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Synthesis and characterization of nanostructured molybdenum & tungsten carbide materials, and study of diffusion model

100%
Covington L., Munirathinam K., Islam A., Roberts K.
Polish Journal of Chemical Technology
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2012
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vol. 14
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issue 1
28-34
EN
Powders of two molybdenum carbides (Mo2C and MoC1-x) and tungsten carbide (WC) were prepared by means of temperature programmed reaction (TPR) method. Mo2C and MoC1-x were synthesized by reacting MoO3 with a preselected molar ratio of methane/hydrogen and carbon monoxide/hydrogen gas mixtures respectively. WC was prepared using tungsten oxide (WO3) and a methane/hydrogen gas mixture. These carbides were ultrasonically dispersed in de-ionized water. Samples were characterized using room temperature x-ray diffraction and scanning microscopy. A kinetic diffusion model is also studied to determine diffusivities in solids where the diffusing species desorbs or reacts at the external surfaces, and where the diffusivity does not vary appreciably with concentrations. The method involves measuring the flux of the diffusive species into the solid under the influence of a temperature program.
2
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Characterization of CdSe quantum dots with bidentate ligands by capillary electrophoresis

100%
Oszwałdowski S., Zawistowska-Gibuła K., Roberts K.
Open Chemistry
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2011
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vol. 9
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issue 4
572-584
EN
The CdSe quantum dots (QDs) with bidentate ligands: a-diimine (NN) and dihydrolipoic acid (DHLA) were synthesized and characterized by UV-Vis, particle size and capillary electrophoretic techniques. Two systems were analyzed: CdSe with one ligand (CdSe/ligand) and CdSe with two different ligands (CdSe//ligand1/ligand2), where ligand = α-diimine or DHLA. Hydrodynamic features of functionalized QDs were characterized by zone capillary electrophoretic (CZE), and particle size techniques and these methods were consistent. It was established that CZE, micellar (MEKC) and microemulsion (MEEKC) modes were suitable for separating charged CdSe QDs and that no peaks were obtained for QDs passivated with electrically neutral ligands. For CdSe QDs with neutral (NN) ligands, a preconcentration method with the use of a micellar plug was introduced for visualizing these QDs. A sharp peak representing neutral QDs was obtained within the zone of micellar plug of a non-ionic surfactant, Here, a ligand character used for CdSe modification and the type of the electrophoretic method applied were the determining factors for the QDs peak visualization. Moreover, examples of visualization of charged and neutral QDs on the same run were presented, and for this purpose, dual mechanism (separation/preconcentration) was proposed. [...]
3
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Capillary electrophoretic separation and characterizations of CdSe quantum dots

100%
Oszwałdowski S., Zawistowska K., Grigsby L., Roberts K.
Open Chemistry
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2010
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vol. 8
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issue 4
806-819
EN
We have developed a capillary electrophoresis method to characterize the QD surface ligand interactions with various surfactant systems. The method was demonstrated with 2–5 nm CdSe nanoparticles surface-passivated with trioctylphosphine oxide (TOPO). Water solubility was accomplished by surfactant-assisted phase transfer via an oil-in-water microemulsion using either cationic, anionic, or non-ionic surfactants. Interaction between the QD surface ligand (TOPO) and the alkyl chain of the surfactant molecule produces a complex and dynamic surface coating that can be characterized through manipulation of CE separation buffer composition and capillary surface modification. Additional characterization of the QD surface ligand interactions with surfactants was accomplished by UV-VIS spectroscopy, photoluminescence, and TEM. It is anticipated that studies such as these will elucidate the dynamics of QD surface ligand modifications for use in sensors. [...]
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