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Wyniki wyszukiwania dla: X-RAY COMPUTED MICROTOMOGRAPHY
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Effect of Laser Treatment on Intrinsic Mechanical Stresses in Titanium and Some of Its Alloys
PublikacjaLaser surface treatment conducted at different power levels is an option to modify titanium bone implants to produce nano- and microtopography. However, such processing can lead to excess mechanical stress within the surface layer. This research aims to calculate the level of such residual stresses after the surface processing of Ti grade IV, Ti15Mo, and Ti6Al7Nb alloys with an Nd:YAG laser. Light and scanning electron microscopies...
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High Temperature Corrosion Evaluation of Porous Hastelloy X Alloy in Air and Humidified Hydrogen Atmospheres
PublikacjaIn this work a commercially available porous Hastelloy X alloy is characterized in terms of high temperature corrosion resistance. The alloy was oxidized in the temperature range from 500C to 900C in air and humidified hydrogen for 100 hours. Corrosion rates and porosity changes were measured. Microstructural characterization was performed using X-ray diffractometry and scanning electron microscopy. Results show that porous alloys...
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Optical rotation in the lithium triborate nonlinear crystal
PublikacjaA dual-wavelength polarimetric technique at 633 and 661 nm has been used for the characterization of a nonlinear lithium triborate (LiB3O5) nonenantiomorphous biaxial crystal. The mismatch of the crystallographic and optical coordinate systems was taken into account. The optical rotatory power for light propagation along one of the optical axes is ρ = 7.06° mm−1. The gyration tensor component along the bisector between the x and...
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Concentration‐Induced Hetero‐Valent Partial‐Inverse Occupation of Infrared Phosphor
PublikacjaInfrared luminescent materials have evoked much attention from chemists and material scientists. Although substantial progress is made in materials design, the luminescent mechanism remains ambiguous in the complex structures, presenting major barriers to developing novel infrared luminescent materials. Herein, this study aims to deliberate a complete discussion on infrared phosphors with concentration-induced hetero-valent partial-inverse...
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Mechanical Properties of Additively Manufactured Polymeric Materials—PLA and PETG—For Biomechanical Applications
PublikacjaThe study presented herein concerns the mechanical properties of two common polymers for potential biomedical applications, PLA and PETG, processed through fused filament fabrication (FFF)—Material Extrusion (ME). For the uniaxial tension tests carried out, two printing orientations—XY (Horizontal, H) and YZ (Vertical, V)—were considered according to the general principles for part positioning, coordinates, and orientation typically...
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Insight into the microstructural and durability characteristics of 3D printed concrete: Cast versus printed specimens
PublikacjaThis study presents the comparison of microstructural and durability characteristics of 3D printed concrete (3DPC) depending on its production method (printing or casting). Printed samples with different numbers of layers, as well as a cast specimen with an identical mix composition, were produced and compared, with their microstructural pore and solid characteristics quantitatively and qualitatively investigated. For this purpose,...
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Crystal structure and physical properties of AePd1-xP1+x (Ae = Ca, Sr)
PublikacjaWe report the discovery of two new compounds AePd1-xP1+x (Ae = Ca, Sr) crystallized in different hexagonal structures. Single crystals of AePd1-xP1+x (Ae = Ca, Sr) are obtained using the Bi-flux method. Crystallographic analysis by both powder and single crystal X-ray diffraction shows that CaPd1-xP1+x crystallizes in a non-centrosymmetric hexagonal structure with the space group P-6m2 (No.187) and lattice parameters a = b = 4.0391(9)...
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Nickel(II) tri-tert-butoxysilanethiolates with N-heterocyclic bases as additional ligands: Synthesis, molecular structure and spectral studies
PublikacjaW publikacji przedstawiono metodę syntezy trzech kompleksów silanotiolanowych z takimi N-heterocyklicznymi zasadami jak: pirydyna, 2-metylopirydyna i 3,5-dimetylopirydyna. Dla tych kompleksów przeprowadzono badania X-Ray, analizy elementarnej. Przy pomocy rentgenowskiej analizy strukturalnej wykazano różną koordynację atomu centralnego - niklu.
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Backscattering properties of southern Baltic herring
PublikacjaReliable TS(L) relationship is required to improve acoustic algorithms of abundanceestimation of Baltic herring. The relationships, empirically obtained in different parts of theBaltic Sea, produce up to 8 dB – difference in the herring TS. In order to develop an accurateTS(L) relationship, it is important to analyze factors controlling the TS variability. Thepossible impact of the regional difference...
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Modification of TiO2 nanotubes by graphene–strontium and cobalt molybdate perovskite for efficient hydrogen evolution reaction in acidic medium
PublikacjaHerein, 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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Novel Class of Proton Conducting Materials—High Entropy Oxides
PublikacjaHere, for the first time, we present data on proton conductivity of high-entropy, single-phase perovskites. The BaZr0.2Sn0.2Ti0.2Hf0.2Ce0.2O3−δ, BaZr0.2Sn0.2Ti0.2Hf0.2Y0.2O3−δ, BaZr1/7Sn1/7Ti1/7Hf1/7Ce1/7Nb1/7Y1/7O3−δ, and BaZr0.15Sn0.15Ti0.15Hf0.15Ce0.15Nb0.15Y0.10O3−δ single-phase perovskites were synthesized. Before electrical measurements, materials were characterized using X-ray diffraction (XRD), scanning electron microscopy...
