Experimental and theoretical studies on bis(glycine) lithium nitrate (BGLiN): A physico-chemical approach

Good quality and bulk size single crystal (size: 20×13×8 mm³) of bis(glycine) lithium nitrate (BGLiN) was grown by a slow evaporation solution technique from the aqueous solutions at constant temperature i.e. 27 °C using synthesized materials. Crystal system and lattice parameters were determined by single crystals as well as powder X-ray diffraction analysis. The lattice parameters of the titled compound are a=10.0223 Å, b=5.0343 Å, c=17.0510 Å, and V=860.312 Å³ and it crystallized in an orthorhombic system with space group Pca2₁ obtained by single crystal XRD. Elemental composition was confirmed by energy dispersive X-ray spectroscopic analysis. Optical absorption spectrum was recorded and various optical parameters such as optical transmission (~60%), and optical band gap (4.998 eV) were calculated. Photoluminescence study shows that the grown crystal is free from major defects. Crystalline perfection of the grown crystal was assessed and found good. Ground state optimized geometry has been obtained by using DFT with 6-31G(d,p) basis set. HOMO and LUMO energy gap was found to be 6.01 eV and dipole moment was 1.65 D.     

X-ray diffraction analysis of the surface acoustic wave propagation in langatate crystal

X-ray diffraction on a langatate crystal (La₃Ga_5.5Ta_0.5O₁₄, LGT) modulated by a Λ=12 μm Rayleigh surface acoustic wave (SAW) was studied in a double axis X-ray diffractometer scheme at the BESSY synchrotron radiation source. SAW propagation in the crystal causes sinusoidal modulation of the crystal lattice and the appearance of diffraction satellites on the rocking curves, with their number, angular positions, and intensities depending on the wavelength and amplitude of acoustic vibrations of the crystal lattice. Strong absorption of X-ray radiation in LGT enables the observation of the diffraction spectra extinction at certain SAW amplitudes. X-ray diffraction spectra analysis makes it possible to determine SAW amplitudes and wavelengths, to measure the power flow angles, and investigate the diffraction divergence in acoustic beam in LGT.     

Chemical composition and structural phase changes of Pd sample and properties of novel synthesized structure at dense deuterium gas under irradiation by γ-quanta

Studies have been carried out into the element composition of Pd and brass with associated materials and synthesized novel structure, placed in dense deuterium gas in a deuterium high-pressure chamber (DHPC) under the pressure 3 kbar and irradiated with ??-quanta of energy up to 8.8 MeV. Using the methods of scanning electron microscopy, microelement chemical analysis and X-ray diffraction, it was determined that in the absence in the chamber volume and walls of all HPC-forming materials the synthesized structure is largely composed of alumosilicates and Al and Si oxides with high content of Ti compounds as rutile TiO₂. Pd_1.5D₂. Considerable anomalies in the chemical composition were found both in the surface and at large depth in a Pd specimen. The entire Pd surface turned into a structure comprised of Pd clusters, Cu and Zn compounds, with a notable content of Mg, Al, S, Si, K, Ca, Ti and Fe compounds. Results of evaluative calculations, including computation of the Q-value, are presented for nuclear reactions produced in a saturated with deuterium Pd specimen and dense deuterium gas under the action of ??-quanta, neutrons and protons of energies up to E _n + E _p ?? E _?? ? E _D MeV generated by deuteron fission. The obtained results can be explained by ??collective effects?? as chain reactions caused by deuteron fission induced by protons (E _p > 3.39 MeV) and neutrons (E _n > 2.25 MeV), as well as by thermonuclear synthesis of deuterium atoms elastically scattered by protons of energies up to E _P < E _?? ? E _D MeV.     

