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Search results for: SINGLE-CRYSTAL X-RAY STUDY
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Investigation of the structural and thermal properties of aluminum-rich Ca–Al–Si–O–N glasses
PublicationIn this paper, we investigate the structure and thermal properties of aluminum-rich transparent Ca–Al–Si–O–N glasses. The obtained glasses were prepared by a traditional melt-quenching technique at 1650 °C using AlN as the nitrogen source. The obtained glasses have a nAl/nSi>1 and contain up to 17 eq.% of N. The structure of the glasses was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, infrared, and Raman...
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Modification of TiO2 nanotubes by graphene–strontium and cobalt molybdate perovskite for efficient hydrogen evolution reaction in acidic medium
PublicationHerein, we demonstrate that modification of TiO2 nanotubes with graphene–strontium and cobalt molybdate perovskite can turn them into active electrocatalysts for hydrogen evolution reaction (HER). For this purpose, a simple method of hydrothermal synthesis of perovskites was developed directly on the TiO2 nanotubes substrate. Moreover, the obtained hybrids were also decorated with graphene oxide (GO) during one-step hydrothermal...
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Fatigue Bending of V-Notched Cold-Sprayed FeCoCrNiMn Coatings
PublicationCold-spray coatings were produced by FeCoCrNiMn high-entropy alloy powders deposited on carbon steel substrate. The coatings were realized at intermediate temperature and high pressure (at 1100 °C and 7 MPa). The coating microstructure was characterized by scanning electron microscopy and X-ray diffraction, revealing a very dense deposition and high flattening ratio of the splatted particles. This had a large influence on the...
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3D Hierarchical Boron-Doped Diamond-Multilayered Graphene Nanowalls as an Efficient Supercapacitor Electrode
PublicationSynthesis of stable hybrid carbon nanostructure for high-performance supercapacitor electrode with long life-cycle for electronic and energy storage devices is a real challenge. Here, we present a one-step synthesis method to produce conductive boron-doped hybrid carbon nanowalls (HCNWs), where sp2-bonded graphene has been integrated with and over a three-dimensional curved wall-like network of sp3-bonded diamond. The spectroscopic...
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Boron Difluoride Complexes of Carbamoyl Meldrum's Acids
Publication5-[Hydroxy(aryl/alkylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-diones react with BF3•Et2O in mild conditions leading to the formation of boron difluoride complexes of carbamoyl Meldrum's acids. The X-ray structure has been obtained for one representative complex. The obtained new compounds are fairly stable at standard ambient conditions and easily isolable.
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OPTIMIZATION OF NASICON PREPARATION METHOD
PublicationNasicon is a solid conductor which has an ability to conduct Na+ ions and it is used in solid gas sensors. In this article a method of Nasicon preparation appropriate for gas sensing application by solgel technique is presented. Influence of the fabrication process parameters on properties of obtained samples was determined. Results of X-Ray diffraction, density, porosity, conductivity, and activation energies measurement are presented.
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The effects of bifunctional linker and reflux time on the surface properties and photocatalytic activity of CdTe quantum dots decorated KTaO3 composite photocatalysts
PublicationNovel CdTe-KTaO3composite photocatalysts were successfully synthesized by using thioglycolic acid(TGA) or 3-mercaptopropionic acid (MPA) as linker molecules which facilitated attachment of CdTequantum dots to the surface of KTaO3nanocubes. The as-prepared photocatalysts were characterizedby UV–vis diffuse reflectance spectroscopy (DRS), X-ray diffraction (XRD), scanning electron microscopy(SEM), transmission electron microscopy...
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Curing epoxy with electrochemically synthesized Zn Fe3-O4 magnetic nanoparticles
PublicationCathodic electrodeposition (CED) was applied in synthesis of undoped and zinc (Zn) doped Fe3O4 nanoparticles. Changes in the lattice structure of nanoparticles were monitored using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) supported by dispersive X-ray spectrometry (EDS), and vibrating sample magnetometry (VSM). Detailed analyses explored the formation of ZnxFe3–xO4 nanoparticles with x ≈ 0.1,...
