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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: 1886; Downloads: 55
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Criticality of depth of intensity modulation and simulation of refractive index profile in thermal lens technique
Mohanachandran Nair Sindhu Swapna, 2020, original scientific article

Keywords: thermal lens, chopper
Published in RUNG: 05.07.2022; Views: 948; Downloads: 0
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16.
Effect of duty cycle on photothermal phenomenon – a thermal lens study
Mohanachandran Nair Sindhu Swapna, 2019, original scientific article

Keywords: Photothermal phenomena Thermal lens technique Optical chopper Duty cycle variation
Published in RUNG: 05.07.2022; Views: 1020; Downloads: 0
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Carbon nanoparticles assisted energy transport mechanism in leaves: A thermal lens study
Mohanachandran Nair Sindhu Swapna, 2019, original scientific article

Abstract: In the world of increasing population and pollution due to carbon emissions, the research for effective utilization of futile diesel soot for fruitful applications has become a necessity for a sustainable development. The contribution to pollution from vehicles and industries due to the aging of engines has caused a crisis. Carbon nanoparticles (CNPs) have been the subject of interest because of their good physical, chemical, and biological properties. The present work investigates the role of CNPs produced by internal combustion engines on the energy transport mechanism among leaf pigments using the sensitive and nondestructive single beam thermal lens technique. The studies reveal the absorption changes by various chlorophyll pigments with the concentration of CNPs sprayed on the leaves. Though for low concentrations CNPs lower the photon absorbance by chlorophyll pigments, the effect gets reversed at higher concentrations. The variation of thermal diffusivity with CNP concentration and its role in the energy transport mechanism among chlorophyll pigments are also studied. It is found that CNP concentrations of 625-2500mg/l are good for better intra-pigment energy transport leading to increased rate of photosynthesis and plant yield and thereby helping in attaining food security. The variation of CNP assisted energy transport among leaf pigments on the production of nicotinamide adenine dinucleotide phosphate (NADPH) and carbohydrates is also studied with ultraviolet (UV) and near-infrared (NIR) spectroscopy.
Keywords: carbon nanoparticle, soot, energy transport, thermal lens, photosynthesis
Published in RUNG: 05.07.2022; Views: 1072; Downloads: 0
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