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At least 1,153 records · Page 64

Local atomic structure of K{sub x}Na{sub (1−x)}NbO{sub 3} by total x-ray diffraction

Local atomic structure of K{sub x}Na{sub (1−x)}NbO{sub 3} with 0.0 ≤ x ≤ 1.0 was studied using atomic Pair Distribution Function analysis based on x-ray diffraction. Powdered crystals were found to exhibit a re-entrant behavior by being orthorhombic (Amm2) for x < 0.42, monoclinic (Pm) for 0.42 ≤ x ≤ 0.63 and again orthorhombic (Amm2) for x > 0.63. Non-centrosymmetric structure of NaNbO{sub 3} (Amm2) was also evident in the piezoresponse force microscopy analysis revealing the presence of the ferroelectric domains and switching behavior. Lowering of the crystallographic symmetry for 0.42 ≤ x ≤ 0.63 is discussed in terms of differences in the sizes of Na{sup +} and K{sup +} ions and Na–O and K–O bond lengths. Besides being a bridging phase, as suggested by the previous studies on lead-based compositions, present study suggests that lower symmetry monoclinic phase of compositionally disordered perovskite solid solutions could also be a manifestation of the difference in the sizes of constituent ions and bond lengths.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Copper-based alloys, crystallographic and crystallochemical parameters of alloys in binary systems Cu-Me (Me=Co, Rh, Ir, Cu, Ag, Au, Ni, Pd, Pt)

The article presents the results of the analysis of phase equilibrium of ordered phases in binary systems based on copper Cu- Me (where Me - Co, Rh, Ir, Ag, Au, Ni, Pd, Pt) to find correlations of crystallochemical and crystallographic factors. It is established that the packing index in disordered solid solutions in binary systems based on copper is close to the value of 0.74 against the background of an insignificant deviation of atomic volumes from the Zen’s law.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Structural and Mössbauer spectroscopic study of Fe-Ni alloy nanoparticles

Nano-crystalline Fe-Ni alloys have been synthesized in ethylene glycol medium. Based on XRD studies it is confirmed that, in these alloys Fe atoms are incorporated at Ni site to form Ni-Fe solid solutions. Mössbauer studies have established that for alloy particles having smaller size there is significant concentration of two different types of paramagnetic Fe species and their relative concentration decreased with increase in particle size.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Cu Interlayer-Induced High-Strength Laser-Welded AISI 304 Steel-Niobium Joint

Joining niobium to austenitic stainless steel is necessary for the fabrication of particle accelerators. However, the brittle iron-niobium intermetallics formed in the joint significantly reduce the joint strength. Copper was used as an interlayer to prevent the brittle phase formation while joining niobium to AISI 304 steel. The laser beam was first focused on the Cu-steel faying surface and then on the Cu-Nb faying surface. The tensile strength of the joint is greater than that of the Nb. The weld microstructure consists of austenite with Cu-rich precipitates along with the austenitic grain boundaries and Cu-rich phase embedded with Nb-rich particles and dendrites. Solid solution strengthening of Cu by Fe and second-phase strengthening of Cu by Nb play a critical role in improving the mechanical properties of the joint. These results highlight new possibilities for the joining of niobium to steel.

36 MATERIALS SCIENCE↗

Dynamics of charge carrier recombination and capture in laser nanostructures with InGaAsSb/AlGaAsSb quantum wells

Time dynamics of photoluminescence intensity was studied in InGaAsSb/AlGaAsSb quantum wells with different compositions of the barrier solid solution and with different width of the quantum wells. The time of charge carrier capture in quantum wells, the energy relaxation times, lifetime related to resonant Auger recombination were estimated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Structure of Relaxor Ferroelectric (1 – 2х)BiScO{sub 3} · хPbTiO{sub 3} · хPbMg{sub 0.33}Nb{sub 0.67}O{sub 3} with х = 0.42 in the Polarized and Depolarized States

An X-ray diffraction study of ceramic samples of relaxor ferroelectric (1 – 2х)BiScO{sub 3} · хPbTiO{sub 3} · хPbMg{sub 0.33}Nb{sub 0.67}O{sub 3} with х = 0.42 in the polarized and depolarized states has been performed. It is established by Rietveld method that in both cases samples contain two perovskite-like phases, which are solid solutions. One of them has cubic symmetry. The second phase is characterized by the polar tetragonal sp. gr. P4mm in the polarized state and the monoclinic noncentrosymmetric sp. gr. Cm in the depolarized state.