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Substrate characterization in a electrochemically derived Manganium-Cobaltium thin films
Open Research DataManganium-Cobaltium thin films were electrochemically deposited on a Ni foams subsrates in a one-step process at −1.1 V vs. Ag/AgCl in an aqueous solution of differently concentrated Mn(NO3)2·4H2O and Co(NO3)2·6H2O with the deposition time limited by charges of 60, 120, and 200 mC at 25 °C. The concentration ratios of Mn(NO3)2·4H2O to Co(NO3)2·6H2O...
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XPS study of the YST ceramics
Open Research DataYttrium-doped strontium titanate was prepared via conventional solid-state reaction method from Y2O3 (Sigma Aldrich, 99,9%), TiO2 (Sigma Aldrich, 99%) and SrCO3 (Sigma Aldrich,98%). For comparision, two other techniques were used for synthesis: Pechini and wet methods. Both kind of samples were measured, after and before reduction process (in a hydrogen)....
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High-conducting Bi4V2-xFexO11-δ ceramics containing Fe2O3 nanocrystals: Structure and properties
PublicationThe topography, structure, thermal, magnetic, and electrical properties of Bi4V2-xFexO11-δ ceramics substituted with x = 0.5 and 0.7 Fe were studied. The microscope analysis showed the presence of iron-rich nanocrystals formed on the Bi-Fe-V-O grains. The X-ray diffraction studies confirmed that grains are built mostly of tetragonal Bi4V1.5Fe0.5O10.5 phase. Thermal properties analysis showed an order-disorder type γ ↔ γʹ phase...
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Fabrication and Study of BiNbO4 Ceramics
PublicationAim of the present research was to fabricate and study crystalline structure as well as dielectric properties of BiNbO4 ceramics. In the present study BiNbO4 ceramics was fabricated by solid state reaction from the mixture of simple oxides viz. Bi2O3, and Nb2O5. Stoichiometric mixture of the powders was thermally analyzed so parameters of the thermal treatment were determined. The EDS measurements proved conservation of the chemical...
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Influence of pore formers on electrical properties of CaTi0.9Fe0.1O3-δ perovskite-type ceramics
PublicationPorous CaTi0.9Fe0.1O3-δ (CTF) perovskites were synthesized by the standard solid state method at different sintering temperatures with carbon black (CB), corn starch (CS) and potato starch (PS) as pore-forming agents. The ceramic samples of porosity between 9% and 42% with 5 - 40 μm pore sizes, were obtained by a 6 h sintering at either 1130º C or 1200º C of precursor powder prepared at 1470º C. X-ray diffraction analysis proved...
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Intramolecular interactions in crystals of tris(2,6-diisopropylphenoxy)silanethiol and its sodium salts
PublicationHydrolytically stable tris(2,6-diisopropylphenoxy)silanethiol has been obtained and reacted with sodium. Solid state interactions within and between the molecules of tris(2,6-diisopropylphenoxy)silanethiol including S-H---π-interactions between the S-H unit and the π-system of the arene have been analyzed. The interactions are documented by X-ray diffraction and FT-IR spectroscopy.
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Halogen bonded polypseudorotaxanes based on a pillar[5]arene host
PublicationTwo crystalline supramolecular polypseudorotaxanes were obtained by combining permethylated pillar[5]arene as a macrocyclic wheel with 1,4-bis(1-imidazolyl)butane and 1,4-bis(iodoethynyl)benzene or 1,4-diiodo-1,3-butadiyne linked by C–I⋯N halogen bonds and creating a polyrotaxane axis. The resulting highly ordered supramolecular arrays were characterized by X-ray crystallography.
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Isostructural zinc and cadmium silanethiolates with bridging biimidazole co-ligands – Enhanced luminescence of zinc complex
PublicationTwo dinuclear complexes of zinc and cadmium with silanethiolate and bridging biimidazole ligands are characterized by X-ray diffraction, FT-IR, UV–Vis and emission spectroscopies. The complexes 1 (Zn) and 2 (Cd) are isostructural but exhibit different electronic structures and different character of frontier HOMO orbitals as indicated by DFT calculations. Lluminescence studies prove strong emission properties of zinc complex.
