1. Microstructure and surface topography study of nanolayered TiAlN/CrN hard coatingPeter Panjan, Peter Gselman, Matjaž Panjan, Tonica Bončina, Aljaž Drnovšek, Mihaela Albu, Miha Čekada, Franc Zupanič, 2022, original scientific article Abstract: The microstructure and surface topography of PVD hard coatings are among the most
important properties, as they significantly determine their mechanical, tribological and other properties. In this study, we systematically analyzed the microstructure and topography of a TiAlN/CrN
nanolayer coating (NL-TiAlN/CrN), not only because such coatings possess better mechanical and
tribological properties than TiAlN and CrN monolayer coatings, mainly because the contours of the
individual layers, in the cross-sectional STEM or SEM images of such coatings, make it easier to
follow topographic and microstructural changes that occurred during its growth. We investigated
the effects of the substrate rotation modes on the microstructure and surface topography of the
NL-TiAlN/CrN coating, as well as on the periodicity of the nanolayer structure. The influence of the
substrate material and the ion etching methods were also studied, while special attention was given to
the interlayer roughness and influence of non-metallic inclusions in the steel substrates on the growth
of the coating. The topographical features of the NL-TiAlN/CrN coating surface are correlated with
the observations from the cross-sectional TEM and FIB analysis. Selected non-metallic inclusions,
covered by the NL-TiAlN/CrN coating, were prepared for SEM and STEM analyses by the focused
ion beam. The same inclusions were analyzed prior to and after deposition. We found that substrate
rotation modes substantially influence the microstructure, surface topography and periodicity of the
NL-TiAlN/CrN layer. Non-metallic inclusions in the substrates cause the formation of shallow craters
or protrusions, depending on their net removal rates during the substrate pretreatment (polishing
and ion etching), as compared to the matrix. Keywords: magnetron sputtering, nanolayer hard coatings, growth defects, surface topography, interlayer roughness, non-metallic inclusion, focused ion beam (FIB), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM) Published in DKUM: 19.03.2025; Views: 0; Downloads: 3
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2. Hybrid nanostructures of ▫$Fe_3O_4$▫ and Au prepared via coprecipitation and ultrasonic spray pyrolysisLan Kresnik, Peter Majerič, Darja Feizpour, Klementina Pušnik Črešnar, Rebeka Rudolf, 2024, original scientific article Abstract: The coupled processes of coprecipitation and ultrasonic spray pyrolysis (USP) were used to synthesize Fe3O4-Au hybrid nanostructures. The first coprecipitation method enabled the synthesis of Fe3O4 nanoparticles by mixing iron salts’ ions (Fe2+ and Fe3+) and ammonia as the base, and USP was used as the coating process of the Fe3O4 nanoparticles with Au. The formatted hybrid nanostructures consist of Fe3O4 nanoparticles that have Au on their surface in the form of gold nanoparticles (AuNPs). AuNPs have a crystalline structure and range in size from 10 to 200 nm. Additional characterization techniques, including ICP-OES, TEM, SEM, EDS, DLS, zeta potential, and room temperature magnetic hysteresis loops, were used to determine the chemical, physical, and magnetic properties of the Fe3O4 nanoparticles and hybrid nanostructures. It was found that USP produces separate AuNPs too (not just on the Fe3O4 surface), suggesting a bimodal formation of AuNPs. The zeta potential of the Fe3O4 nanoparticles showed poor stability (−15 mV), indicating a high tendency to aggregate, and the zeta potential of the hybrid nanostructures was also very low (≅0), which, comparatively means even worse stability. The saturation magnetization of the Fe3O4 nanoparticles was 35 emu/g, which is relatively lower than that of bulk Fe3O4, while the saturation magnetization of the hybrid nanostructures was significantly lower (0.1 emu/g) compared to the Fe3O4 nanoparticles. Keywords: magnetic NPs, gold NPs, transmission electron microscopy, magnetic properties Published in DKUM: 29.11.2024; Views: 0; Downloads: 14
