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NONDESTRUCTIVE THERMAL, OPTICAL, CHEMICAL AND STRUCTURAL CHARACTERIZATION OF ADVANCED MATERIALS BY OPTOTHERMAL TECHNIQUES
Hanna Budasheva, doctoral dissertation

Abstract: Advanced materials are promising ones in application in fields where it is necessary to decrease energy consumption and ensure better performance at a lower cost. They are materials, which have enhanced properties compared to conventional materials in the field of their applications.1 The huge group of them contributes significantly to every aspect of our lives. Among them, chosen for the present study, are resins for passive sampling of iron species in natural water and sediments, anticorrosive coatings, and multilayered polysaccharide aerogels for medical applications. The composition and structure of each material determine its chemical, mechanical and physical properties, consequently their performance.2 The ability to use advanced materials in areas where their impact will be significant is largely dependent on the ability to precisely determine their characteristics to identify their properties that are either unique or has a better value. Therefore, the development of new methods or improvement of already known ones will make a great contribution to the development of the fields of application of the selected materials. The present study is focused on the examination of the chosen materials by determining their optical, chemical, thermal and structural properties for applying them further in the desired applications. To provide the needed characterization, optothermal techniques such as optothermal beam deflection spectrometry (BDS) and thermal lens spectrometry (TLS) are developed and applied. This dissertation is composed of the following chapters: introduction, theoretical background, optothermal techniques, research goal, part I (gels for passive sampling of iron species in natural water and sediments), part II (anticorrosive coatings), part II (polysaccharide aerogels), references. The core of this dissertation is presented in chapters 5 to 7. Each of the chapters separately covers the information about a selected group of advanced materials, including the sections describing sample preparation, developing the required characterization method, results, and conclusion. The connection link of these chapters is the study of the diffusion process of iron into different types of binding gels in passive samplers; external composites through the anticorrosive layers; drugs into the surrounding during the drug delivery process. In Part I, the BDS method for the study was chosen, it was optimized, and a detailed protocol was developed for the determination of iron in passive sampler gels. The iron residues in the initial solutions were checked by a suitably tuned TLS method. The developed technique was applied to get the iron species distribution in the gel samples deposited in the sediments in the Vrtojbica River. The method was applied to the gels applied on ice from Antarctica in order to obtain the iron species distribution on its surface as well. The obtained results were validated using the TLS, UV-Vis and ICP-MS methods. The chapter contains the analysis of the Fe diffusion depth into the resin sampler, which is presented for the first time. The information is obtained by using the mathematical model and applying it to the obtained practical results by frequency scanning of the gels. The crucial information about the thermal properties of their layers containing Fe-ions from the fitting procedure was extracted. On the basis of these results, information about the diffusion depth of Fe inside the gels was obtained, which has not been previously described in the literature. In Part II, the porosity in the anticorrosion coatings on the basis of their thermal parameters was determined. For the first time, the opened porosity was extracted from the total one. The analysis of Si/Zr-based hybrid sol-gel coatings has shown that the addition of cerium salts into the sol-gel matrix produces changes in its physical, chemical and corrosion properties. And it was found that the sample with the biggest amount of incorporated zirconium and loaded with cerium has the lowest values of porosity and, hence, the best barrier properties of the coating. The obtained thermal parameters of the Si/Zr-based hybrid sol-gel coatings by BDS were validated by the use of the photothermal radiometry method. On the other hand, the analysis of siloxane methacrylate coating has shown that the sol-gel hybrid methodology offers an important route for modification of thermal properties by a combination of inorganic to organic contents where the former than as an integral part of the coating network affects the thermal properties without the need for introducing fillers or nanoparticles. In Part III, the multilayered structure of the samples, containing hyaluronic acid, amoxicillin and fucoidan layers deposited on stainless support has been analyzed by the use of the BDS technique. The thermal parameters of each layer were determined, as well as their thickness. The results revealed the diffusion between neighboring layers and followed changes in the properties of the whole sample, which is reflected in its thermal properties. Such data for multilayered materials, which potentially can be used for drug delivery systems, are presented for the first time. Presented results indicated the ability of the BDS system for the chemical characterisation of the solid materials, the detection of their thermal parameters; investigation of total, opened and closed porosity; determining the thickness of layers in multilayered structures. The TLS method served as the validating one for the purpose of getting comprehensive information in liquid samples about their chemical composition. In summary, this dissertation explores alternative ways to apply optothermal methods to various areas of advanced materials to characterize them in order to improve their initial properties.
Keywords: optothermal beam deflection spectrometry, thermal lens spectrometry, diffusive gradients in thin films, iron species, anticorrosive layers, porosity, polysaccharide aerogels, multilayered structures
Published in RUNG: 29.08.2022; Views: 3647; Downloads: 65
.pdf Full text (5,46 MB)

