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Povzetek: The surface properties of hydrocarbon polymers are inadequate for numerous applications. Hence, they require alteration via functionalisation with desired functional groups. Hydroxyl groups are often preferred, since they enable appropriate polarity for the irreversible grafting of desired molecules. In this study, the surface kinetics resulting from the treatment of polystyrene with hydroxyl (OH) radicals from the gas phase was fundamentally investigated through a precisely-designed experiment. Polystyrene samples were exposed to various known fluences of OH radicals, and the evolution of surface functional groups versus the OH fluence was monitored using high-resolution X-ray photoelectron spectroscopy (XPS). The fluences of OH radicals varied between 1 × 1018 and 4 × 1023 m−2 in the process of finding a threshold fluence for the formation of specific groups. The surface concentration of carbonyl (C=O) groups could be measured using XPS at a fluence of approximately 5 × 1020 m−2. The C=O groups became measurable at a fluence of approximately 1.5 × 1021 m−2, and carboxyl (COOH)/ester groups at approximately 4 × 1021 m−2. As deduced from the XPS, a concentration of C=O groups at approximately 5 % occurred before the degradation of the aromatic ring. The formation of other oxygen-functional groups required opening of the aromatic ring. The results have been explained using a two-step process, considering available theories vis-a-vis initial stages in the functionalisation of PS with polar functional groups.
Ključne besede: polistiren, kinetika površinske funkcionalizacije, OH radikali, vpliv doze radikalov, časovni razvoj, polystyrene, surface functionalisation kinetics, OH radicals
Objavljeno v DiRROS: 09.11.2023; Ogledov: 257; Prenosov: 110
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Objavljeno v DiRROS: 14.09.2023; Ogledov: 265; Prenosov: 81
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Povzetek: Hysteresis is a general phenomenon regularly observed in various materials. Usually, hysteretic behavior is an intrinsic property that cannot be circumvented in the non-equilibrium operation of the system. Herein, we show that, at least with regard to the hysteretic behavior of phase-separating battery materials, it is possible to enter (deeply) the hysteretic loop at finite battery currents. This newly observed electric response of the electrode, which is inherent to phase-separating materials, is, for the first time, related to its microscopic origin arising from a (significant) share of the active material residing in an intraparticle phase-separated state. This intriguing observation was further generalized by revealing that a phase-separating material can feature (significantly) different chemical potentials at the same bulk lithiation level and temperature when exposed to the same finite current and external voltage hysteresis. Therefore, the intraparticle phase-separated state significantly affected the DC and AC characteristics of the battery. The experimental evidence for entering the intraparticle phase-separated state is supported by thermodynamic reasoning and advanced modeling. The current findings will help advance the understanding, control, diagnostics, and monitoring of batteries composed of phase-separating materials while also providing pertinent motivation for the enhancement of battery design and performance.
Ključne besede: battery, phase-separating materials, Lithium iron phosphate, voltage hysteresis, intraparticle phase-separated
Objavljeno v DiRROS: 06.09.2023; Ogledov: 335; Prenosov: 163
Celotno besedilo (5,07 MB)
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Povzetek: The recombination of neutral oxygen atoms in the ground state on the oxidized nickel samples was studied experimentally in the range of pressures where the maximum density occurs in weakly ionized low-pressure oxygen plasma, i.e. between 40 and 200 Pa. The recombination coefficient was determined in the flowing afterglow. The source of oxygen atoms was plasma sustained in a quartz tube of inner diameter 4.7 mm by a microwave discharge in the surfatron mode. The recombination coefficient was determined in the afterglow chamber, which was a Pyrex tube with an inner diameter of 36 mm. The density of oxygen atoms in the afterglow chamber was varied by adjusting the discharge power, the gas flow, the pressure, and the position of a recombinator. Such flexibility of the experimental system enabled adjustment of the temperature of the oxidized nickel samples independently from the O-atom density in its vicinity or other parameters. The density of oxygen atoms in the afterglow chamber at various system parameters was determined by the Šorli method, which is reliable, and has an accuracy of about 20%. The recombination coefficient was determined by calorimetry. The coefficient was inversely proportional to the square root of the pressure and exponentially to the sample temperature. Systematic measurements performed at various pressures and temperatures enabled empirical formula, which were explained qualitatively by recombination kinetics.
Ključne besede: heterogenous surface recombination, recombination coefficient, nickel, nickel oxide, temperature
Objavljeno v DiRROS: 30.08.2023; Ogledov: 324; Prenosov: 191
Celotno besedilo (2,44 MB)
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Povzetek: Calorimetry is a commonly used method in plasma characterization, but the accuracy of the method is tied to the accuracy of the recombination coefficient, which in turn depends on a number of surface effects. Surface effects also govern the kinetics in advanced methods such as atomic layer oxidation of inorganic materials and functionalization of organic materials. The flux of the reactive oxygen atoms for the controlled oxidation of such materials depends on the recombination coefficient of materials placed into the reaction chamber, which in turn depends on the surface morphology, temperature, and pressure in the processing chamber. The recombination coefficient of a well-oxidized cobalt surface was studied systematically in a range of temperatures from 300 to 800 K and pressures from 40 to 200 Pa. The coefficient increased monotonously with decreasing pressure and increasing temperature. The lowest value was about 0.05, and the highest was about 0.30. These values were measured for cobalt foils previously oxidized with oxygen plasma at the temperature of 1300 K. The oxidation caused a rich morphology with an average roughness as deduced from atomic force images of 0.9 µm. The results were compared with literature data, and the discrepancy between results reported by different authors was explained by taking into account the peculiarities of their experimental conditions.
Objavljeno v DiRROS: 25.08.2023; Ogledov: 312; Prenosov: 150
Celotno besedilo (3,59 MB)
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