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3. Autolysis affects the iron cargo of ferritins in neurons and glial cells at different rates in the human brainSowmya Sunkara, Snježana Radulović, Saška Lipovšek Delakorda, Christoph Birkl, Stefan Eggenreich, Anna Maria Birkl-Toeglhofer, Maximilian Schinagl, Daniel Funk, Michael Stöger-Pollach, Johannes Haybaeck, Walter Gössler, Stefan Ropele, Gerd Leitinger, 2023, original scientific article Abstract: Iron is known to accumulate in neurological disorders, so a careful balance of the iron concentration is essential for healthy brain functioning. An imbalance in iron homeostasis could arise due to the dysfunction of proteins involved in iron homeostasis. Here, we focus on ferritin—the primary iron storage protein of the brain. In this study, we aimed to improve a method to measure ferritin-bound iron in the human post-mortem brain, and to discern its distribution in particular cell types and brain regions. Though it is known that glial cells and neurons differ in their ferritin concentration, the change in the number and distribution of iron-filled ferritin cores between different cell types during autolysis has not been revealed yet. Here, we show the cellular and region-wide distribution of ferritin in the human brain using state-of-the-art analytical electron microscopy. We validated the concentration of iron-filled ferritin cores to the absolute iron concentration measured by quantitative MRI and inductively coupled plasma mass spectrometry. We show that ferritins lose iron from their cores with the progression of autolysis whereas the overall iron concentrations were unaffected. Although the highest concentration of ferritin was found in glial cells, as the total ferritin concentration increased in a patient, ferritin accumulated more in neurons than in glial cells. Summed up, our findings point out the unique behaviour of neurons in storing iron during autolysis and explain the differences between the absolute iron concentrations and iron-filled ferritin in a cell-type-dependent manner in the human brain. Keywords: ferritin, human brain, energy-filtered transmission electron microscopy, quantitative magnetic resonance imaging, autolysis Published in DKUM: 20.03.2024; Views: 228; Downloads: 38
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4. Microstructure of NiTi orthodontic wires observations using transmission electron microscopyJanko Ferčec, Darja Feizpour, Borut Buchmeister, Franc Rojko, Bojan Budič, Borut Kosec, Rebeka Rudolf, 2014, original scientific article Abstract: This work presents the results of the microstructure observation of six different types of NiTi orthodontic wires by using Transmission Electron Microscopy (TEM). Within these analyses the chemical compositions of each wire were observed in different places by applying the EDS detector. Namely, the chemical composition in the orthodontic wires is very important because it shows the dependence between the phase temperatures and mechanical properties. Micro- structure observations showed that orthodontic wires consist of nano-sized grains containing precipitates of Ti2Ni and/or TiC. The first precipitated Ti2Ni are rich in Ti, while the precipitated TiC is rich in C. Further investigation showed that there was a difference in average grain size in the NiTi matrix. The sizes of grains in orthodontic wires are in the range from approximately 50 to 160 nm and the sizes of precipitate are in the range from 0,3 μm to 5 μm. Keywords: orthodontic wires, nickel-titanium orthodontic wire, NiTi wire, shape memory alloys, SMA wires, microstructure, transmission electron microscopy, TEM, average grain size Published in DKUM: 03.07.2017; Views: 1524; Downloads: 127
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5. Synthesis of NiTi/Ni-TiO[sub]2 composite nanoparticles via ultrasonic spray pyrolysisPeter Majerič, Rebeka Rudolf, Ivan Anžel, Jelena Bogovic, Srečko Stopić, Bernd Friedrich, 2015, original scientific article Abstract: In this paper we present the production of NiTi/Ni-TiO2 composite nanoparticles via the synthesis method called ultrasonic spray pyrolysis (USP). The precursor solution for the synthesis of spherical NiTi particles was prepared from an orthodontic wire with a chemical composition of Ni (amount fraction x = 51.46 %) and Ti (x = 48.54 %). TEM microscopy, in combination with EDX analyses, was used for a detailed characterization of the obtained NiTi nanoparticles. The results showed the nanoparticle sizes ranging from 60 nm to 600 nm, depending on the parameters of the production procedure. This showed the versatility of the new USP synthesis procedure, proving its usefulness for different materials and applications. Keywords: ultrasonic spray pyrolysis, NiTi/Ni-TiO2 composite nanoparticles, characterization, Transmission electron microscope (TEM), TEM microscopy Published in DKUM: 23.03.2017; Views: 1610; Downloads: 134
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