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Absolute Porosity Analysis in Carbon Allotropic Nanofluids: A Sankar–Swapna Model Approach
Mohanachandran Nair Sindhu Swapna, SREEJYOTHI S, Sankararaman S, 2020, original scientific article

Abstract: Porous materials have gained significant attention in recent years as a class of material exhibiting interesting chemical and physical properties. The existing methods of porosity analysis have limitations that prevent absolute porosity measurement. Hence, a technique independent of surface physical properties alone can give the absolute porosity of the material. The porosity greatly influences the thermal diffusivity of a material. The manuscript is the first report of employing the Sankar–Swapna model for analyzing the porosity variations in carbon allotropic nanofluids. The model helps not only in getting information about the absolute porosity variations among samples, but also suggests morphological modifications through the thermal diffusivity study using the sensitive single-beam thermal lens technique. The variations in thermal diffusivity and absolute porosity values are also correlated to morphological modifications based on the theoretical model and thereby proposing this as a surrogate method for absolute porosity analysis.
Keywords: absolute porosity, Sankar–Swapna model, thermal diffusivity, thermal lens, thermal conductivity
Published in RUNG: 04.07.2022; Views: 2125; Downloads: 0
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Meshless modeling of thermo-mechanics of low-frequency electromagnetic direct chill casting
Boštjan Mavrič, 2017, doctoral dissertation

Abstract: The aim of this dissertation is to devise a meshless model describing the thermomechanical phenomena, which occur during DC casting of aluminium alloys under the influence of electromagnetic stirring. The thermoemchanical phenomena are important, because they can cause several type of defects, which can significantly deteriorate the quality of the resulting billet. The two most important of them are the hot tearing, which causes cracks to appear in the mushy zone, and the porosity, which demonstrates itself as micrometer sized voids in the microstructure of the billet. To calculate the stresses and strains, a computational model of the stationary state of the process, stated in axial symmetry, is formulated. It uses Eulerian formulation by fixing the computational domain to the mold of the casting device allowing the material to move through the computational domain. The stresses are calculated from the stress equilibrium equations. The small strain approximation is used to consider the three contributions to strain. The strain consists of the thermal strain, which is caused by the inhomogeneous thermal profile in the billet, the viscoplastic strain, which is caused by the irreversible deformation because of the large stresses occurring in the billet, and the elastic strain. The spatial discretization of the governing equations is performed by local radial basis function collocation method (LRBFCM) and the temporal discretization is achieved by the method of lines with implicit Euler formula. The method used for spatial discretization uses radial basis functions augmented by monomials to approximate the solution values on localized stencils. This approximation is used to construct the discretization coefficients of the differential operators present in the model. A flexible framework for formulation of multiphysics problems is developed to use the obtained discretization coefficients to construct the temporal discretization of the governing equations. The node arrangement, on which the spatial discretization is performed, was generated by a point-repel algorithm. The performance of the method is tested on several benchmark test cases. The accuracy of the discretization is estimated by comparing the analytic and the numerical solution to several stationary problems in thermomechancis. Of special interest is the performance of the method with respect to the choice of the shape parameter, which determines the spatial scale of the radial basis functions. Besides this, the dependence of the condition number of the interpolation matrix on the shape parameter is studied. The condition number is found fit to replace the condition number as the shape-determining free parameter of the method. The implementation of the solver of time dependent problems is tested on problem of thermoelasticity, which couples the thermal transport with the elastic waves. The results of the problem are compared with the finite element method, showing good agreement of the two methods. The results are also compared with the results obtained by meshless local Petrov-Galerkin method and the proposed local collocation method demonstrated significantly better solution quality in the studied case. The performance of the solver used to solve the system of nonlinear equations given by the viscoplastic constitutive equations is estimated on a quasi zero-dimensional problem. The results are found to match perfectly. Solution of a more complicated problem is obtained with the proposed method and the finite-element method, both methods giving practically the same solution, although some serious limitations of the chosen finite element solver are exposed during the selection of the problem parameters. Finally, the devised method is applied to the problem of DC casting of aluminium alloys. The thermomechanical model relies on a model of heat and mass transfer to obtain the input fields needed in the solver. The required fields are: temperature, pressure, liquid
Keywords: thermomechanics, viscoplasticity, aluminium alloys, direct-chill casting, electromagnetic stirring, hot tearing, porosity, meshless methods, local collocation method, radial basis functions, shape parameter
Published in RUNG: 28.06.2017; Views: 7166; Downloads: 263
.pdf Full text (21,30 MB)

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