957 resultados para Metamictization, brannerite, uranyl, titanium, mineral, Raman spectroscopy, U-O bond length
Resumo:
Raman spectra of two well-defined types of cobaltkoritnigite and koritnigite crystals were recorded and interpreted. Significant differences in the Raman spectra of cobaltkoritnigite and koritnigite were observed. Observed Raman bands were attributed to the (AsO3OH)2− stretching and bending vibrations, stretching and bending vibrations of water molecules and hydroxyl ions. Both Raman and infrared spectra of cobaltkoritnigite identify bands which are attributable to phosphate and hydrogen phosphate anions proving some substitution of phosphate for arsenate in the structure of cobaltkoritnigite. The OH⋯O hydrogen bond lengths in the crystal structure of koritnigite were inferred from the Raman spectra and compared with those derived from the X-ray single crystal refinement. The presence of (AsO3OH)2− units in the crystal structure of cobaltkoritnigite and koritnigite was proved from the Raman spectra which supports the conclusions of the X-ray structure analysis.
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A series of rubber composites were prepared by blending styrene-butadiene rubber (SBR) latex and the different particle sized kaolinites. The thermal stabilities of the rubber composites were characterized using thermogravimetry, digital photography, scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and Raman spectroscopy. Kaolinite SBR composites showed much greater thermal stability when compared with that of the pure SBR. With the increase of kaolinite particle size, the pyrolysis products became much looser; the char layer and crystalline carbon content gradually decreased in the pyrolysis residues. The pyrolysis residues of the SBR composites filled with the different particle sized kaolinites showed some remarkable changes in structural characteristics. The increase of kaolinite particle size was not beneficial to form the compact and stable crystalline carbon in the pyrolysis process, and resulted in a negative influence in improving the thermal stability of kaolinite/SBR composites.
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Erythropoietin (EPO), a glycoprotein hormone of ∼34 kDa, is an important hematopoietic growth factor, mainly produced in the kidney and controls the number of red blood cells circulating in the blood stream. Sensitive and rapid recombinant human EPO (rHuEPO) detection tools that improve on the current laborious EPO detection techniques are in high demand for both clinical and sports industry. A sensitive aptamer-functionalized biosensor (aptasensor) has been developed by controlled growth of gold nanostructures (AuNS) over a gold substrate (pAu/AuNS). The aptasensor selectively binds to rHuEPO and, therefore, was used to extract and detect the drug from horse plasma by surface enhanced Raman spectroscopy (SERS). Due to the nanogap separation between the nanostructures, the high population and distribution of hot spots on the pAu/AuNS substrate surface, strong signal enhancement was acquired. By using wide area illumination (WAI) setting for the Raman detection, a low RSD of 4.92% over 150 SERS measurements was achieved. The significant reproducibility of the new biosensor addresses the serious problem of SERS signal inconsistency that hampers the use of the technique in the field. The WAI setting is compatible with handheld Raman devices. Therefore, the new aptasensor can be used for the selective extraction of rHuEPO from biological fluids and subsequently screened with handheld Raman spectrometer for SERS based in-field protein detection.
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Pure phase Cu2ZnSnS4 (CZTS) nanoparticles were successfully synthesized via polyacrylic acid (PAA) assisted one-pot hydrothermal route. The morphology, crystal structure, composition and optical properties as well as the photoactivity of the as-synthesized CZTS nanoparticles were characterized by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectrometer, UV-visible absorption spectroscopy and photoelectrochemical measurement. The influence of various synthetic conditions, such as the reaction temperature, reaction duration and the amount of PAA in the precursor solution on the formation of CZTS compound was systematically investigated. The results have shown that the crystal phase, morphology and particle size of CZTS can be tailored by controlling the reaction conditions. The formation mechanism of CZTS in the hydrothermal reaction has been proposed based on the investigation of time-dependent phase evolution of CZTS which showed that metal sulfides (e.g., Cu2S, SnS2 and ZnS) were formed firstly during the hydrothermal reaction before forming CZTS compound through nucleation. The band gap of the as-synthesized CZTS nanoparticles is 1.49 eV. The thin film electrode based on the synthesized CZTS nanoparticles in a three-electrode photoelectrochemical cell generated pronounced photocurrent under illumination provided by a red light-emitting diode (LED, 627 nm), indicating the photoactivity of the semiconductor material.
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This thesis is a step forward in understanding the growth of graphene, a single layer of carbon atoms, by annealing Silicon Carbide (SiC) thin films in Ultra High Vacuum. The research lead to the discovery that the details of the transition from SiC to graphene, providing, for the first time, atomic resolution images of the different stages of the transformation and a model of the growth. The epitaxial growth of graphene developed by this study is a cost effective procedure to obtain this material directly on Si chips, a breakthrough for the future electronic industry.
