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Search results for: X-RAY DIFFRACTION
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Fe3–xInSnxO6 (x = 0, 0.25, or 0.5): A Family of Corundum Derivatives with Sn-Induced Polarization and Above Room Temperature Antiferromagnetic Ordering
PublicationThree new double corundum derivative compounds, Fe3−xInSnxO6 (x = 0. 0.25, or 0.5), were synthesized at high pressure and temperature (6 GPa and 1400− 1450 °C). All of the compounds order antiferromagnetically well above room temperature (TN = 608, 532, and 432 K for x = 0, 0.25, and 0.5, respectively). The x = 0 phase crystallizes as centrosymmetric R3̅c, but the inclusion of closed-shell d10 Sn4+ induces x = 0.25 and 0.5 to crystallize...
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Tin oxide nanoparticles from laser ablation encapsulated in a carbonaceous matrix – a negative electrode in lithium-ion battery applications
PublicationThis report concerns carbonaceous electrodes doped with tin(II) oxide nanoparticles. Tin nanoparticles are obtained by pulsed laser ablation in water. Crystalline nanoparticles have been encapsulated in a carbonaceous matrix formed after pyrolysis of a mixture consisting of tin/tin(IV) oxide nanoparticles and gelatine. The obtained material is characterized by means of X-ray diffraction, selected area diffraction, scanning electron...
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Synthesis and structure of Bi 5 FeTi 3 O 15 ceramics
PublicationAim of the present research was to fabricate and study crystal structure and phase composition of Bi5FeTi3O15 (BTFO) ceramics exhibiting Aurivillius - type structure. By means of simultaneous thermal analysis and X-ray diffraction analysis the process of synthesis of BTFO ceramics has been studied. Mixed oxide method followed by pressureless sintering was used for ceramics preparation. Three endothermic thermal effects have been...
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Niobiany ziem rzadkich - właściwości i zastosowania
PublicationRare earth niobates are a very interesting group of materials. These compound have different properties which could be changes in a wide range by appropriate doping. X-Ray diffraction examinations for some compounds of RE3NbO7 group were shown
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Structural and mechanical properties of hydroxyapatite coatings formed by ion-beam assisted deposition
PublicationThe ion-beam assisted deposition (IBAD) is an advanced method capable of producing crystalline coatings at low temperatures. We determined the characteristics of hydroxyapatite Ca10(PO4)6(OH)2 target and coatings formed by IBAD using X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX). The composition of the coatings'...
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Electronic and ionic relaxations in strontium-borate glass and glass-ceramics containing bismuth and vanadium oxides
PublicationThe topography, microstructure and electrical properties of strontium-borate glass and SBO glass containing bismuth and vanadium oxides, were studied. The structure was measured using X-ray diffraction (XRD), Energy Dispersive X-ray Spectrometer (EDS) and Scanning electron microscope (SEM) methods. The A.C. complex conductivity was investigated as a function of temperature and frequency. The influence of the quantity of bismuth...
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Interactions between components of SrTi0.98 Nb0.02O3-δ-YSZ and SrTi0.98 Nb0.02O3-δ -CeO2 composites
PublicationComposites consisting of SrTiO3-based perovskite and either yttria-stabilized zirconia or ceria were investigated. The mechanical compatibility and possible inter-diffusion between phases were characterized by scanning electron microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy. A gradual disappearance of Ce-containing phases with an increase in the temperature of reduction in hydrogen was noticed. Moreover,...
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Luminescence of TeO2:Eu thin films
Open Research DataTellurium dioxide doped by europium thin films were deposited by magnetron sputtering method and simultaneously heated at 200 oC. Presence of Eu ions and their valence states was confirmed by X-ray photoemission spectroscopy measurements. The structure of the films as well as the influence of europium dopant on crystalline structure of the films was...
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Fabrication, structural and electrical properties of Sr(V,Nb)O 3-δ perovskite materials
PublicationThe SrV1-xNbxO3-δ materials with different niobium content in perovskite B-sublattice were prepared by a solid-state reaction process. The microstructure and phase compositions of obtained samples were analyzed by the X-ray diffraction technique (XRD) and scanning electron microscopy (SEM). The electrical conductivity of samples was measured by a DC 4-wire method in range of 100–600 °C in different gas conditions. The oxidation...
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Effect of isovalent substitution on microstructure and phase transition of LaNb1−xMxO4 (M=Sb, V or Ta; x=0.05–0.3)
PublicationLaNb1−xMxO4 oxides with pentavalent elements of different ionic sizes (M=Sb, Ta and V, x=0.05–0.3) were synthesized by the solid state reaction method. Special interest was devoted to the antimony substituted lanthanum niobate which is a new material in this group. Rietveld analysis of the X-ray diffraction patterns was used to determine the influence of the material composition on unit cell parameters. On the basis of dilatometric...