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Reactive deposition of TiNx layers in a DC-magnetron discharge
PublikacjaTiNx layers have been deposited in 'balanced mode' and 'unbalanced mode' of a reactive DC-magnetron plasma (carrier gas argon, reactive gas nitrogen) under different conditions. Discharge power and reactive gas flow have been varied. The layers have been examined by X-ray photoelectron spectroscopy (XPS), X-ray reflectometry (XR), and spectroscopic ellipsometry (SE). The results of the layer analyses were combined with plasma investigations...
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3D Hierarchical Boron-Doped Diamond-Multilayered Graphene Nanowalls as an Efficient Supercapacitor Electrode
PublikacjaSynthesis 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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Investigation of the structural and thermal properties of aluminum-rich Ca–Al–Si–O–N glasses
PublikacjaIn 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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Fatigue Bending of V-Notched Cold-Sprayed FeCoCrNiMn Coatings
PublikacjaCold-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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OPTIMIZATION OF NASICON PREPARATION METHOD
PublikacjaNasicon 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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Boron Difluoride Complexes of Carbamoyl Meldrum's Acids
Publikacja5-[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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Evolution of charge density wave order in continuous solid solutions Lu(Ni1-xCox)C2
PublikacjaPseudo-ternary solid solutions, Lu(Ni1-xCox)C2 (0 ≤ x ≤ 1), were studied by means of powder X-ray diffraction, differential thermal analysis as well as electrical resistivity and heat capacity measurements. The crystal structure of the Lu(Ni1-xCox)C2 series, as investigated by means of X-ray powder diffraction, is of structure type CeNiC2, space group Amm2, Pearson symbol oS8. The structural analysis reveals a non-monotonous evolution,...
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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
PublikacjaNovel 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
PublikacjaCathodic 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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High-conducting Bi4V2-xFexO11-δ ceramics containing Fe2O3 nanocrystals: Structure and properties
PublikacjaThe 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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Evaluation of cathode materials for electrochemical photocatalyst deposition
PublikacjaElectrochemical 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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Intramolecular interactions in crystals of tris(2,6-diisopropylphenoxy)silanethiol and its sodium salts
PublikacjaHydrolytically 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
PublikacjaTwo 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
PublikacjaTwo 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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Diaminophosphinoboranes: effective reagents for phosphinoboration of CO2
PublikacjaThe 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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Structure and hyperfine interactions in Bi1−xNdxFeO3 solid solutions prepared by solid-state sintering
PublikacjaThe series of polycrystalline ceramic powders, Bi1xNdxFeO3 (x = 0.11) was successfully synthesized by mixed oxide method followed by pressureless sintering. X-ray diffraction and Mössbauer spectroscopy were used as complementary methods to study structure and hyperfine interactions of the samples. It was found that with an increase of Nd content, within the range of x = 0.20.3 a structural phase transition from rhombohedral to...
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Effects of La Content on the Densification, Microstructure, and Conductivity of Doped La10−x Ge6 O26±δ Electrolytes
PublikacjaIn this study, the influence of La content on the characteristics of Nb-, Mo-, and W-doped LaxGe6O26±δ electrolytes was investigated through sintering study, X-ray diffraction, scanning electron microscopy, and conductivity measurement. The densification of LaxGe5.5Nb0.5O26±δ and LaxGe5.5W0.5O26±δ was retarded as the x reached 9.75, while that of LaxGe5.5Mo0.5O26±δ improved with increasing La content. The average grain size slightly...
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The influence of nanostructures size on V2O5 electrochemical properties as cathode materials for lithium ion battery
PublikacjaIn this paper, V2O5 nanostructures with a size depending on the annealing temperature are successfully synthesized by a sol-gel method. The crystal structure and morphology of samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), selected area electron diffraction (SEAD) and scanning electron microscopy (SEM), respectively. Electrochemical testing such...
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Local Structure and Stability of SEI in Graphite and ZFO Electrodes Probed by As K-edge Absorption Spectroscopy
PublikacjaThe 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
PublikacjaHighly 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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The Effect of Titanium Oxyfluoride Morphology on Photocatalytic Activity of Fluorine-Doped Titanium(IV) Oxide
PublikacjaTitanium oxyfluoride (TiOF2) is a metastable product that can be obtained in a fluorine-rich environment. This material can also be a valuable precursor in the synthesis of titanium(IV) oxide (TiO2). However, the effect of TiOF2 morphology on the physicochemical properties of TiO2 has not been studied so far. In this work, single-phase TiOF2 was prepared by a solvothermal method. The as-synthesized samples exhibited a variety of...
