Synthesis and magnetic properties of Ni-doped zinc oxide powders

Polycrystalline Zn_1−xNi_xO diluted magnetic semiconductors have been successfully synthesized by an auto-combustion method. X-ray diffraction measurements indicated that the 5 at% Ni-doped ZnO had the pure wurtzite structure. Refinements of cell parameters from powder diffraction data revealed that the cell parameters of Zn_0.95Ni_0.05O were a little bit larger than ZnO. Transmission electron microscopy observation showed that the as-synthesized powders were of the size ∼60 nm. Magnetic investigations showed that the nanocystalline Zn_0.95Ni_0.05O possessed room temperature ferromagnetism with the saturation magnetic moment of 0.1 emu/g (0.29 μ_B/Ni²⁺).     

Thermal expansion and structure of orthorhombic CaMnO3

The structure of CaMnO₃ has been studied from room temperature to 800 °C by high-resolution synchrotron X-ray powder diffraction. It is concluded that CaMnO₃ remains orthorhombic in Pbnm over the entire temperature range, with the expansion in the cell volume well fitted to the expression Vol=207.37(2)+0.00563(8)T+1.17(9)×10^-6T². The magnitude of the MnO₆ tilts is estimated from the refined structural parameters and these progressively reduce as the temperate is increased.     

A high-pressure Raman and X-ray diffraction study of the perovskite SrCeO3

A high-pressure structural study of SrCeO₃ has been performed at room temperature by Raman spectroscopy and X-ray diffraction up to 32 and 45 GPa, respectively. A first-order reversible phase transition is observed at about 12 GPa in both techniques. A second weak structural change, taking place between 18 and 25 GPa, can be suspected from Raman data. The increase in the number of Raman bands and diffraction lines is an indication that the symmetry is lowered and the compound does not evolve towards the ideal cubic perovskite structure. A Rietveld analysis of X-ray data was performed for the low-pressure phase and the atomic positions and the cell lattice parameters variations are reported in this paper. The volume compressibility derived from Raman modes (5.6×10⁻¹² Pa⁻¹), involving mainly bond-stretching for each type of polyhedron, is found to be close to the one obtained from volume cell variations measured by X-ray diffraction (7.9×10⁻¹² Pa⁻¹).     

Equation of state for technetium from X‐ray diffraction and first-principle calculations

The ambient temperature equation of state (EoS) of technetium metal has been measured by X-ray diffraction. The metal was compressed using a diamond anvil cell and using a 4:1 methanol-ethanol pressure transmitting medium. The maximum pressure achieved, as determined from the gold pressureEquation of state for technetium from X-ray diffraction and first-principle calculations scale, was 67 GPa. The compression data shows that the HCP phase of technetium is stable up to 67 GPa. The compression curve of technetium was also calculated using first-principles total-energy calculations. Utilizing a number of fitting strategies to compare the experimental and theoretical data it is determined that the Vinet equation of state with an ambient isothermal bulk modulus of B_0T=288 GPa and a first pressure derivative of B′=5.9(2) best represent the compression behavior of technetium metal.     

Magneto-structural correlations in Pr0.15Gd0.85Mn2Ge2

Magneto-structural correlations in Pr_0.15Gd_0.85Mn₂Ge₂ have been studied by synchrotron diffraction in the temperature range between 11 and 300 K. This compound crystallizes in the ThCr₂Si₂-type structure (space group ). The unit cell parameters a and c were determined by Rietveld refinements as a function of temperature. Anomalies in the temperature dependence of the unit cell parameters a and c, the c/a ratio and the unit cell volume V at about 240 and 140 K, which is close to the magnetic phase transition temperatures, indicate a pronounced magneto-structural correlation. Spontaneous volume change and linear magnetostrictions are derived as a function of temperature.     