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Evaluation of cathode materials for electrochemical photocatalyst deposition
PublicationElectrochemical deposition of photocatalyst, especially TiO2, onto several cathode materials was investigated and evaluated. The deposited films were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDX) and electrochemical measurements. Photocatalytic activity was determined by the decomposition of cyclohexane in air by irradiation with ultraviolet light emitting diodes. It was found that...
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Diaminophosphinoboranes: effective reagents for phosphinoboration of CO2
PublicationThe monomeric diaminophosphinoboranes readily react with CO2 under mild conditions to cleanly form products of the general formula R2P-C(=O)-O-B(NR2)2 in the absence of a catalyst. The isolated products from the CO2-phosphinoboration were fully characterized by NMR spectroscopy, IR spectroscopy, and X-ray diffraction. The mechanism of CO2 phosphinoboration with diaminophosphinoboranes was elucidated by DFT calculations.
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SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF NIOBIUM-DOPED HYDROXYAPATITE CERAMICS
PublicationHydroxyapatite (HAp) ceramic materials are considered as one of the most promising implant materials in bone surgery and in dentistry. They exhibit unique biocompatibility, bioactivity, and osteoconductivity, which are the most desirable biomaterial features. However, HAp itself is brittle, has low strength, high degree of crystallinity and low solubility at physiological pH. Doping synthetic HAp with metal ions plays an important...
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THERMION-C2S_10 Ionic thermoelectri effect in the phase transition in Cu2Se
Open Research DataThe dataset contains results of measurements of the ionic thermoelectric effect in copper selenide with Cu1.99Se and Cu1.8Se compositions. X-Ray diffraction data, SEM images and EDX spectra of the samples are also in the dataset.
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Local Structure and Stability of SEI in Graphite and ZFO Electrodes Probed by As K-edge Absorption Spectroscopy
PublicationThe evolution of the solid electrolyte interphase (SEI) during the first Li uptake in advanced Li-ion electrodes is studied by X-ray absorption spectroscopy (XAS). The As atoms present in the electrolyte solution were used as a local probe for monitoring the SEI growth on different electrodes. High-quality As K-edge spectra were collected in fluorescence mode for a set of graphite and carbon-coated ZnFe2O4 electrodes. XAS measurements...
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Enhanced visible light photocatalytic activity of Pt/I-TiO2 in a slurry system and supported on glass packing
PublicationHighly photoactive I/TiO2, Pt/I-TiO2 nanocomposites were obtained using a hydrothermal and wet impregnation method. The incorporation of iodine and modification with 0.05 mol% of platinum leads to enhanced photocatalytic activity as compared to singly doped TiO2 due to the presence of impurity energy level in the structure of TiO2. X-ray diffraction, TEM microscopy, UV–Vis spectroscopy, X-ray photoelectron spectroscopy and BET...
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Measurements of ultrasonic bulk and guided wave propagation in additively manufactured cubes and plates obtained by ultrasonic pulse velocity analyzer and scanning laser vibrometry
Open Research DataThe DataSet contains the results of measurements of ultrasonic wave propagation in additively manufactured samples made of polylactic acid (PLA). Three types of raster angles in two consecutive layers were assumed: 0°/90° (#1), 45°/-45° (#2) and 90°/90° (#3) with respect to the x-axis. For each printing variants a cubic sample (#C1-3) with dimensions...
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Ce site dilution effects in the antiferromagnetic heavy fermion CeIn3
PublicationLa-doped intermetallic single crystals of Ce1−xLaxIn3 were synthesized via an In self-flux method throughout the entire range (x = 0–1). The prototypical heavy-fermion compound CeIn3 shows an antiferromagnetic phase transition at 10.1 K and becomes superconducting near a critical pressure where TN is completely suppressed. As the La concentration increases, Ce moments are diluted, and the lattice constant increases linearly, satisfying Vegard’s...
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Effect of plasma sprayed and laser re-melted Al2O3 coatings on hardness and wear properties of stainless steel
PublicationCommercially available austenic stainless steel substrate was coated with commercially available, raw Al2O3 powder applied by means of plasma spraying method and then re-melted with CO2 laser beam of various parameters. Tribological and mechanical properties of the 120 J/mm and 160 J/mm laser re-melted coatings were compared with the tribological and mechanical properties of the “as-sprayed” coating. The influence of the laser...