36 MATERIALS SCIENCE↗

Extreme Spectroscopy: In situ nuclear materials behavior from optical data

In the nuclear industry, materials are regularly exposed to high temperature or/and irradiation and a better knowledge and understanding of their behavior under such extreme conditions is a key-point for improvements and further developments. Nowadays, Raman spectroscopy begins to be well known as a promising technique in the post mortem and remote characterization of nuclear materials exposed to extreme conditions. On this topic, at ANIMMA 2013 conference, we have presented some results about its implementation in the study of model or real nuclear fuel. However, the strength of Raman spectroscopy as in situ characterization tool is mainly its ability to be implemented remotely through optical fibers. Aware of this, implementation of other optical techniques can be considered in order to gain information not only on the structural dynamics of materials but also on the electronic charge carrier populations. In this paper, we propose to present our last advances in Raman characterization of nuclear materials and enlarge to the in situ use of complementary optical spectroscopies. Emphasis will be made on the information that can be gained to the behavior of the model fuel depleted UO{sub 2} under extreme conditions of high temperature and ionic irradiation: - In Situ Raman identification of the radiolysis alteration products of UO{sub 2} in contact with water under ionic irradiation. - In Situ Raman recording of the damaged dynamic of UO{sub 2} under inert atmosphere. - In Situ Raman and photo-luminescence study of virgin and damaged UO2 at high temperature. - In Situ study of electronic charge carriers' behavior in U{sub x}Th{sub 1-x}O{sub 2} solid solutions by mean of Iono- and Thermo- luminescence under and post- ionic irradiation. (authors)

36 MATERIALS SCIENCE↗

Crystal structure and magnetic properties and Zn substitution effects on the spin-chain compound Sr{sub 3}Co{sub 2}O{sub 6}

The effects of substituting Co on the spin-chain compound Sr{sub 3}Co{sub 2}O{sub 6} with Zn were investigated by synchrotron X-ray diffraction, magnetic susceptibility, isothermal magnetization, and specific heat measurements. To the best of our knowledge, this is the first report to describe the successful substitution of Co in Sr{sub 3}Co{sub 2}O{sub 6} with Zn. The substitution was carried out by a method involving high pressures and temperatures to obtain Sr{sub 3}CoZnO{sub 6}, which crystalized into a K{sub 4}CdCl{sub 6}-derived rhombohedral structure with a space group of R-3c, similar to the host compound. With the Zn substitution, the Ising-type magnetic anisotropy of the host compound remarkably reduced; the newly formed Sr{sub 3}CoZnO{sub 6} became magnetically isotropic with Heisenberg-type characteristics. This could probably be ascribed to the establishment of a different interaction pathway, –Co{sup 4+}(S=1/2)–O–Zn{sup 2+}(S=0)–O–Co{sup 4+}(S=1/2)–. Details of the magnetic properties of Zn substituted Sr{sub 3}Co{sub 2}O{sub 6} were reported. - Graphical abstract: Crystal structure of the spin-chain compound Sr{sub 3}CoZnO{sub 6} synthesized at 6 GPa. Zn atoms preferably occupy the trigonal prism sites rather than the octahedral sites. As a result, the compound is much magnetically isotropic. Highlights: • Effects of substituting Co with Zn on spin-chain magnetism of Sr{sub 3}Co{sub 2}O{sub 6} were studied. • High-pressure synthesis resulted in a solid solution of Sr{sub 3}CoZnO{sub 6}. • Sr{sub 3}CoZnO{sub 6} showed more isotropic magnetism than the host Sr{sub 3}Co{sub 2}O{sub 6}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Magnetic properties of spin frustrated spinel ZnFe{sub 2}O{sub 4}/ZnCr{sub 2}O{sub 4} superlattices