Role of composite MnO2 cathode on electrochemical cells based on polymer electrolyte (PEO/NaClO3)

Thin-film sodium-ion-conducting polymer electrolyte based on polyethylene oxide (PEO) system was prepared by solvent casting method. The thin-film electrolytes were characterized by X-ray diffraction (XRD), infrared (IR), cyclic voltammetry (CV) and alternating current conductivity, and Wagner’s polarization method. The complexation of salt with PEO was confirmed by XRD and IR studies. The charge transport of these electrolytes is mainly due to ions, which was confirmed by the transference number experiment. The conductivity studies show that the conductivity value of PEO/NaClO₃ complex increases with the increase of temperature as well as the addition of low molecular weight polyethylene glycol, dimethyl formamide, and propylene carbonate. The electrolyte stability and cell reversibility were analyzed by CV studies. Electrochemical cells have been fabricated with a common cell configuration Na|electrolyte|(MnO₂ + I₂ + C + electrolyte), and their discharge characteristic studies were made through a load 100 kΩ at room temperature. The measured open circuit voltage ranges from 2.80 to 2.54 V with short circuit current ranges from 667 to 1,000 μA and several other cell parameters were evaluated. Finally, the merit of the composite cathode is found with the comparison of the MnO₂ cathode.     

Electrochemical deposition of quaternary Cu2ZnSnS4 thin films as?potential solar cell material

Quaternary compound semiconductor Cu₂ZnSnS₄ (CZTS), which appears to be a promising candidate for the absorber of a thin film type solar cell, was grown on polycrystalline Ag substrates by electrochemical epitaxial method. The elements were deposited in the following sequence: S/Sn/S/Cu/S/Zn/S/Cu… , the order being one cycle of SnS, one cycle of ZnS and two cycles of CuS. Morphology of the deposit has been characterized by field emission scanning electron microscopy (FE-SEM) with an energy dispersive X-ray (EDX) analyzer. X-ray diffraction (XRD) studies showed a (112) preferred orientation for the deposit. X-ray photoelectron spectroscopy (XPS) of the deposit indicated an approximate ratio 2:1:1:4 of Cu, Zn, Sn, and S, the expected stoichiometry for the deposit, and similar results have been obtained from EDX data. Near IR absorption measurements of the deposit at room temperature indicated a direct band gap of 1.5 eV, and open-circuit potential (OCP) studies indicated a good p-type property, both of which were suitable for fabricating a thin film solar cell.     

Electrosynthesis and characterization of Fe doped CdSe thin films from ethylene glycol bath

The CdSe and Fe doped CdSe (Fe:CdSe) thin films have been electrodeposited potentiostatically onto the stainless steel and fluorine doped tin oxide (FTO) glass substrates, from ethylene glycol bath containing (CH₃COO)₂·Cd·2H₂O, SeO₂, and FeCl₃ at room temperature. The doping concentration of Fe is optimized by using (photo) electrochemical (PEC) characterization technique. The deposition mechanism and Fe incorporation are studied by cyclic voltammetry. The structural, surface morphological and optical properties of the deposited CdSe and Fe:CdSe thin films have been studied by X-ray diffraction, scanning electron microscopy (SEM) and optical absorption techniques respectively. The PEC study shows that Fe:CdSe thin films are more photosensitive than that of undoped CdSe thin films. The X-ray diffraction analysis shows that the films are polycrystalline with hexagonal crystal structure. SEM studies reveal that the films with uniformly distributed grains over the entire surface of the substrate. The complete surface morphology has been changed after doping. Optical absorption study shows the presence of direct transition and a considerable decrease in bandgap, E_g from 1.95 to 1.65 eV.     

In situ neutron diffraction study (300-1273 K) of non-stoichiometric strontium ferrite SrFeOx

The high-temperature cubic phase of non-stoichiometric strontium ferrite SrFeO_x (2.5≤x≤3.0) has been studied by in situ neutron powder diffraction in air over the temperature range 300-1273 K. The composition of SrFeO_x changes within the range 2.56≤x≤2.81 from 1273 to 673 K, respectively.Rietveld refinements of the diffraction patterns show that the high-temperature cubic phase of SrFeO_x is consistent with a face-centred Fm3c structure. This structure leads to agreement with previous density measurements. This cell allows the high-temperature structure of SrFeO_x to be described in terms of a solid solution of the composition end members. Cubic SrFeO_x at high temperature is found to closely obey Vegard's law. The density of cubic SrFeO_x is also found to exhibit a linear relationship with composition.     

