of optimization techniques for DMLS as a whole. A historical sketch of nickel alloys and the development of IN718 is given. A literature review detailing the microstructure of IN718 is presented. Creep data analysis and identification of active creep mechanisms are evaluated. High-resolution microstructural characterization of DMLS and wrought IN718 are discussed in detail throughout various chapters of this thesis. Finally, an initial effort in developing a processing model that would allow for parameter optimization is presented.
ContributorsRogers, Blake Kenton (Author) / Tasooji, Amaneh (Thesis advisor) / Petuskey, William (Committee member) / Rogers, Bradley (Committee member) / Arizona State University (Publisher)
Created2017