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Thickness and structure change of titanium (IV) oxide thin films synthesized by the sol–gel spin coating method
PublicationTitanium dioxide is a well-known material in nanotechnology, while it provides new opportunities due to its interesting properties, for example, as a semiconductor with a quite significant forbidden band gap energy of 3.2 eV. In this study, thin films of titanium dioxide (TiO2) were synthesized in amorphous and crystallographic systems using the sol–gel process. Atomic Force Microscopy (AFM), Raman spectroscopy and X-ray diffraction...
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Reduced Graphene Oxide Joins Graphene Oxide To Teach Undergraduate Students Core Chemistry and Nanotechnology Concepts
PublicationNovel carbon nanomaterials such as reduced graphene oxide (rGO) and graphene oxide (GO) can be easily incorporated into the undergraduate curriculum to discuss basic chemistry and nanotechnology concepts. This paper describes a laboratory experiment designed to study the differences between GO and rGO regarding their physico-chemical properties (e.g. color, hydrophobicity, type of functional groups, electrical conductivity etc.)....
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Silicon Oxycarbide-Graphite Electrodes for High-Power Energy Storage Devices
PublicationHerein we present a study on polymer-derived silicon oxycarbide (SiOC)/graphite composites for a potential application as an electrode in high power energy storage devices, such as Lithium-Ion Capacitor (LIC). The composites were processed using high power ultrasound-assisted sol-gel synthesis followed by pyrolysis. The intensive sonication enhances gelation and drying process, improving the homogenous distribution of the graphitic...
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Terbium Substituted Lanthanum Orthoniobate: Electrical and Structural Properties
PublicationThe results of electrical conductivity studies, structural measurements and thermogravimetric analysis of La1−xTbxNbO4+δ (x = 0.00, 0.05, 0.1, 0.15, 0.2, 0.3) are presented and discussed. The phase transition temperatures, measured by high-temperature x-ray diffraction, were 480 °C, 500 °C, and 530 °C for La0.9Tb0.1NbO4+δ, La0.8Tb0.2NbO4+δ, and La0.7Tb0.3NbO4+δ, respectively. The impedance spectroscopy results suggest mixed conductivity...
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Thermal Instability of Gold Thin Films
PublicationThe disintegration of a continuous metallic thin film leads to the formation of isolated islands, which can be used for the preparation of plasmonic structures. The transformation mechanism is driven by a thermally accelerated diffusion that leads to the minimalization of surface free energy in the system. In this paper, we report the results of our study on the disintegration of gold thin film and the formation of nanoislands...
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Symmetrical and unsymmetrical diphosphanes with diversified alkyl, aryl and amino substituents
PublicationWe present the comprehensive study of diphosphanes with diversified substituents regarding their syntheses, structures, and properties. To this end, we have synthesized a series of novel unsymmetrical alkyl, aryl and amino-substituted diphosphanes of the general formula R1R2P-PR3R4 (where R1, R2, R3, R4 = tBu, Ph, Et2N or iPr2N) via salt metathesis reactionof halophosphanes with metal phosphides in high yield. We vastly expanded...
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Depth chemical profile in a CeIr3 sample
Open Research DataThe polycrystalline sample of CeIr3 used in the present studies was synthesized by arc-melting cerium (4N) and iridium (3N5) in an arc furnace on a water-cooled copper hearth using a tungsten electrode under a high purity argon atmosphere. A piece of zirconium was used as an oxygen getter. First, a button of Ir was prepared by arc-melting the iridium...
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Ambiphilic phosphorous compounds
Open Research DataResults of theoretical and experimental studies on ambiphilic phosphorous compounds:
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Determination of the chemical structure of potential organic impurities occurring in drug substance opipramol
PublicationThe tricyclic antipsychotic and antidepressant drug opipramol (opipramole) was examined with regard to the chemical structure of its organic impurities. Impurities were isolated from the technical product by chromatographic methods and their chemical structures were established by 1H NMR, MS and FTIR and further confirmed by comparison with commercially available products or with products obtained by independent synthesis, and...