Superlattice films composed of frustrated spin systems, [ZnFe{sub 2}O{sub 4}]{sub m}/[ZnCr{sub 2}O{sub 4}]{sub m}, are grown on MgAl{sub 2}O{sub 4} (111) substrates by pulsed laser deposition, and their frustrated magnetism is studied. The superlattice films show spin-glass behavior and the spin-glass transition temperature (T{sub g}) varies nonmonotonically as a function of the layer thickness m. T{sub g} increases with decreasing m due to an increase in the inhomogeneous exchange interaction between Cr{sup 3+} and Fe{sup 3+} at the interface. However, below m = 4, a decrease in T{sub g} is observed. Compared with the solid solution Zn(CrFe)O{sub 4} film and the other superlattices, the decrease in T{sub g} is considered to be a unique property of the periodically modulated short period superlattices.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Revealing Insights into Li x FePO 4 Nanocrystals with Magnetic Order at Room Temperature Resulting in Trapping of Li Ions

A systematic report on the structures, magnetic properties, and electrochemical performance of Li x FePO 4 was carried out. Interestingly, it was discovered that the magnetic phase transition temperature is around 295 K in Li x FePO 4 (x ≤ 0.12) nanocrystals, which is higher than that of LiFePO 4 (T N = 51(1) K) and FePO 4 (TN = 114(1) K) phases. The origin of magnetic order around room temperature (RT) in LixFePO 4 (x ≤ 0.12) is proposed to be due to both Fe 2+ –Fe 3+ superexchange and the broken local symmetries induced by Fe 2+ –Li + antisite defects. Ab initio calculations were adopted to calculate the total energy change of the ferromagnetic state and antiferromagnetic state (ΔE) to qualitatively estimate T N and proved the existence of the magnetic order around room temperature. Due to the strong Lorentz force in RT magnetic domains, Li ions will be trapped and form sub-10 nm solid solution domains of Li 0+δ FePO 4 , which have a direct relationship with electrochemical performance during (de)lithiation procedures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Structure and Hardness of Ceramics Produced through High-Temperature Nitridation of Titanium Foil

We have studied the variation in the phase composition, elemental composition, and microstructure of rolled titanium samples during thermal annealing in a nitrogen atmosphere at 1300, 1500, 1700, and 2000°C. The results demonstrate that the nitridation process can yield compact titanium nitride-based ceramics or TiN/TiN{sub x}/α-Ti〈N〉 heterostructures. X-ray diffraction data for the near-surface region of the samples before and after nitridation and those for cross-sectional fracture surfaces of heterostructures are used to infer orientation relationships between the TiN phase and α-Ti〈N〉 solid solution. Scanning electron microscopy results for cross-sectional fracture surfaces indicate that complete nitridation of the samples leads to the formation of a three-layer microstructure.

36 MATERIALS SCIENCE↗

High-Temperature Properties and Microstructural Stability of the AISI H13 Hot-Work Tool Steel Processed by Selective Laser Melting

The microstructural stabilities, softening resistance, and high-temperature tensile properties of the H13 hot-work tool steel by selective laser melting (SLM) were systematically studied. A series of tempering procedures were performed on the as-SLMed specimens. Afterwards, the mechanism of softening resistance behavior was discussed based on the XRD, SEM, EBSD observations, hardness measurements, and high-temperature tensile tests. It was found that the as-SLMed H13 consisted of α-iron and γ-iron. The carbide-stabilizing elements aggregated as the cell-like substructures for the rapid solidification of the SLM process. After the softening resistance treatment, the retained austenite transformed to ferrite and carbide mixtures. The cell-like substructures dissolved slowly into the matrix when the temperature was below 550 °C. These factors increased the hardness and retarded the softening of the material. When the temperature was 600 °C, the microstructural constituents transformed to soft ferrite and globular carbides, which lead to a considerable decrease of the hardness. Due to the grain refinement, solid solution strengthening, and residual stress, the as-SLMed H13 exhibited better mechanical properties than that of the wrought counterparts.