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Tight networks of interwoven carbon nanotube bundles are formed in our highly conductive composite. The composite possesses propertiessuggesting a two-dimensional percolative network rather than other reported dispersions displaying three-dimensional networks. Binding nanotubes into large but tight bundles dramatically alters the morphology and electronic transport dynamics of the composite. This enables itto carry higher levels of charge in the macroscale leading to conductivities as high as 1600 S/cm. We now discuss in further detail, the electronic and physical properties of the nanotube composites through Raman spectroscopy and transmission electron microscopy analysis. When controlled and usedappropriately, the interesting properties of these composites reveal their potential for practical device applications. For instance, we used this composite to fabricate coatings, whic improve the properties of an electromagnetic antenna/amplifier transducer. The resulting transducer possesses a broadband range up to GHz frequencies. A strain gauge transducer was also fabricated using changes in conductivity to monitor structural deformations in the composite coatings.
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There is a growing need for new biodiagnostics that combine high throughput with enhanced spatial resolution and sensitivity. Gold nanoparticle (NP) assemblies with sub-10 nm particle spacing have the benefits of improving detection sensitivity via Surface enhanced Raman scattering (SERS) and being of potential use in biomedicine due to their colloidal stability. A promising and versatile approach to form solution-stable NP assemblies involves the use of multi-branched molecular linkers which allows tailoring of the assembly size, hot-spot density and interparticle distance. We have shown that linkers with multiple anchoring end-groups can be successfully employed as a linker to assemble gold NPs into dimers, linear NP chains and clustered NP assemblies. These NP assemblies with diameters of 30-120 nm are stable in solution and perform better as SERS substrates compared with single gold NPs, due to an increased hot-spot density. Thus, tailored gold NP assemblies are potential candidates for use as biomedical imaging agents. We observed that the hot-spot density and in-turn the SERS enhancement is a function of the linker polymer concentration and polymer architecture. New deep Raman techniques like Spatially Offset Raman Spectroscopy (SORS) have emerged that allow detection from beneath diffusely scattering opaque materials, including biological media such as animal tissue. We have been able to demonstrate that the gold NP assemblies could be detected from within both proteinaceous and high lipid containing animal tissue by employing a SORS technique with a backscattered geometry.
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The authors combine nanostenciling and pulsed laser deposition to patterngermanium(Ge)nanostructures into desired architectures. They have analyzed the evolution of the Ge morphology with coverage. Following the formation of a wetting layer within each area defined by the stencil’s apertures, Gegrowth becomes three dimensional and the size and number of Ge nanocrystals evolve with coverage. Micro-Raman spectroscopy shows that the deposits are crystalline and epitaxial. This approach is promising for the parallel patterning of semiconductor nanostructures for optoelectronic applications.
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The combination of nanostenciling with pulsed laser deposition (PLD) provides a flexible, fast approach for patterning the growth of Ge on Si. Within each stencilled site, the morphological evolution of the Ge structures with deposition follows a modified Stranski–Krastanov (SK) growth mode. By systematically varying the PLD parameters (laser repetition rate and number of pulses) on two different substrate orientations (111 and 100), we have observed corresponding changes in growth morphology, strain and elemental composition using scanning electron microscopy, atomic force microscopy and μ-Raman spectroscopy. The growth behaviour is well predicted within a classical SK scheme, although the Si(100) growth exhibits significant relaxation and ripening with increasing coverage. Other novel aspects of the growth include the increased thickness of the wetting layer and the kinetic control of Si/Ge intermixing via the PLD repetition rate.
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We report a new method for the growth of reduced graphene oxide (rGO) on the 316L alloy of stainless steel (SS) and its relevance for biomedical applications. We demonstrate that electrochemical etching increases the concentration of metallic species on the surface and enables the growth of rGO. This result is supported through a combination of Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), density functional theory (DFT) calculations and static water contact angle measurements. Raman spectroscopy identifies the G and D bands for oxidized species of graphene at 1595 cm(-1) and 1350 cm(-1), respectively, and gives an ID/IG ratio of 1.2, indicating a moderate degree of oxidation. XPS shows -OH and -COOH groups in the rGO stoichiometry and static contact angle measurements confirm the wettability of rGO. SEM and AFM measurements were performed on different substrates before and after coronene treatment to confirm rGO growth. Cell viability studies reveal that these rGO coatings do not have toxic effects on mammalian cells, making this material suitable for biomedical and biotechnological applications.