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Analysis of Interspike-Intervals for the General Class of Integrate-and-Fire Models with Periodic Drive
PublicationWe study one-dimensional integrate-and-fire models of the general type x˙=F (t, x) and analyze properties of the firing map which iterations recover consecutive spike timings. We impose very week constraints for the regularity of the function F (t, x), e.g. often it suffices to assume that F is continuous. If additionally F is periodic in t, using mathematical study of the displacement sequence of an orientation preserving circle...
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Assessment of FSW Welds Made of Aluminum Alloy AW7075-T651.
PublicationThis paper summarizes the results of experimental studies in which the aluminum alloy AW7075-T651 was friction stir welded (FSW) using various combinations of process parameters (rotational - R and travel speed - T). Mechanical properties of the test welds were assessed by using static tensile test and Vickers hardness measurement. The temperature of the welded plates was monitored during welding by means of thermocouples placed...
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The Characteristic of Surface Layers on Austenitic Stainless SteelAfter Glow-discharge Nitriding Process.
PublicationThis paper presents investigation of surface layers. The diffusion layers were produced by using different parameters of reactive atmosphere (N2:H2). The research of the surface layers was performed using scanning electron microscope (SEM). The results of energy dispersive X-ray (EDX) analysis and X-ray diffraction (XRD) analysis are presented. Research reveals the influence of chemical constitution of reactive atmosphere on the...
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Enhanced photocatalytic properties of lanthanide-TiO2 nanotubes: An experimental and theoretical study
PublicationA series of Er-, Yb-, Ho-, Tb-, Gd-, Pr-TiO2 nanotubes (RE-NTs) was prepared via an electrochemical method. The as-prepared photocatalysts were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–vis absorption, scanning electron microscopy (SEM) and luminescent spectroscopy. The experiments demonstrated that toluene in the gas phase was successfully degraded under visible light (LEDs λmax = 465...
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Preparation and characterization of Pt–N/TiO2 photocatalysts and their efficiency in degradation of recalcitrant chemicals
PublicationSeries of Pt–N/TiO2 photocatalysts were synthesized using the sol–gel method. The photocatalysts’ characteristics by X-ray diffractometry (XRD), scanning transmission electron microscopy (STEM), diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS) showed that sample with the molar ratio Ti:N equal 1:4 and platinum nanoparticles size of about 3 nm had anatase structure, about 94 m2/g specific surface area...
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Highly Active TiO2 Microspheres Formation in the Presence of Ethylammonium Nitrate Ionic Liquid
PublicationSpherical microparticles of TiO2 were synthesized by the ionic liquid-assisted solvothermal method at different reaction times (3, 6, 12, and 24 h). The properties of the prepared photocatalysts were investigated by means of UV-VIS diffuse-reflectance spectroscopy (DRS), Brunauer–Emmett–Teller (BET) surface area measurements, scanning electron microscopy (SEM), X-ray diffraction analysis (XRD), and X-ray photoelectron spectroscopy...
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Shales Leaching Modelling for Prediction of Flowback Fluid Composition
PublicationThe object of the paper is the prediction of flowback fluid composition at a laboratory scale, for which a new approach is described. The authors define leaching as a flowback fluid generation related to the shale processing. In the first step shale rock was characterized using X-ray fluorescence spectroscopy, X-ray diractometry and laboratory analysis. It was proven that shale rock samples taken from the selected sections of horizontal...
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Chemical composition of La-Sr-Ce-Ni-Ti ceramics material measured by XPS method
Open Research DataLa-Sr-Ce-Ni-Ti (LSCNT) based ceramics sample was manufactured by standard solid state reaction.Prepared powder was pressed into pilled and sintered in a furnace in air atmosphere for 10h. Annealing temperature was 1200 Celsius degree. To calculate chemical composition and determine valence states of the elements, X-Ray photoemission spectroscopy (XPS)...
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Nanokrystaliczne warstwy ceramiczne otrzymywane metodą pirolizy aerozolowej w tlenkowych ogniwach paliwowych
PublicationNiniejsza rozprawa doktorska dotyczy badań materiałów wytwarzanych w postaci cienkich, nanokrystalicznych warstw ceramicznych metodą pirolizy aerozolowej dla zastosowań w tlenkowych ogniwach paliwowych (SOFC). Badane są trzy możliwe obszary zastosowań wytwarzanych warstw tj. osadzanie powłok ochronnych na stalowych interkonektorach dostarczających gazy do elektrody tlenowej, wytwarzanie bariery ochronnej zapobiegającej dyfuzji...