36 MATERIALS SCIENCE↗

Microstructure and Phase Composition of Ni-Based Alloy Obtained by High-Speed Direct Laser Deposition

Phase composition and structural features of nickel-based alloy EP741 obtained by high-speed direct laser deposition were discussed in the paper. The technology of high-speed direct laser deposition has been successfully applied during the formation of samples with the various operating parameters of the experimental device. The laser power was between 450 and 1200 W, the scanning speed was 1.2 mm/s, the powder feed rate was 45 g/min, and the laser beam diameter was 1.2 mm. The structure and phase composition of the initial material and as-deposited samples were studied using optical and scanning electron microscopy, x-ray analysis and transmission electron microscopy. The investigation has shown that spherical particles of powder (EP741) can be used to form products by additive manufacturing with the presence of additional heat treatment, since almost all the as-deposited samples obtained do not contain cracks, and large volume of pores was observed only in the sample obtained with the power of 450 W. In addition, the phase composition of the as-deposited samples showed a high content of precipitating phase Ni{sub 3}(Al, Ti) in matrix, which is coherent to the solid solution based on nickel. In theory, the presence of Ni{sub 3}(Al, Ti) phase corresponds to the heat-treated nickel-base alloy obtained by standard methods of processing.

36 MATERIALS SCIENCE↗

Structural, Electrochemical and Hydrogen Sorption Studies of Nanocrystalline Ti-V-Co and Ti-V-Ni-Co Alloys Synthesized by Mechanical Alloying Method

In this paper, Ti-V-Co and Ti-V-Ni-Co alloys are considered as the hydrogen storage systems and the negative electrodes in Ni-MH{sub x} secondary batteries. This work shows results of studies that have been made on Ti{sub 0.5}V{sub 1.5−x}Co{sub x} and Ti{sub 0.5}V{sub 1.4−x}Ni{sub 0.1}Co{sub x} nanocrystalline alloys (x = 0, 0.1 0.2, 0.3) synthesized by the mechanical alloying technique. The goal of this study is to determine an effect of partial replacement of V by Co atoms on hydrogen storage and electrochemical properties of Ti-V and Ti-V-Ni alloys. X-ray diffraction studies have proven that 14 h of the ball milling has resulted in crystallization of body-centered-cubic solid solution. Studies performed on high-resolution transmission electron microscope confirm creation of nanocrystalline materials. Hydrogen sorption/desorption measurements that have been performed at 303 K show that Co accelerates the hydrogen sorption process, diminishes hysteresis and ameliorates the hydrogen storage reversibility. Properties of Ti-V-Co alloys, described in this work, originate mainly from structure of these materials. Electrochemical measurements of Ti-V-Co alloys have shown these materials poorly absorb hydrogen in 6 M KOH solution. Ti{sub 0.5}V{sub 1.4−x}Ni{sub 0.1}Co{sub x} alloys are characterized by better activation properties and improved cyclability in comparison to Co-free Ti{sub 0.5}V{sub 1.4}Ni{sub 0.1} alloy.

36 MATERIALS SCIENCE↗

Effects of Ag addition on FePt L1{sub 0} ordering transition: A direct observation of ordering transition and Ag segregation in FePtAg alloy films

FePt and (FePt){sub 91.2}Ag{sub 8.8} alloy films were deposited by magnetron sputtering. The average coercivity of (FePt){sub 91.2}Ag{sub 8.8} films reaches 8.51 × 10{sup 5} A/m, which is 0.63 × 10{sup 5} A/m higher than that of the corresponding FePt films. Ag addition effectively promotes the FePt L1{sub 0} ordering transition at a relatively low annealing temperature of 400 °C. The promotion mechanism was investigated by using in situ high-resolution transmission electron microscopy (HRTEM) and ex situ X-ray absorption fine structure (XAFS). The concurrence of ordering transition and Ag segregation in FePtAg alloy films was first observed by using in situ heating HRTEM. The time-resolved evolution reveals more details on the role of Ag addition in FePt low-temperature ordering. Ex situ XAFS results further confirm that Ag replaces Fe sites in the as-deposited films and segregates from FePt-Ag solid solution phase through annealing at elevated temperatures. The segregation of Ag atoms leaves vacancies in the grain. The vacancy formation is believed to accelerate the diffusion of Fe and Pt atoms, which is critical for the L1{sub 0} ordering transition.