Optical polarized properties related to the oxygen vacancy in the CaMoO4 crystal

The electronic structures, dielectric functions and absorption spectra for the CaMoO₄ (CMO) crystal with and without oxygen vacancy V_O²⁺ have been calculated using the CASTEP code with the lattice structure optimized. The calculated results indicate that the optical properties of the CMO crystal show anisotropy and its optical symmetry coincides with the lattice structure geometry of the CMO crystal. The calculated absorption spectra indicate that the perfect CMO crystal does not display absorption band in the visible and near-ultraviolet range. However, in this range, the absorption spectra of the CMO crystal containing V_O²⁺ exhibit one peak at about 1.84 eV (673 nm). It predicates that the 680 nm absorption band is related to the existence of V_O²⁺ in the CMO crystal.     

Structural and magnetic studies on RPtIn deuterides (R=Tb,Er, Tm)

In this communication, structural and magnetic properties of RPtInD_1.3 (R=Tb, Er, Tm) deuterides are reported. For the first time deuterium-rich compounds were synthesized for the RPtIn family. The investigated deuterides crystallize with the hexagonal ZrNiAl-type crystal structure, with slightly different lattice constants with respect to the basic compounds. In general, the a-lattice constant exhibit contraction, while the c-lattice constant tends to increase upon introducing deuterium. The compounds with Tb and Er shows magnetic ordering at 95 K and 15.5 K, respectively. On the other hand, for Tm based sample no magnetic ordering was evidenced down to 2 K.     

Stabilization of high spin FCC Fe in (Fe/Pd)n multilayers

Polycrystalline (Fe/Pd)_n multilayers are grown onto sapphire substrates at room temperature in a UHV system. The number of periods n=40 and the thickness of Pd layers of t_Pd=4 nm are kept constant, whereas the thickness of the Fe layers is varied from 1.5 to 5 nm. Structural properties are studied by in situ reflection high energy diffraction (RHEED), scanning tunnelling microscopy (STM) and ex situ by X-ray diffraction at small angles and large angles. Analyzing the experimental data using the program SUPREX we obtain interplanar distances of d_Fe=2.03±0.01 Å for an Fe layer thickness larger than about 2.5 nm as expected for (1 1 0) planes of BCC Fe. For Fe layers with thicknesses less than about 2.5 nm the interplanar distance is d_Fe=2.1±0.01 Å, which is close to the distance between (1 1 1) planes of FCC Fe with a lattice parameter of a=3.64 Å. Magnetic susceptibility measurements at temperatures between 1.5 and 300 K for (Fe/Pd)_n multilayers with FCC Fe yield a magnetic moment per Fe atom of μ=2.7±0.1 μ_B, which is about 20% larger compared to μ=2.2 μ_B for BCC Fe. We show that the occurrence of the large magnetic moment originates from FCC Fe being in the high spin (HS) state rather than from polarization effects of Pd at Fe/Pd interfaces.     

Third order nonlinear optical properties of potassium dichromate single crystals by Z-scan technique

Single crystal of potassium dichromate (KDC) has been grown from aqueous solution by slow evaporation technique. The lattice parameters of the grown crystal were determined by X-ray diffraction analysis. The optical absorption studies reveal that the crystal has UV cut-off wavelength around 240 nm. Thermo gravimetric and differential thermal (TGA/DTA) studies revealed that the crystal thermally stable up to 397.1 °C. The mechanical strength of the grown crystal was carried out by Vickers micro hardness test. The crystal perfection was confirmed by etching studies. Third order nonlinear optical studies was performed using by single beam Z-scan technique using continuous Nd:YAG laser. Closed aperture Z-scan studies reveal the negative nonlinearity in the crystals and open aperture Z-scan reveals the saturation absorption. Also various parameters such as nonlinear refractive index n₂, absorption co-efficient β and nonlinear optical susceptibility χ⁽³⁾ were calculated for the grown crystal.     

