5 resultados para Electron energy loss spectroscopy

em Digital Commons at Florida International University


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The present research concentrates on the fabrication of bulk aluminum matrix nanocomposite structures with carbon nanotube reinforcement. The objective of the work was to fabricate and characterize multi-walled carbon nanotube (MWCNT) reinforced hypereutectic Al-Si (23 wt% Si, 2 wt% Ni, 1 wt% Cu, rest Al) nanocomposite bulk structure with nanocrystalline matrix through thermal spray forming techniques viz. plasma spray forming (PSF) and high velocity oxy-fuel (HVOF) spray forming. This is the first research study, which has shown that thermal spray forming can be successfully used to synthesize carbon nanotube reinforced nanocomposites. Microstructural characterization based on quantitative microscopy, scanning and transmission electron microscopy (SEM and TEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), Raman spectroscopy and X ray photoelectron spectroscopy (XPS) confirms (i) retention and macro/sub-macro level homogenous distribution of multiwalled carbon nanotubes in the Al-Si matrix and (ii) evolution of nanostructured grains in the matrix. Formation of ultrathin β-SiC layer on MWCNT surface, due to chemical reaction of Si atoms diffusing from Al-Si alloy and C atoms from the outer walls of MWCNTs has been confirmed theoretically and experimentally. The presence of SiC layer at the interface improves the wettability and the interfacial adhesion between the MWCNT reinforcement and the Al-Si matrix. Sintering of the as-sprayed nanocomposites was carried out in an inert environment for further densification. As-sprayed PSF nanocomposite showed lower microhardness compared to HVOF, due to the higher porosity content and lower residual stress. The hardness of the nanocomposites increased with sintering time due to effective pore removal. Uniaxial tensile test on CNT-bulk nanocomposite was carried out, which is the first ever study of such nature. The tensile test results showed inconsistency in the data attributed to inhomogeneous microstructure and limitation of the test samples geometry. The elastic moduli of nanocomposites were computed using different micromechanics models and compared with experimentally measured values. The elastic moduli of nanocomposites measured by nanoindentation technique, increased gradually with sintering attributed to porosity removal. The experimentally measured values conformed better with theoretically predicted values, particularly in the case of Hashin-Shtrikman bound method.

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Mn+1AXn compounds, the ternary layered nanolaminates have gathered momentum in the last decade since its advent because of their unusual but exciting properties. These technologically important compounds combine some of the best properties of metals and ceramics. Like ceramics they are refractory, oxidation resistant, elastically stiff and relatively light. They also exhibit metallic properties like excellent machinability, thermal and electrical conductivity. This dissertation concentrates on the synthesis of germanium-based 211 Mn+1AXn compounds. The main objective of the research was to synthesize predominantly single phase samples of Cr2GeC, V2GeC and Ti2GeC. Another goal was to study the effect of solid substitutions on the M-site of Mn+1AXn compounds with Ge as an A-element. This study is in itself the first to demonstrate the synthesis of (Cr0.5V0.5)2GeC a novel Mn+1AXn compound. Scanning electron microscopy coupled with energy dispersive spectroscopy, x-ray diffraction and electron probe microanalysis were employed to confirm the presence of predominantly single phase samples of M2GeC compounds where M = Ti, V, Cr and (Cr 0.5V0.5). A large part of the dissertation also focuses on the effect of the compressibility on the Ge-based 211 Mn+1AXn compounds with the aid of diamond anvil cell and high energy synchrotron radiation. This study also concentrates on the stability of these compounds at high temperature and thereby determines its suitability as high temperature structural materials. In order to better understand the effect of substitutions on A-site of 211 Mn+1 AXn compounds under high pressure and high temperature, a comparison is made with previously reported 211 Mn+1AXn compounds with Al, Ga and S as A-site elements.