36 MATERIALS SCIENCE↗

Mechanism of the α-to-β phase transformation in the LaNi 5 -H 2 system

High-energy synchrotron in situ X-ray powder diffraction has been used to elucidate the mechanism of the hydriding phase transformation in a LaNi 5 model hydrogen storage intermetallic in real time. The transformation proceeds at 10 ºC via the transient growth of an interfacial phase, the {gamma} phase, with lattice parameters intermediate between those of the α (dilute solid solution) and β (concentrated hydride) phases. The γ phase forms to partially accommodate the 24% change in unit cell volume between the α and β phases during hydriding and dehydriding. The α, γ and β phases coexist at the nanoscopic level.

08 HYDROGEN↗

Pronounced matrix effect in YbMo{sub 2}Al{sub 4}-type Ca(Au{sub x}Zn{sub 2−x})Au{sub 4} (x=0.09–0.89)

Electron-poor polar intermetallics Ca(Au{sub x}Zn{sub 2−x})Au{sub 4} have been synthesized through fusion of stoichiometric metals in sealed tantalum tubes at 800 °C and annealing at 400 °C for one week. Single crystal X-ray diffraction analyses reveal that this phase belongs to the YbMo{sub 2}Al{sub 4}-type structure (I4/mmm, Pearson symbol tI14), a≈6.943–7.017 Å, c≈5.278–5.286 Å, Z=2, with homogeneous composition range of x=0.09(1)–0.89(1). The structure exhibits a three-dimensional framework of (Au{sub 8}){sub 1/2} featuring square and octagonal channels extending in c, in which Ca and the infinite linear chains of [(Au,Zn){sub 2}]{sub 1/2} are located, respectively. Mulliken population analyses demonstrate that Zn prefers to form the linear chains in the whole homogeneous composition range, consistent with experimental observations. Crystal orbital Hamilton population (COHP) analyses reveal that the channel-to-chain Au–Zn contact has strong bonding interactions regardless of its large interatomic distance (∼2.85 Å), a signature of pronounced matrix effect. The last mentioned effect in YbMo{sub 2}Al{sub 4}-type structures is expected in case the linear chains are defined by small size atoms. - Graphical abstract: Pronounced matrix effect incurred by Au–Au bonding within the gold substructure in Ca(Au{sub x}Zn{sub 2−x})Au{sub 4} results in an elongation of the channel-to-chain Au–Zn interatomic distance without weakening bonding interactions. - Highlights: • The complete solid solution of Ca(Au{sub x}Zn{sub 2−x})Au{sub 4} was accomplished. • Site preference was explained by “coloring” analyses. • Abnormally large Au–Zn distance but with strong bonding was observed. • Pronounced matrix effect incurred by Au–Au bonding in gold substructure was found.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Photocatalytic hydrogen production by water splitting using novel catalysts under UV-vis light irradiation

In this work, photocatalytic hydrogen generation by water splitting (H 2 O (l) →H 2 (g) +1/2O 2 (g) ) has been studied on photocatalysts based on Zn, Cd, Fe and Cu, synthesized by coprecipitation. Iron and copper nanoparticles were incorporated as cocatalysts to enhance the photocatalytic activity of the ZnCd solid solution. The effect of the different synthesis parameters (temperature, elemental atomic ratios, amount of Cu and Fe incorporated in the catalyst and calcination temperature) on the photocatalytic production of hydrogen has been studied in order to determine the best experimental synthesis conditions. The catalysts have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and BET. The experiments of photocatalytic water splitting were performed in aqueous solution of the photocatalysts previously dispersed in a soft ultrasound bath. The photocatalysts were irradiated under different lights ranging from 220 to 700 nm. Furthermore, the photocatalytic activity was found to be clearly dependent on the specific area of the photocatalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