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The crystal structure of (1RS,4RS,5RS,6SR)-5-cyano-5-nitro-6-phenyl-bicyclo[2.2.1]hept-2-ene
PublicationStructure of nitronorbornene derivative C14H12N2O2 synthesized in the reaction of cyclopentadiene with E-2-phenyl-1-cyano-1-nitroethene was determined by single crystal X-ray diffraction analysis. It was found that in analyzed molecule the nitro group is in endo-position whereas phenyl group have exo-ori-entation.
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Agnieszka Witkowska dr hab. inż.
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PtCo cathode electrocatalyst behaviour viewed by in-situ XAFS fuel cell measurements
PublicationW pracy zostały przedstawione wstępne wyniki analizy XAS (X-ray absorption spectroscopy), TEM (transmission electron microscopy) i XRD (X-ray diffraction) nanostruktur PtCo 1:1 (20% fazy metalicznej osadzonej na węglu, Vulcan XC-72) używanych jako elektrokatalizatory w polimerowych ogniwach paliwowych (PEM FC). Pomiary realizowane były również w warunkach pracy ogniwa paliwowego za pomocą specjalnie zoptymalizowanej do pomiarów...
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Metal ion directed template synthesis using 2-acetyl-1,3-indandione and ethylenediamine: steric and electronic restrictions
PublicationA template synthesis using 2-acetyl-1,3-indandione and ethylenediamine results in formation of octahedral Ni complex, whose crystal structure has been resolved using single crystal X-ray diffraction. The structure indicates that only exocyclic enolic oxygen atom of the triketone takes part in the condensation with ethylenediamine.
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Copper(II) complexes of 7-amino-2-methylchromone and 7-aminoflavone: Magneto-structural, spectroscopic and DFT characterization
PublicationFour new complexes of copper(II) consisting of two different chromone derivatives with carbonyl and amine donor atoms: 7-aminoflavone (L1) and 7-amino-2-methylchromone (L2), were synthesized and characterized by X-ray diffraction, UV–Vis, FT-IR, EPR spectroscopy, MS and elemental analysis. In all four compounds, the chromone derivatives were found to act as monodentate O- or N-ligands. The structural characteristics of 1a and...
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Structural investigations of the LTO:Cu thin films
Open Research DataLithium titanate (Li1+xTi2-xO4) doped with Cu2+ ions was synthesized by sol-gel processing method. The structure was characterized by X-ray Diffraction (XRD). All samples revealed presence of LTO spinel phase. X-ray pattern of undoped LTO was free of any impurities and other crystal phases. Similarly, samples with low amount of copper dopant (x = 0.05...
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Structure and optical measurements of Eu doped tellurium oxide thin films
Open Research DataThin films were deposited by magnetron sputtering method and simultaneously heated at 200 oC. Presence of Eu ions and their valence states was confirmed by X-ray photoemission spectroscopy measurements. The structure of the films as well as the influence of europium dopant on crystalline structure of the films was examined by X-ray diffraction method. ...
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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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Structure and optical parameters of Eu doped tellurium oxide thin films prepared by reactive magnetron sputtering method
PublicationIn this work the structural properties and photoluminescence of tellurium dioxide thin films doped by europium were described. Thin films were deposited by magnetron sputtering method and simultaneously heated at 200 °C. Presence of Eu ions and their valence states was confirmed by X-ray photoemission spectroscopy measurements. The structure of the films as well as the influence of europium dopant on crystalline structure of the...
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La 15 Nb x Ge 9 : a superstructure of the Mn 5 Si 3 structure type with interstitial Nb atoms
PublicationThe crystal structure and elementary properties of La15NbxGe9 are reported. Single-crystal X-ray diffraction,from a crystallite with only 0.12 Nb/formula unit, reveals that this compound, although transition metal deficient, crystallizes in a hexagonal “15-1-9”-like structure type, space group P63mc (no. 186) with lattice parameters a = b = 15.5017(2) Å, c = 6.9173(2) Å. The physical properties were examined by specific heat and resistivity...
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Results after grinding C45 steel
Open Research DataThe database contains results from nanoindenter, scanning microscope and also X-ray diffractometer. To determine the residual stresses and the size of the crystallites in the ferrite grains in the grinded surface layer, the Williamson Hall analysis of the X-ray diffraction patterns was performed. XRD diffraction patterns were also used to perform a...
