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

Opis: 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.
Ključne besede: optothermal beam deflection spectrometry, thermal lens spectrometry, diffusive gradients in thin films, iron species, anticorrosive layers, porosity, polysaccharide aerogels, multilayered structures
Objavljeno v RUNG: 29.08.2022; Ogledov: 2354; Prenosov: 58
.pdf Celotno besedilo (5,46 MB)

3.
Coevaporation of doped inorganic carrier-selective layers for high-performance inverted planar perovskite solar cells
Jiexuan Jiang, Andraž Mavrič, Nadiia Pastukhova, Matjaž Valant, Qiugui Zeng, Zeyu Fan, Beibei Zhang, Yanbo Li, 2022, izvirni znanstveni članek

Opis: Inorganic carrier selective layers (CSLs), whose conductivity can be effectively tuned by doping, offer low-cost and stable alternatives for their organic counterparts in perovskite solar cells (PSCs). Herein, we employ a dual-source electron-beam co-evaporation method for the controlled deposition of copper-doped nickel oxide (Cu:NiO) and tungsten-doped niobium oxide (W:Nb2O5) as hole and electron transport layers, respectively. The mechanisms for the improved conductivity using dopants are investigated. Owing to the improved conductivity and optimized band alignment of the doped CSLs, the all-inorganic-CSLs-based PSCs achieves a maximum power conversion efficiency (PCE) of 20.47%. Furthermore, a thin titanium buffer layer is inserted between the W:Nb2O5 and the silver electrode to prevent the halide ingression and improve band alignment. This leads to a further improvement of PCE to 21.32% and a long-term stability (1200 h) after encapsulation. Finally, the large-scale applicability of the doped CSLs by co-evaporation is demonstrated for the device with 1 cm2 area showing a PCE of over 19%. Our results demonstrate the potential application of the co-evaporated CSLs with controlled doping in PSCs for commercialization.
Ključne besede: carrier selective layers, Cu-doped nickel oxide, electron-beam evaporation, perovskite solar cells, W-doped niobium oxide
Objavljeno v RUNG: 17.03.2022; Ogledov: 2024; Prenosov: 121
.pdf Celotno besedilo (1,38 MB)
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4.
Taming the topology of calix[4]arene-based 2D-covalent organic frameworks : interpenetrated vs noninterpenetrated frameworks and their selective removal of cationic dyes
Bikash Garai, Dinesh Shetty, Tina Škorjanc, Felipe Gándara, Nawavi Naleem, Sabu Varghese, Sudhir Kumar Sharma, Maria Baias, Ramesh Jagannathan, Mark Anthony Olson, 2021, izvirni znanstveni članek

Opis: A bowl-shaped calix[4]arene with its exciting host–guest chemistry is a versatile supramolecular building block for the synthesis of distinct coordination cages or metal–organic frameworks. However, its utility in the synthesis of crystalline covalent organic frameworks (COFs) remains challenging, presumably due to its conformational flexibility. Here, we report the synthesis of a periodic 2D extended organic network of calix[4]arenes joined by a linear benzidine linker via dynamic imine bonds. By tuning the interaction among neighboring calixarene units through varying the concentration in the reaction mixture, we show the selective formation of interpenetrated (CX4-BD-1) and non-interpenetrated (CX4-BD-2) frameworks. The cone-shaped calixarene moiety in the structural backbone allows for the interweaving of two neighboring layers in CX4-BD-1, making it a unique example of interpenetrated 2D layers. Due to the high negative surface charge from calixarene units, both COFs have shown high performance in charge-selective dye removal and an exceptional selectivity for cationic dyes irrespective of their molecular size. The charge distribution of the COFs and the resulting selectivity for the cationic dyes were further investigated using computational methods.
Ključne besede: dyes and pigments, covalent organic frameworks, adsorption, layers, chemical structure
Objavljeno v RUNG: 16.03.2021; Ogledov: 2353; Prenosov: 0
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Characterization of organic semiconductor thin layers by transient photocurrent spectroscopy
Nadiia Pastukhova, Egon Pavlica, Gvido Bratina, 2019, objavljeni povzetek znanstvenega prispevka na konferenci

Ključne besede: organic semiconductors, thin layers, spectroscopy
Objavljeno v RUNG: 10.02.2020; Ogledov: 3254; Prenosov: 0
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7.
Morphous aluminium oxide : a promising candidate for a photoanode protection layer
Andraž Mavrič, Chunhua Cui, Matjaž Valant, 2019, objavljeni povzetek znanstvenega prispevka na konferenci

Ključne besede: aluminium oxide, metal oxides, protection layers
Objavljeno v RUNG: 10.02.2020; Ogledov: 3622; Prenosov: 0
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8.
Characterization of organic semiconductor thin layers by transient photocurrent spectroscopy
Nadiia Pastukhova, Egon Pavlica, Gvido Bratina, 2019, objavljeni povzetek znanstvenega prispevka na konferenci

Ključne besede: organic semiconductors, thin layers, spectroscopy
Objavljeno v RUNG: 10.02.2020; Ogledov: 3327; Prenosov: 0
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9.
Evidence of enhanced photocurrent response in corannulene films
Nadya Patukhova, Layla Martin Samos, Egon Pavlica, Gvido Bratina, 2017, izvirni znanstveni članek

Opis: Photoconductivity spectra measured in non-crystalline corannulene thin layers are compared to optical absorption in solution phase and thin films. The unexpected enhanced photoconductivity is correlated with GW–BSE theoretical predictions of corannulene gas-phase excitonic spectra. Theoretical analysis reveals a consistent contribution involving transitions to Super Atomic Molecular Orbitals (SAMOs), a unique set of diffuse orbitals typical of curved conjugated constructs. Results suggest SAMO population via direct photoexcitation as a potential mechanism towards exploiting these diffuse orbitals as conducting channels in suitably assembled quantum nanostructures or solids.
Ključne besede: Coranulene, photoconductivity, thin layers, photoexcitation
Objavljeno v RUNG: 26.09.2017; Ogledov: 4021; Prenosov: 204
.pdf Celotno besedilo (644,91 KB)

10.
Introduction to Electronic Properties and Dynamics of Organic Complexes as Self‐Assembled Monolayers
Maddalena Pedio, 2017, samostojni znanstveni sestavek ali poglavje v monografski publikaciji

Opis: Self‐assembled monolayers (SAMs) of organic‐conjugated transition metal complexes on surfaces is a focus of both device engineering and basic science, since it is a key factor in nearly all important aspects of device performances, including operation voltages, degradation, and efficiency. The huge amount of literature results related to the first monolayer, and reorganization and self‐assembling processes are due to the general accepted result that structural and chemical properties of the first monolayer are the key parameters for controlled thin film growth. Optical and magneto‐electronic properties are intimately connected, and the accurate determination of electronic levels, excitation, and relaxation dynamics is mandatory for the optimization of electronic, photovoltaic, and opto‐electronic devices. Quite a number of electronic states is generated by the interaction of light with complex organic molecules. Time‐resolved spectroscopies are a new investigation tool that gives the possibility of correctly addressing their origin and life time. Examples of prototypical systems are presented and discussed. We review on complementary techniques, trying to single out how different approaches are fundamental to fully characterize these complex systems.
Ključne besede: self‐assembled monolayer (SAM), surface structures molecular layers, nanotechnology, electronic properties, spectroscopies, time resolved
Objavljeno v RUNG: 12.06.2017; Ogledov: 4764; Prenosov: 208
.pdf Celotno besedilo (5,78 MB)

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