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Bi1.5ZnTa1.5O7 (BZT) has been synthesized using an alkoxide based sol-gel reaction route. The evolution of the phases produced from the alkoxide precursors and their properties have been characterized as function of temperature using a combination of thermogravimetric analysis (TGA) coupled with mass spectrometry (MS), infrared emission spectrometry (IES), X-ray diffraction (XRD), ultraviolet and visible (UV-Vis) spectroscopy, Raman spectroscopy, and N2 adsorption/desorption isotherms. The lowest sintering temperature (600∘C) to obtain phase pure BZT powders with high surface area (14.5m2/g) has been determined from the thermal decomposition and phase analyses.The photocatalytic activity of the BZT powders has been tested for the decolorization of organic azo-dye and found to be photoactive under UV irradiation.The electronic band structure of the BZT has been investigated using density functional theory (DFT) calculations to determine the band gap energy (3.12 eV) and to compare it with experimental band gap (3.02 eV at 800∘C) from optical absorptionmeasurements. An excellent match is obtained for an assumption of Zn cation substitutions at specifically ordered sites in the BZT structure.
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Arc discharge between graphite electrodes under a relatively high pressure of hydrogen yields graphene flakes generally containing 2-4 layers in the inner wall region of the arc chamber. The graphene flakes so obtained have been characterized by X-ray diffraction, atomic force microscopy, transmission electron microscopy, and Raman spectroscopy. The method is eminently suited to dope graphene with boron and nitrogen by carrying out arc discharge in the presence of diborane and pyridine respectively.
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Graphene is a fascinating new nanocarbon possessing, single-, bi- or few- (<= ten) layers of carbon atoms forming six-membered rings. Different types of graphene have been investigated by X-ray diffraction, atomic force microscopy, transmission electron microscopy, scanning tunneling microscopy and Raman spectroscopy. The extraordinary electronic properties of single-and bi-layer graphenes are indeed most unique and unexpected. Other properties of graphene such as gas adsorption characteristics, magnetic and electrochemical properties and the effects of doping by electrons and holes are equally noteworthy. Interestingly, molecular charge-transfer also markedly affects the electronic structure and properties of graphene. Many aspects of graphene are yet to be explored, including synthetic strategies which can yield sufficient quantities of graphene with the desired number of layers.
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Studies of valence bands and core levels of solids by photoelectron spectroscopy are described at length. Satellite phenomena in the core level spectra have been discussed in some detail and it has been pointed out that the intensity of satellites appearing next to metal and ligand core levels critically depends on the metal-ligand overlap. Use of photoelectron spectroscopy in investigating metal-insulator transitions and spin-state transitions in solids is examined. It is shown that relative intensities of metal Auger lines in transition metal oxides and other systems provide valuable information on the valence bands. Occurrence of interatomic Auger transitions in competition with intraatomic transitions is discussed. Applications of electron energy loss spectroscopy and other techniques of electron spectroscopy in the study of gas-solid interactions are briefly presented.
Resumo:
Solid materials can exist in different physical structures without a change in chemical composition. This phenomenon, known as polymorphism, has several implications on pharmaceutical development and manufacturing. Various solid forms of a drug can possess different physical and chemical properties, which may affect processing characteristics and stability, as well as the performance of a drug in the human body. Therefore, knowledge and control of the solid forms is fundamental to maintain safety and high quality of pharmaceuticals. During manufacture, harsh conditions can give rise to unexpected solid phase transformations and therefore change the behavior of the drug. Traditionally, pharmaceutical production has relied on time-consuming off-line analysis of production batches and finished products. This has led to poor understanding of processes and drug products. Therefore, new powerful methods that enable real time monitoring of pharmaceuticals during manufacturing processes are greatly needed. The aim of this thesis was to apply spectroscopic techniques to solid phase analysis within different stages of drug development and manufacturing, and thus, provide a molecular level insight into the behavior of active pharmaceutical ingredients (APIs) during processing. Applications to polymorph screening and different unit operations were developed and studied. A new approach to dissolution testing, which involves simultaneous measurement of drug concentration in the dissolution medium and in-situ solid phase analysis of the dissolving sample, was introduced and studied. Solid phase analysis was successfully performed during different stages, enabling a molecular level insight into the occurring phenomena. Near-infrared (NIR) spectroscopy was utilized in screening of polymorphs and processing-induced transformations (PITs). Polymorph screening was also studied with NIR and Raman spectroscopy in tandem. Quantitative solid phase analysis during fluidized bed drying was performed with in-line NIR and Raman spectroscopy and partial least squares (PLS) regression, and different dehydration mechanisms were studied using in-situ spectroscopy and partial least squares discriminant analysis (PLS-DA). In-situ solid phase analysis with Raman spectroscopy during dissolution testing enabled analysis of dissolution as a whole, and provided a scientific explanation for changes in the dissolution rate. It was concluded that the methods applied and studied provide better process understanding and knowledge of the drug products, and therefore, a way to achieve better quality.