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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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(CsX)Cu5O2(PO4)2 (X = Cl, Br, I): A Family of Cu2+ S = 1/2 Compounds with Capped-Kagomé Networks Composed of OCu4 Units
PublicationThree new salt inclusion compounds (CsX)Cu5O2(PO4)2 (X = Cl, Br, I), phosphate analogues of the kagomé mineral averievite, are reported. Their crystal structures are composed of trigonal networks of corner-sharing OCu4 anion-centered tetrahedra, forming capped-kagomé planes, which can also be regarded as two-dimensional slices along the [111] direction of a pyrochlore lattice. Magnetization and heat capacity measurements reveal...
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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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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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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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The influence of nanostructures size on V2O5 electrochemical properties as cathode materials for lithium ion battery
PublicationIn 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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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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Oxidation step in the preparation of benzocamalexin: The crystallographic evidence
PublicationThe 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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Jarosław Chojnacki prof. dr hab. inż.
PeopleBorn in 1961 in Bydgoszcz, professional education started at the Chemical Technical Highschool (I. Łukasiewicz). He graduated from the Faculty of Chemistry at the Gdańsk University of Technology in 1986, defending the work on ion-selective electrodes. Subsequent studies were related to organic and siliconorganic synthesis and, from 2002 year on, to crystallography. The doctoral thesis concerned the Silanotiolanes of coinage metals...
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Antimony substituted lanthanum orthoniobate proton conductor – structure and electronic properties.
PublicationX‐ray and neutron diffraction have been utilized to analyze the crystalline and electronic structure of lanthanum orthoniobate substituted by antimony. Using X‐ray absorption spectroscopy and photoelectron spectroscopy, changes in the electronic structure of the material upon substitution have been analyzed. The structural transition temperature between fergusonite and scheelite phases for 30 mol% antimony substitution was found...
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Novel Class of Proton Conducting Materials—High Entropy Oxides
PublicationHere, 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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The structure of lead-silicate glasses and nanocomposites doped with iron oxide
Open Research DataThe structure of iron-doped glasses and glass-ceramics were studied. Samples has the composition of 50SiO2–(50−x)PbO–xFe2O3, where x=15, 20 and 25 (in mol%). All samples were prepared by the conventional melt quenching technique; the melting was conducted in air at 1623 K in alumina crucibles. The melts were poured on a brass plate preheated to 573...
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The synthesis and structure of a potential immunosuppressant: N-mycophenoyl malonic acid dimethyl ester
PublicationThe 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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NOx Photooxidation over Different Noble Metals Modified TiO2
PublicationWe compared the activity enhancement effect of noble metal deposited on TiO2 in photocatalytic nitrogen oxides oxidation. Titanium dioxide was decorated with Ag, Au, Pt or Pd in the sol-gel process. Synthesized catalysts were characterized by X-ray diffraction (XRD), Brunauer–Emmett–Teller measurement (BET), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and energy dispersive X-ray analysis (EDX)....
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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
PublicationOne 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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Ferromagnetic nanocrystallites in the SiO2 - PbO - Fe2O3 glass system
PublicationThe 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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Spin-glass behavior in a binary Pr 3 Ir intermetallic compound
PublicationPolycrystalline Pr3Ir was synthesized by arc melting. Its cementite-type crystal structure (Pnma) was confirmed by powder X-ray diffraction and estimated lattice parameters are in agreement with literature. Physical properties were measured by means of the ac and dc magnetic susceptibility, electrical resistivity and heat capacity. Our results indicate spin-glass behavior in Pr3Ir with a freezing temperature Tf = 6.58 K and activation...
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Mössbauer Spectroscopy and Magnetoelectric Effect Studies of Multiferroic Ceramics Based on BiFeO<sub>3</sub>
PublicationIn this work the results of investigations for (BiFeO3)x(BaTiO3)1-x and Bi1-xNdxFeO3 solid solutions are described. Samples were prepared by the conventional solid-state sintering method. X-ray diffraction, 57Fe Mössbauer spectroscopy, and magnetoelectric effect measurements were applied as complementary methods to determine the structure and magnetic properties of materials. For (BiFeO3)x(BaTiO3)1-x solid solutions Mössbauer...
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Evolution of charge density wave order in continuous solid solutions Lu(Ni1-xCox)C2
PublicationPseudo-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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Structural and electrical properties of titanium-doped yttrium niobate
PublicationIn this work, the influence of the substitution of niobium by titanium in Y3Nb1-xTixO7-δ on the structural and electrical properties is reported. Several experimental techniques, i.e. X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), X-Ray Photoelectron Spectroscopy (XPS) and Electrochemical Impedance Spectroscopy (EIS), were applied to investigate the system Y3Nb1-xTixO7-δ. Titanium in Y3Nb1-xTixO7-δ is an acceptor-type...
