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11.
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: 2594; Downloads: 59
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12.
Thermal diffusivity downscaling of molybdenum oxide thin film through annealing temperature-induced nano-lamelle formation: a photothermal beam deflection study
S. Soumya, Vimal Raj, Mohanachandran Nair Sindhu Swapna, Sankaranarayana Iyer Sankararaman, 2021, original scientific article

Abstract: The present work proposes a method of downscaling the thermal diffusivity (α) of MoO3 thin films through annealing temperature-induced nano-lamelle formation. The thermal diffusivity modification of the MoO3 films, prepared by the doctor blade method, is investigated by the sensitive transverse photothermal beam deflection technique. The X-ray diffraction analysis confirms the structural phase transformation from monoclinic to orthorhombic in the films annealed from 300 to 450 °C. The thermal induced anisotropy of the film is evident from the variation of the morphology index and texture coefficient. The field emission scanning electron microscopic analysis unveils the morphology modifications from blocks to the nano-lamelle structure with layers of average thickness ~ 77 nm. The thermal diffusivity measurement reveals a 53% reduction upon annealing the film to 450 °C. The drastic reduction is achieved through the annealing temperature-induced nano-lamelle formation and the phase transformation from monoclinic to orthorhombic in the MoO3 films.
Keywords: thermal diffusivity, molybdenum oxide, thin film, nano-lamelle, photothermal beam deflection
Published in RUNG: 04.07.2022; Views: 1408; Downloads: 26
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13.
Thermal diffusivity of molybdenum oxide nanowire film: a photothermal beam deflection study
Mohanachandran Nair Sindhu Swapna, 2021, original scientific article

Abstract: The paper reports the preparation of thin film with MoO3 nanowires (NWs) by the doctor blade method and the study of its thermal diffusivity (α) by the sensitive photothermal beam deflection (PTD) method. When the Field Emission Scanning Electron Microscopic and Atomic Force Microscopic analysis unveil its morphology as NW bundles, the X-ray diffraction analysis reveals the structure to be orthorhombic. The NWs formed are of diameter ~ 20 nm and length up to 5 μm. The standardization of the transverse PTD setup is done by determining the value of α of iron, which agrees well with literature reports. The thermal diffusivity of MoO3 NW film is obtained as 0.0036 cm2 /s, which is 9.48% of its bulk counterpart. The reduction in the thermal diffusivity of NW makes it a suitable candidate for thermoelectric applications.
Keywords: Nanowires Molybdenum oxide Photothermal beam deflection Thermal diffusivity
Published in RUNG: 04.07.2022; Views: 1493; Downloads: 0
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14.
Optimization of PTD system for characterization of transparent and semi-transparent samples
Hanna Budasheva, Dorota Korte, Mladen Franko, 2022, published scientific conference contribution abstract

Keywords: beam deflection spectrometry, materials characterisation, procedure optimisation
Published in RUNG: 01.07.2022; Views: 1432; Downloads: 6
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Study of Drug Diffusion rate by beam deflection technique
Mohanachandran Nair Sindhu Swapna, 2017, original scientific article

Abstract: Drug administration is an unavoidable part of treatment. When a drug is administered orally or intravenously, it gets absorbed into the blood stream. The rate and efficiency of absorption depend on the route of administration. When a drug is administered through the oral route, it penetrates the epithelial cells of the intestinal mucosa. The diffusion of the drug into the blood stream depends on various parameters, such as concentration, temperature, and the nature of the mucous membrane. The passive diffusion of drugs is found to obey Fick’s law. Water soluble drugs penetrate the cell membrane through aqueous channel or pores. Hence, the study of diffusion of drugs into the water and finally into the blood stream is important. An attempt has been made to study the diffusion of the drug in water as 60% to 80% of human body is water. For the study of drug diffusion in water, a commonly used cough syrup of specific gravity 1.263 is used. It is found that the diffusion rate increases with the concentration of the drug.
Keywords: laser beam deflection, diffusion coefficient, Fick’s law, sodium chloride, syrup
Published in RUNG: 30.06.2022; Views: 1406; Downloads: 0
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