Fluid synthesis and structure of a new polymorphic modification of boron nitride

A new previously unknown phase of boron nitride with a hardness of 0.41–0.63 GPa has been pre-pared by the supercritical fluid synthesis. The presence of a new phase is confirmed by the X-ray spectra and IR absorption spectra, where new reflections and bands are distinguished. The fundamental reflection of the X-ray diffraction pattern is d = 0.286–0.291 nm, and the characteristic band in the infrared absorption spectrum is observed at 704 cm^?1. The X-ray diffraction pattern and the experimental and theoretical infrared absorption spectra show that a new synthesized boron nitride phase can be a cluster crystal (space group 211) with a simple cubic lattice. Cage clusters of a fullerene-like morphology B₂₄N₂₄ with point symmetry O are arranged in lattice sites.     

Magnetic frustration in the antiferromagnetic Kondo lattice YbPtAl: Anomalous magnetic behavior at high pressures

We have investigated the magnetic and electronic properties of the antiferromagnetic Kondo lattice YbPtAl using the ¹⁷⁰Yb Mössbauer effect at ambient pressure (1.8<T<10 K), electrical resistance (1.8<T<300 K) and X-ray diffraction (T=300 K) techniques at high pressures up to 26 GPa. We find a complex magnetic state in YbPtAl at ambient pressure and an unusual volume-induced change of T_N. It is suggested, that the anomalous volume dependence of T_N is due to the interplay between frustrated anisotropic exchange interactions and magnetocrystalline anisotropy. The magnetic frustration originates from the topology of the crystal lattice.     

Thermal evolution of the crystal structure of the correlated 4d post-perovskite CaRhO3

Thermal effect on the orthorhombic crystal structure (Cmcm) of the correlated 4d post-perovskite CaRhO₃ was investigated by an X-ray powder diffraction method between 60 K and 300 K. Anisotropic thermal evolution of the structure was observed over the temperature range, and in addition, an anomalous change of the lattice parameters was detected at the antiferromagnetic transition temperature of 90 K, indicating possible correlations between the lattice and the magnetic order.     

The kinetics of hydrogen (deuterium) sorption by thin palladium layers studied with a piezoelectric quartz crystal microbalance

The kinetics of the hydrogen (deuterium) Sorption processes in the α-phase region of a thin electrodeposited Pd layer (thickness 3 × 10^?5 cm) are reported. Measurements have been performed with a piezoelectric quartz crystal microbalance using an AT-cut crystal with a resonance frequency f⁰_q = 5.27 MHz and a sensitivity of ～10¹⁰ digits g^?1, at a constant temperature 80.3 ± 0.05 °C and different pressures. Both the absorption and the desorption of H₂(D₂) on Pd layers are controlled successively by a chemisorption step (second order kinetics) in the early stage of the processes and by a surface migration step (first order kinetics), in the subsequent stage of the processes. Consistent with the reported piezoelectric quartz crystal microbalance measurements, thermal desorption and electrochemical desorption studies, a mechanism is suggested which takes into account the adsorption ofH(D) atoms on two different surface states: (a) a “pre-dissolved” state which does not depend on the surface nature; (b) and adsorption state, the density of which depends upon the structure and nature of the Pd sample. The kinetic control of the entire processes (sorption and desorption) depends on the ratio of the density of sites (a) to (b).     

Evolution of structural properties of iron oxide nano particles during temperature treatment from 250 °C-900 °C: X-ray diffraction and Fe K-shell pre-edge X-ray absorption study