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High-Temperature Structural and Electrical Properties of BaLnCo2O6 Positrodes
PublicationThe application of double perovskite cobaltites BaLnCo2O6−δ (Ln = lanthanide element) in electrochemical devices for energy conversion requires control of their properties at operating conditions. This work presents a study of a series of BaLnCo2O6−δ (Ln = La, Pr, Nd) with a focus on the evolution of structural and electrical properties with temperature. Symmetry, oxygen non-stoichiometry, and cobalt valence state have been examined...
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Ceramic composites for single-layer fuel cells
PublicationComposite materials consisting of acceptor doped lanthanum orthoniobate electrolyte phase (La0.98Ca0.02NbO4) and Li2O:NiO:ZnO semiconducting phase were synthesized. The precursor powder of La0.98Ca0.02NbO4 was prepared in nanocrystalline (mechanosynthesis) and microcrystalline (solid-state synthesis) form. The composite can be applied in a single-layer fuel cell, because of the presence of two phases acting as an anode and a cathode...
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Enhanced Electrochemical Performance of MnCo1.5Fe0.5O4Spinel for Oxygen Evolution Reaction through Heat Treatment
PublicationMnCo1.5Fe0.5O4 spinel oxide was synthesized using the sol−gel technique, followed by heat treatment at various temperatures (400, 600, 800, and 1000 °C). The prepared materials were examined as anode electrocatalysts for watersplitting systems in alkaline environments. Solid-state characterization methods, such as powder X-ray diffraction and X-ray absorption spectroscopy (XAS), were used to analyze the materials’ crystallographic...
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Nanomateriały o właściwościach magnetycznych, fotokatalitycznych, biobójczych
PublicationTematyka badawcza pracy doktorskiej obejmuje preparatykę i charakterystykę nanomateriałów o właściwościach magnetycznych, fotokatalitycznych, biobójczych. Celem pracy była preparatyka nanomateriałów na bazie TiO2 oraz ZnFe2O4 oraz zastosowanie nanokompozytów w fotokatalizie heterogenicznej do degradacji ksenobiotyków niepodatnych na rozkład biologiczny i otrzymywania funkcjonalnych materiałów budowlanych. Otrzymane nanokompozyty...
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XRD investigations of the lithium titanate thin films
Open Research DataNanocrystalline thin films with 800 nm thickness were prepared by sol–gel method. To examine the influence of the annealing temperature on as-prepared films crystallization, the coatings were heated at temperature from 500 °C up to 600 °C for 20h. Structure of manufactured thin films was investigated using X-ray diffraction (XRD). The most visible...
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The structure of lead-borate glasses containing nanocrystallites of iron oxides
Open Research DataThe structure of iron-doped glasses and glass-ceramics were studied. Glass samples of composition of xFe2O3–(100 − x)(B2O3–2PbO) (2.5 b x b 37, in mol%) were prepared by the conventional melt quenching technique. The melting was conducted in alumina crucibles at the temperature of 1523 K. The melts were poured on a preheated (573 K) brass plate and...
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Influence of dopants on structure of polycrystalline bismuth niobate
PublicationBismuth niobate (BiNbO4) has attracted attention as a low-fired ceramics with promising microwave application potential. BiNbO4 ceramics was fabricated by mixed oxide method and sintered at temperature T<1000˚C. As the sintering aids a small amount of CuO oxide was used. The crystalline structure of the ceramic samples was examined by X-ray diffraction method at room temperature. The Rietveld refinement method was used for analysis...
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Pressure effects on the superconductivity of the HfPd2Al Heusler compound: Experimental and theoretical study
PublicationPolycrystalline HfPd2Al has been synthesized using the arc-melting method and studied under ambient-pressure conditions by x-ray diffraction from room temperature up to 450 °C. High-pressure x-ray diffraction up to 23 GPa was also performed using Diacell-type membrane diamond anvil cells. The estimated linear thermal expansion coefficient was found to be α=1.40(3)×10−5K−1, and the bulk modulus derived from the fit to the third-order...
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Hydrothermal reactions: From the synthesis of ligand to new lanthanide 3D-coordination polymers
PublicationThe organic ligand 2,5-piperazinedione-1,4-diaceticacid (H2PDA) was synthesized under hydrothermal conditions starting from the iminodiacetic acid and catalyzed by oxalic acid. The X-ray powder diffraction data indicates that the compound crystallizes in the P21/c space group as reported in the literature. The ligand was also characterized by elemental analysis, magnetic nuclear resonance, infrared spectroscopy and thermogravimetric...