985 resultados para Thermal Microscopy
Resumo:
Transparent SrO-2B(2)O(3) (SBO) glasses were fabricated via the conventional melt-quenching technique. X-ray diffraction (XRD) and differential thermal analysis (DTA) studies carried out on the as-quenched glasses confirmed their amorphous and glassy nature, respectively. The thermal parameters were evaluated for the as-quenched glass-plates using non-isothermal DTA experiments. The average values of the activation energies for the glass transition and crystallization of these glasses were 800 +/- 10 kJ/mol and 298 +/- 10 kJ/mol respectively. The values of the kinetic parameters that were obtained by different non-isothermal techniques were in close agreement.
Resumo:
The layered double hydroxides (LDHs) of Co with trivalent cations decompose irreversibly to yield oxides with the spinel structure. Spinel formation is aided by the oxidation of Co(II) to Co(III) in the ambient atmosphere. When the decomposition is carried out under N-2, the oxidation of Co(II) is suppressed, and the resulting oxide has the rock salt structure. Thus, the Co-Al-CO32-/Cl- LDHs yield oxides of the type Co1- Al-x(2x/3)rectangle O-x/3, which are highly metastable, given the large defect concentration. This defect oxide rapidly reverts back to the original hydroxide on soaking in a Na2CO3 solution. Interlayer NO3- anions, on the other hand, decompose generating a highly oxidizing atmosphere, whereby the Co-Al-NO3- LDH decomposes to form the spinel phase even in a N-2 atmosphere. The oxide with the defect rock salt structure formed by the thermal decomposition of the Co-Fe-CO32- LDH under N2, on soaking in a Na2CO3 solution, follows a different kinetic pathway and undergoes a solution transformation into the inverse spinel Co(Co, Fe)(2)O-4. Fe3+ has a low octahedral crystal field stabilization energy and therefore prefers the tetrahedral coordination offered by the structure of the inverse spinel rather than the octahedral coordination of the parent LDH. Similar considerations do not hold in the case of Ga- and In-containing LDHs, given the considerable barriers to the diffusion of M3+ (M=Ga, In) from octahedral to tetrahedral sites owing to their large size. Consequently, the In-containing oxide residue reverts back to the parent hydroxide, whereas this reconstruction is partial in the case of the Ga-containing oxide. These studies show that the reversible thermal behavior offers a competing kinetic pathway to spinel formation. Suppression of the latter induces the reversible behavior in an LDH that otherwise decomposes irreversibly to the spinel.
Resumo:
In this paper we address the fundamental issue of temperature fluctuation during the thermal denaturation (or the unzipping of the two strands on heating) of double stranded (ds) DNA. From our experiments we observe the presence of extremely high thermal fluctuations during DNA denaturation. This thermal fluctuation is several orders higher than the thermal fluctuation at temperatures away from the denaturation temperature range. This fluctuation is absent in single stranded (ss) DNA. The magnitude of fluctuation is much higher in heteropolymeric DNA and is almost absent in short homopolymeric DNA fragments. The temperature range over which the denaturation occurs (i.e., over which the thermal fluctuation is large) depends on the length of the DNA and is largest for the longest DNA.
Resumo:
Lignin was graft copolymerized with methyl methacrylate using manganic pyrophosphate as initiator. This modified lignin was then blended (up to 50 wt%) with low density polyethylene (LDPE) using a small quantity of poly[ethylene-co-(glycidyl methacrylate)] (PEGMA) compatibilizer. The mechanical properties of the blend were substantially improved by using modified lignin in contrast to untreated lignin. Differential scanning calorimetry studies showed loss of crystallinity of the LDPE phase owing to the interaction between the blend components. Thermogravimetric analysis showed higher thermal stability of modified lignin in the domain of blend processing. This suggested that there is scope for useful utilization of lignin, which could also lead to the development of eco-friendly products. (c) 2005 Society of Chemical Industry.
Resumo:
The temperature variation of the coefficient of thermal expansion of caesium bromide has been computed in quasiharmonic approximation and compared with the experimental results.