Iron oxide nano particles with nominal Fe₂O₃ stoichiometry were synthesized by a wet, soft chemical method with heat treatment temperatures from 250 °C to 900 °C in air. The variation in the structural properties of the nano particles with the heat treatment temperature was studied by X-ray diffraction and Fe K-shell X -ray absorption spectroscopy. X-ray diffractograms show that at lower annealing temperatures the nano particle comprise both maghemite and hematite phases. With increasing temperature, the remainder of the maghemite phase transforms completely to hematite. Profile analysis of the leading Bragg reflections reveals that the average crystallite size increases from 50 nm to 150 nm with increasing temperature. The mean primary particle size decreases from 105 nm to 90 nm with increasing heat treatment temperature. The X-ray diffraction results are paralleled by systematic changes in the pre-edge structure of the Fe K-edge X-ray absorption spectra, in particular by a gradual decrease of the t_2g/e_g peak height ratio of the two leading pre-edge resonances, confirming oxidation of the Fe from Fe²⁺ towards Fe³⁺. Transmission electron microscopy (TEM) on the samples treated at temperatures as high as 900 °C showed particles with prismatic morphology along with the formation of stacking fault like defects. High resolution TEM with selected area electron diffraction (SAED) of samples heat treated above 350 °C showed that the nano particles have well developed lattice fringes corresponding to that of (110) plane of hematite.     

硼(氮、氟)掺杂对TiO2纳米颗粒光学性能的影响

利用X射线衍射谱、拉曼光谱和紫外-可见光吸收光谱研究了硼(氮、氟)掺杂对TiO₂纳米颗粒光学性能的影响.X射线衍射谱和拉曼光谱结果表明,掺硼(氮、氟)对TiO₂纳米颗粒的锐钛矿相晶体结构无明显影响,而其锐钛矿晶格出现畸变(c/a值增大),这被归因于掺杂原子对TiO₂纳米颗粒表面氧原子缺位沿晶格c轴方向的占据.另外,掺硼(氮、氟)TiO₂纳米颗粒吸收带红移与TiO相似文献   

Low-stability pre-transitional states,orderdisorder phase transitions,and <Emphasis Type="Italic">B</Emphasis>2–<Emphasis Type="Italic">A</Emphasis>1 structure transformations in the Cu – 40 at.% Pd alloys

Low-stability states and peculiarities of structural changes in the region of phase transitions are investigated using the Cu–Pd ~40 at.% Pd alloys as an example. To this end, the crystal lattice and long-range atomic order parameters and the Debye-Waller factors were determined in situ directly in the temperature range of the B2–A1 phases and the order – disorder phase transition using X-ray structural analysis. Based on the data obtained, peculiarities of the B2 and A1 phases in the CuPd alloys were analyzed near the structure-phase transitions and the behavior pattern of atomic vibrations in the crystal lattice was discussed. It is shown that in the CuPd alloys with ~40 at.% Pd, low-stability states are observed, which exhibit a number of anomalous phenomena (such as anisotropy of atomic displacements, splitting, heterophase fluctuations, nonlinearity of the lattice parameter and long-range order parameter dependences, etc.), which precede transformation of the alloy.     

Synthesis and characterization of the Pd/InVO4-TiO2 co-doped thin films with visible light photocatalytic activities

Novel Pd/InVO₄-TiO₂ thin films with visible light photocatalytic activity were synthesized from the Pd and InVO₂ co-doped TiO₂ sol via sol-gel method. The photocatalytic activities of Pd/InVO₄-TiO₂ thin films were investigated based on the oxidative decomposition of methyl orange in aqueous solution. The as-prepared samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy (UV-vis). The results indicate that the Pd/InVO₄-TiO₂ thin films are compact, uniform and consist of sphere nanoparticles with diameters about 80-100 nm. The UV-vis spectra show that the Pd/InVO₄-TiO₂ thin films extend the light absorption spectrum toward the visible region. XPS results reveal that doped Pd exist in the form of metallic palladium. The photocatalytic experiments demonstrate that Pd doping can effectively enhance the photocatalytic activities of InVO₄-TiO₂ thin films in decomposition of aqueous methyl orange under visible light irradiation. It has been confirmed that Pd/InVO₄-TiO₂ thin films could be excited by visible light (E < 3.2 eV) due to the existence of the Pd and InVO₄ doped in the films.     