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In this study, an Atomic Force Microscopy (AFM) roughness analysis was performed on non-commercial Nitinol alloys with Electropolished (EP) and Magneto-Electropolished (MEP) surface treatments and commercially available stents by measuring Root-Mean-Square (RMS) , Average Roughness (Ra), and Surface Area (SA) values at various dimensional areas on the alloy surfaces, ranging from (800 x 800 nm) to (115 x 115µm), and (800 x 800 nm) to (40 x 40 µm) on the commercial stents. Results showed that NiTi-Ta 10 wt% with an EP surface treatment yielded the highest overall roughness, while the NiTi-Cu 10 wt% alloy had the lowest roughness when analyzed over (115 x 115 µm). Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) analysis revealed unique surface morphologies for surface treated alloys, as well as an aggregation of ternary elements Cr and Cu at grain boundaries in MEP and EP surface treated alloys, and non-surface treated alloys. Such surface micro-patterning on ternary Nitinol alloys could increase cellular adhesion and accelerate surface endothelialization of endovascular stents, thus reducing the likelihood of in-stent restenosis and provide insight into hemodynamic flow regimes and the corrosion behavior of an implantable device influenced from such surface micro-patterns.

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We calculate the differential cross section for weak electron scattering reaction, e + 3He-' 3H + ve, for energies from 100 MeV to 6 GeV as a function of outgoing nucleus angle from 0 to n/2 radians. We find that the differential cross section at low [q2] increases with electron energy from 0.1 GeV to 6.0 GeV, such that the peak value at 6.0 GeV is approximately 3.2 x 10-40 cm 2 / ster, a factor of 10 larger than the peak value at 0.1 GeV. We also find that the width of the peak falls very rapidly with increasing electron energy. At high [q2] we find that the differential cross section falls by approximately three orders of magnitude making experimental observation at this time unlikely. The contributions of the individual form factors are obtained for electron energies of 0.5GeV and 2.0 GeV. It is found that at low [q2] the form factors, FA(q2) and Fv(q2), make contributions of similar size to the differential cross section and might be simultaneously determined , but for the case of FM(q2) we find that the contribution is too small to determine. It is also found that at large [q2] values, the contribution of FM(q2) is substantially enhanced , but that the cross section is probably too small to enable a direct determination of FM(q2).

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Ribonucleotide reductases (RNR) are essential enzymes that catalyze the reduction of ribonucleotides to 2'-deoxyribonucleotides, which is a critical step that produces precursors for DNA replication and repair. The inactivation of RNR, logically, would discontinue producing the precursors of the DNA of viral or cancer cells, which then would consequently end the cycle of DNA replication. Among different compounds that were found to be inhibitors of RNR, 2'-azido-2'-deoxynucleotide diphosphates (N3NDPs) have been investigated in depth as potent inhibitors of RNR. Decades of investigation has suggested that the inactivation of RNR by N3NDPs is a result of the formation of a nitrogen-centered radical (N·) that is covalently attached to the nucleotide at C3' and cysteine molecule C225 [3'-C(R-S-N·-C-OH)]. Biomimetic simulation reactions for the generation of the nitrogen-centered radicals similar to the one observed during the inactivation of the RNR by azionuclotides was investigated. The study included several modes: (i) theoretical calculation that showed the feasibility of the ring closure reaction between thiyl radicals and azido group; (ii) synthesis of the model azido nucleosides with a linker attached to C3' or C5' having a thiol or vicinal dithiol functionality; (iii) generation of the thiyl radical under both physiological and radiolysis conditions whose role is important in the initiation on RNR cascades; and (iv) analysis of the nitrogen-centered radical species formed during interaction between the thiyl radical and azido group by electron paramagnetic resonance spectroscopy (EPR). Characterization of the aminyl radical species formed during one electron attachment to the azido group of 2'-azido-2'-deoxyuridine and its stereospecifically labelled 1'-, 2'-, 3'-, 4'- or 5,6-[2H 2]-analogues was also examined. This dissertation gave insight toward understanding the mechanism of the formation of the nitrogen-centered radical during the inactivation of RNRs by azidonucleotides as well as the mechanism of action of RNRs that might provide key information necessary for the development of the next generation of antiviral and anticancer drugs.