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Oxidation step in the preparation of benzocamalexin: The crystallographic evidence
PublikacjaThe study of oxidation step in the preparation of benzocamalexin by the α-amidoalkylation–oxidation sequence revealed the formation of perchloro-1,2-phenylene dibenzoate as the product of transformation of tetrachloro- 1,2-benzoquinone applied as the oxidant. The structures of benzocamalexin and perchloro-1,2-phenylene dibenzoate were confirmed by X-ray diffraction analysis. The extraction step in the final isolation of benzocamalexin...
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Role of MnO in manganese–borate binary glass systems: a study on structure and thermal properties
PublikacjaStructural and thermal properties of x MnO−(100−x)B2O3 (where x=40, 50 and 60 mol%) glass samples have been investigated with the employment of various techniques. Fourier transform infrared spectroscopy results revealed the influence of MnO on glass matrix. Decrease of B–O bond-related band intensities has been observed. MnO addition was found to introduce broken [BO2O−]n chains. Differential scanning calorimetry (DSC) measurements...
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Terbium Substituted Lanthanum Orthoniobate: Electrical and Structural Properties
PublikacjaThe 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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Determination of the chemical structure of potential organic impurities occurring in drug substance opipramol
PublikacjaThe 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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The synthesis and structure of a potential immunosuppressant: N-mycophenoyl malonic acid dimethyl ester
PublikacjaThe synthesis of a potential immunosuppressant, i.e. dimethyl ester of N-mycophenoyl malonic acid was optimized in the reaction of mycophenolic acid (MPA) with amino malonic dimethyl ester in the presence of propanephosphonic anhydride (T3P) as a coupling reagent. The structural properties of the obtained MPA derivative were investigated by NMR, MS and single crystal X-ray diffraction methods. Theoretical considerations of conformational...
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Fermi-liquid behavior of binary intermetallic compounds Y3 M (M = Co, Ni, Rh, Pd, Ir, Pt)
PublikacjaA series of polycrystalline samples of Y3 M (M = Co, Ni, Rh, Pd, Ir, Pt), intermetallic binary compounds were synthesized by the arc-melting method. Powder x-ray diffraction (pXRD) confirmed the orthorhombic cementite-type crystal structure and allowed for the estimation of the lattice parameters. Physical properties were investigated by means of electrical resistivity and heat capacity measurements between 1.9 K and 300 K. All...
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Highly Active TiO2 Microspheres Formation in the Presence of Ethylammonium Nitrate Ionic Liquid
PublikacjaSpherical 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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Experimental tuning of AuAg nanoalloy plasmon resonances assisted by machine learning method
PublikacjaPlasmonic nanostructures based on AuAg nanoalloys were fabricated by thermal annealing of metallic films in an argon atmosphere. The nanoalloys were chosen because they can extend the wavelength range in which plasmon resonance occurs and thus allow the design of plasmonic platforms with the desired parameters. The influence of initial fabrication parameters and experimental conditions on the formation of nanostructures was investigated....
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Preparation and characterization of Pt–N/TiO2 photocatalysts and their efficiency in degradation of recalcitrant chemicals
PublikacjaSeries 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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Assessment of FSW Welds Made of Aluminum Alloy AW7075-T651.
PublikacjaThis 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.
PublikacjaThis 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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Novel complexes possessing Hg–(Cl, Br, I)⋯O=C halogen bonding and unusual Hg₂S₂(Br/I)₄ kernel. The usefulness of τ₄′ structural parameter
PublikacjaOne mononuclear and two binuclear Hg(II) complexes have been synthesized and characterized by X-ray diffraction, ATR IR and Hirshfeld surface analysis. Single-crystal X-ray diffraction showed that binuclear compounds are centrosymmetric and isostructural. All complexes form bifurcated intermolecular N–H···O hydrogen bonds that contribute to a formation of the centrosymmetric dimers. In binuclear complexes, sulfur atoms of thiourea...
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Enhanced photocatalytic properties of lanthanide-TiO2 nanotubes: An experimental and theoretical study
PublikacjaA 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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Ferromagnetic nanocrystallites in the SiO2 - PbO - Fe2O3 glass system
PublikacjaThe structure of 50% SiO2 - 35% PbO - 15% Fe2O3, 50% SiO2 - 30% PbO - 20% Fe2O3 and 50% SiO2 - 25% PbO - 25% Fe2O3 (in mol%) glass was investigated by the means of AFM microscopy and X-ray diffraction. Observation by the atomic force microscopy shows that each of prepared iron oxide glass doesn't have homogeneous structure and some nanocrystallites were detected. Next, test with neodymium magnet found out strong magnetic properties...
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Shales Leaching Modelling for Prediction of Flowback Fluid Composition
PublikacjaThe 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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Możliwości wykorzystania spektroskopii fotoelektronów w analizie jakości środowiska wodnego
PublikacjaSpektroskopia 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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Lower rim substituted p-tert-butylcalix[4]arene; Part 14. Synthesis, structures and binding studies of calix[4]arene thioamides
PublikacjaA 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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Characterization of Small Azocrown Ether Stereoisomers.
PublikacjaWyizolowano 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.