RAIRS studies of CO adsorption on Pd/CeO2−x(1 1 1)/Pt(1 1 1)

Reflection absorption infrared spectroscopy (RAIRS) has been used to investigate the adsorption of CO on CeO_2−x-supported Pd nanoparticles at room temperature. The results show that when CeO_2−x is initially grown on Pt(1 1 1), a small proportion of the surface remains as bare Pt sites. However, when Pd is deposited onto CeO_2−x/Pt(1 1 1), most of the Pd grows directly on top of the CeO_2−x(1 1 1). RAIR spectra of CO adsorption on 1 ML Pd/CeO_2−x/Pt(1 1 1) show a broad CO-Pd band, which is inconsistent with a single crystal Pd surface. However, the 5 ML and 10 ML Pd/CeO_2−x/Pt(1 1 1) spectra show vibrational bands consistent with the presence of Pd(1 1 1) and (1 0 0) faces, suggesting the growth of Pd nanostructures with well defined facets.     

An XAS study of the defect structure of Ti-doped α-Cr2O3

The bulk defect structure in Cr_2−xTi_xO₃ (x = 0.05, 0.20 and 0.30) has been studied by X-ray absorption spectroscopy measurements at the Cr and Ti K-edges. The results show that the Ti is predominantly present in the IV oxidation state and resides on the normal Cr host lattice site. The dopant is charge compensated by Cr³⁺ vacancies and there is evidence for the formation of defect clusters; however, the detailed structure of these clusters could not be deduced.     

Study of palladium nanoparticles synthesized in alkali borosilicate glass pores by the X-ray line shift method

Metallic Pd synthesized in porous glass with an average pore diameter of 7 ± 2 nm has been studied using the X-ray diffraction and X-ray line shift methods for the first time. The irregular dependence of the reflection width in X-ray patterns on the diffraction angle has been revealed. This can be caused by crystallite growth mostly in the [111] direction or by tetrahedral distortions of the fcc lattice. The shift (difference in energy) of K _α1 lines (ΔE _α1 = 19 ± 2 meV) for nanostructured Pd in comparison with the bulk material is first detected. The detected effect is considered within the assumption of the palladium electron redistribution between Pd 5s- and 4d-bands.     

Effect of surface oxidation on the surface condition and deuterium permeability of a palladium membrane

Oxidation and deoxidation of a Pd membrane was conducted in a quartz tube oven in a temperature range of 23-500 °C. The micromorphology and chemical composition of the Pd membrane surface was characterized using scanning electronic microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Micropores and PdO began to form on the Pd membrane surface after oxidation at 240 °C for 1 h and their quantity increased gradually with increasing temperature. A rough Pd membrane surface was obtained when the temperature rose to 500 °C. The PdO on the Pd membrane surface was completely deoxidized once more using H₂ at room temperature, but the rough surface morphology caused by oxidation remained. The deuterium permeability of the Pd membrane was tested using special equipment in the China National Key Laboratory and the results indicated that the rough Pd membrane surface had higher deuterium permeability than the original membrane. The improved deuterium permeability could be attributed to the higher Pd membrane surface area, which provided deuterium atoms with more adsorption sites and dissociation sites.     

Synthesis of BaSO4 nanoparticles by precipitation method using sodium hexa metaphosphate as a stabilizer

We describe the synthesis and structure of Barium sulfate nanoparticles by precipitation method in the presence of water soluble inorganic stabilizing agent, sodium hexametaphosphate, (NaPO₃)₆. The structural parameters were refined by the Rietveld refinement method using powder X-ray diffraction data. Barium sulfate nanoparticles were crystallized in the orthorhombic structure with space group Pbnm (No. 62) having the lattice parameters a=7.215(1) (Å), b=8.949(1) (Å) and c=5.501(1) (Å) respectively. Transmission electron microscopy study reveals that the nanoparticles are size range, 30–50 nm. Fourier transform infrared spectra showed distinct absorption due to the SO₄^2? moiety at 1115 and 1084 cm^?1 indicating formation of barium sulfate nanoparticles free from the phosphate group from the stabilizer used in the synthesis.