Resumo:
This thesis comprises four intercomplementary parts that introduce new approaches to brittle reaction layers and mechanical compatibility of metalloceramic joints created when fusing dental ceramics to titanium. Several different methods including atomic layer deposition (ALD), sessile drop contact angle measurements, scanning acoustic microscopy (SAM), three-point bending (TPB, DIN 13 927 / ISO 9693), cross-section microscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS) were employed. The first part investigates the effects of TiO2 layer structure and thickness on the joint strength of the titanium-metalloceramic system. Samples with all tested TiO2 thicknesses displayed good ceramics adhesion to Ti, and uniform TPB results. The fracture mode was independent of oxide layer thickness and structure. Cracking occurred deeper inside titanium, in the oxygen-rich Ti[O]x solid solution surface layer. During dental ceramics firing TiO2 layers dissociate and joints become brittle with increased dissolution of oxygen into metallic Ti and consequent reduction in the metal plasticity. To accomplish an ideal metalloceramic joint this needs to be resolved. The second part introduces photoinduced superhydrophilicity of TiO2. Test samples with ALD deposited anatase TiO2 films were produced. Samples were irradiated with UV light to induce superhydrophilicity of the surfaces through a cascade leading to increased amount of surface hydroxyl groups. Superhydrophilicity (contact angle ~0˚) was achieved within 2 minutes of UV radiation. Partial recovery of the contact angle was observed during the first 10 minutes after UV exposure. Total recovery was not observed within 24h storage. Photoinduced ultrahydrophilicity can be used to enhance wettability of titanium surfaces, an important factor in dental ceramics veneering processes. The third part addresses interlayers designed to restrain oxygen dissolution into Ti during dental ceramics fusing. The main requirements for an ideal interlayer material are proposed. Based on these criteria and systematic exclusion of possible interlayer materials silver (Ag) interlayers were chosen. TPB results were significantly better in when 5 μm Ag interlayers were used compared to only Al2O3-blasted samples. In samples with these Ag interlayers multiple cracks occurred inside dental ceramics, none inside Ti structure. Ag interlayers of 5 μm on Al2O3-blasted samples can be efficiently used to retard formation of the brittle oxygen-rich Ti[O]x layer, thus enhancing metalloceramic joint integrity. The most brittle component in metalloceramic joints with 5 μm Ag interlayers was bulk dental ceramics instead of Ti[O]x. The fourth part investigates the importance of mechanical interlocking. According to the results, the significance of mechanical interlocking achieved by conventional surface treatments can be questioned as long as the formation of the brittle layers (mainly oxygen-rich Ti[O]x) cannot be sufficiently controlled. In summary in contrast to former impressions of thick titanium oxide layers this thesis clearly demonstrates diffusion of oxygen from sintering atmosphere and SiO2 to Ti structures during dental ceramics firing and the following formation of brittle Ti[O]x solid solution as the most important factors predisposing joints between Ti and SiO2-based dental ceramics to low strength. This among other predisposing factors such as residual stresses created by the coefficient of thermal expansion mismatch between dental ceramics and Ti frameworks can be avoided with Ag interlayers.
Resumo:
Controlling the properties of nanostructures requires a detailed understanding of structure, microstructure, and chemistry at ever-decreasing length scales. The modern day transmission electron microscope has thus become an indispensable tool in the study of nanostructures. In this Perspective, we present a brief account of the capabilities of the TEM with some typical examples for characterizing nanostructures. The modern-day TEM has moved from a simple characterization tool to a nanoscale laboratory enabling in situ observation of several fundamental processes at unprecedented resolution levels.
Resumo:
An exact solution for determining the thermal stresses in a finite short cylinder due to an axisymmetric steady temperature field along the curved surface has been given. It is shown that a part of the solution obtained for this problem can be used to determine the thermal stresses in a finite solid cylinder heated over the end surfaces. Numerical results for a finite cylinder symmetrically heated over a portion on the curved surface and heated over the complete end surfaces have been given.
Resumo:
A new equation for predicting the thermal conductivities of organic liquids using dimension-less analysis is given. The equation (Equation Presented) correlates 51 different liquids tested within 11% average error and 17% standard deviation. A comparison of the proposed equation with the available correlations and its application to some industrially important liquids show that this equation can be safely used to calculate the thermal conductivities at 20°C. and 1 atm. pressure for organic liquids of known molecular weight. Cp and ΔHv - the only two parameters for which experimental values must be known for making use of this equation - can be calculated using other well known correlations. The proposed equation is not applicable to inorganic liquids.
Resumo:
The preparation of three different types of carbonates of praseodymium, neodymium and terbium has been described. The carbonates have been characterized by potentiometry, chemical analysis, X-ray crystallography, infra-red spectroscopy and by their thermal behaviour. The thermal decomposition of several carbonates has been studied exhaustively under a variety of conditions and the stoicheiometry, thermodynamics and energetics of the reactions at various stages of decomposition have been examined. The stoicheiometry of the oxides obtained as final products of decomposition has been examined.
Resumo:
A three-dimensional exact solution for determining the thermal stresses in a finite hollow cylinder subject to a steady state axisymmetric temperature field over one of its end surfaces has been given. Numerical results for a hollow cylinder, having lenght to outer diameter ratio equal to one and inner to outer diameter ratio equal to 0.75, subjected to a symmetric temperature variation over the end surfaces of the cylinder have been given.
Resumo:
A method of determining the thermal stresses in a flat rectangular isotropic plate of constant thickness with arbitrary temperature distribution in the plane of the plate and with no variation in temperature through the thickness is presented. The thermal stress have been obtained in terms of Fourier series and integrals that satisfy the differential equation and the boundary conditions. Several examples have been presented to show the application of the method.
Resumo:
A three-dimensional rigorous solution for determining thermal stresses in a finite solid cylinder due to a steady state axisymmetric temperature field over one of its end surfaces is given. Numerical results for a solid cylinder having a length to diameter ratio equal to one and subjected to a symmetric temperature variation over half the radius of the cylinder at the end surfaces are included. These results have been compared with the results of the approximate solution given by W. Nowacki.