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Mild X-linked Alport syndrome due to the COL4A5 G624D variant originating in the Middle Ages is predominant in Central/East Europe and causes kidney failure in midlife
PublicationA study of 269 children enrolled into a National Registry for children with persistent glomerular hematuria identified 131 individuals with genetically confirmed X-linked Alport Syndrome. A single variant c.1871G>A p.Gly624Asp (G624D) in COL4A5 was predominant and accounted for 39% of Xlinked Alport Syndrome in unrelated Polish families (44 of 113). To evaluate its origins, the genetic variation in a 2.79 Mb segment encompassing...
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Lower rim substituted p-tert-butylcalix[4]arene; Part 14. Synthesis, structures and binding studies of calix[4]arene thioamides
PublicationA number of p-tert-butylcalix[4]arene thioamides were synthesized and characterized by 1H-NMR and elemental analysis. Compounds 1-5 are O-substituted derivatives with -CH2-C(=S)-N-X groups, where NX = morpholidyl, NEt2, NHC2H4Ph, NHCH2Ph and NHEt,respectively. The X-ray structures of the ligands 1, 3, 5 and of the complex 3Pb(ClO4)2, (compound 6), are presented and their slightly distorted cone conformation is established. The...
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Możliwości wykorzystania spektroskopii fotoelektronów w analizie jakości środowiska wodnego
PublicationSpektroskopia fotoelektronów w zakresie promieniowania X, (XPS, z ang. X-ray photoelectron spectroscopy) jest nowoczesną metodą analityczną wykorzystywaną w wielu wiodących ośrodkach naukowych na świecie. Jest ona stale ulepszana, jak też poznawane są nowe obszary jej zastosowania. W niniejszym artykule przedstawione zostały możliwości wykorzystania metody XPS w ramach obszarów badawczych powiązanych z gospodarką wodną, takich...
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Characterization of Small Azocrown Ether Stereoisomers.
PublicationWyizolowano i zbadano metodą X-ray, 1H NMR i UV-Vis trwałe izomery E i Z 10-członowej azokorony. Ich struktura w stanie stałym świadczy o naprężonej konformacji w przypadku izomeru trans i nie naprężonej dla izomeru cis. Jest to efektem sprzężenia p grupy azowej z benzenem i naprężenia sterycznego konformacji cząsteczki.
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Photoactivity of decahedral TiO2 loaded with bimetallic nanoparticles: Degradation pathway of phenol-1- 13 C and hydroxyl radical formation
PublicationDecahedral TiO2decorated with bimetallic nanoparticles were synthesized via radiolysis and photode-position method. The effect of bimetallic surface composition (Ag Pt, Ag Au, Au Pd, Au Pt) as well asdeposition technique (simultaneous or sequential) on the photocatalytic activity in phenol degradationand efficiency of hydroxyl radicals generation under UV–vis light irradiation were investigated. Modifiedand pristine decahedral...
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Mn-Co nanofilms on nickel foam measured by XPS mehod
Open Research DataManganium-Cobaltium based thin films were electrochemically deposited on a Ni based subsrates in a one-step process at −1.1 V vs. Ag/AgCl in an aqueous solution of differently concentrated Mn(NO3)2·4H2O and Co(NO3)2·6H2O with the deposition time limited by charges of 60, 120, and 200 mC at 25 °C. The concentration ratios of Mn(NO3)2·4H2O to Co(NO3)2·6H2O...
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Structure and magnetic properties of BeO-Fe2O3-Al2O3-TeO2 glass-ceramic composites
PublicationIn this work, glass-ceramics in the xBeO–20Fe2O3–(80-x)TeO2 system with x = 0–25 mol% were synthesized by the traditional melt quenching route and studied by inductively coupled plasma optical emission spectroscopy, X-ray diffraction, confocal microscopy, infrared and Raman spectroscopy. BeO addition was found to support the crystallization process of Fe2O3 during melting, and an increased BeO content was associated with an increased...