Spray pyrolytic synthesis of samarium doped ceria (Ce0.8Sm0.2O1.9) films for solid oxide fuel cell applications

Uniform, adherent, single phase samarium doped ceria films have been successfully deposited by spray pyrolysis technique for their application in solid oxide fuel cell. These films have been deposited at different substrate temperatures on glass substrate and subsequently heat treated in tube furnace. Effect of substrate temperature and annealing temperature on phase formation was studied with thermo-gravimetric analysis and differential temperature analysis, X-ray diffraction, scanning electron microscope, and energy dispersive X-ray analysis techniques. These studies showed the formation of single phase Ce_0.8Sm_0.2O_1.9 films, at substrate temperature 400 °C and annealing temperature 550 °C. Electrical resistivity of the films, at room temperature was of the order of 10⁷ Ω cm while at 400 °C it is found to be of the order of 10¹ Ω cm. This reveals the use of these films for making low temperature solid oxide fuel cells.     

High pressure cell for neutron diffraction investigations

Abstract

The design of a titanium-zirconium clamped cylinder-piston type pressure cell for neutron diffraction investigations under hydrostatic pressure up to 10 kbars without supports is described. It is the first time that Freon-11 has been used as a hydrostatic pressure transmitting medium. The following results carried out at the room temperature are presented: the discovery of the transition from I to 111 phase in a LiKSO₄ single crystal and the results of the investigation on the influence of pressure upon the structure of the YBaCuO HTSC obtained by means of the powder diffraction method.     

Structural analysis of nickel doped cobalt ferrite nanoparticles prepared by coprecipitation route

Magnetic nanoparticles of nickel substituted cobalt ferrite (Ni_xCo_1−xFe₂O₄:0≤x≤1) have been synthesized by co-precipitation route. Particles size as estimated by the full width half maximum (FWHM) of the strongest X-ray diffraction (XRD) peak and transmission electron microscopy (TEM) techniques was found in the range 18–28±4 nm. Energy dispersive X-ray (EDX) analysis confirms the presence of Co, Ni, Fe and oxygen as well as the desired phases in the prepared nanoparticles. The selective area electron diffraction (SAED) analysis confirms the crystalline nature of the prepared nanoparticles. Data collected from the magnetization hysteresis loops of the samples show that the prepared nanoparticles are highly magnetic at room temperature. Both coercivity and saturation magnetization of the samples were found to decrease linearly with increasing Ni-concentration in cobalt ferrite. Superparamagnetic blocking temperature as determined from the zero field cooled (ZFC) magnetization curve shows a decreasing trend with increasing Ni-concentration in cobalt ferrite nanoparticles.     

The effect of solution temperature on crystallite size and magnetic properties of Zn substituted Co ferrite nanoparticles

In this work zinc substituted cobalt ferrite nanoparticles (Co_0.5Zn_0.5Fe₂O₄) have been synthesized by the coprecipitation method, using stable ferric, zinc and cobalt salts with sodium hydroxide, at different solution temperatures, from room temperature to 363 K. The cobalt-zinc ferrite crystalline phase, the particle size and the morphology of the resulting nanoparticles were studied by X-ray diffraction and transmission electron microscopy. The average crystallite size of each sample was calculated from the broadening of the most intense peak (3 1 1), using Scherrer's formula and the results show crystallite sizes increased from 6 to 8 nm by increasing the solution temperature from room temperature to 363 K respectively. Room temperature VSM measurements show that the prepared nanoparticles have superparamagnetic behavior and did not saturate at maximum field of 800 kA/m. The variation of AC-susceptibility of the samples with respect to temperature was measured and it was found that the blocking temperature increased from 198 to 270 K by increasing the solution temperature from room temperature to 363 K respectively. FTIR spectra of the samples have been analyzed in the frequency range 400-4000 cm⁻¹, which also confirms the results of XRD.     

Anomalies in the physical properties of the α form of bismuth oxide

Several of the physical properties of α-Bi₂O₃ have been studied in the temperature region above room temperature: the thermal expansion, the thermally stimulated current, the permittivity, the electrical resistance, and the specific heat. X-ray diffraction measurements and a thermogravimetric analysis have also been carried out. Several unusual properties in the physical properties of bismuth oxide have been detected in the temperature interval 450–570 K: exothermic maxima on the DTA and DSC curves, a small maximum and a sharp increase of the permittivity of the single crystal, a jump and a change of sign in the thermally stimulated current, and a sharp falloff of the electrical resistance of ceramic samples. At the same time, no appreciable changes in the monoclinic structure of α-Bi₂O₃ have been recorded in the indicated temperature interval. Fiz. Tverd. Tela (St. Petersburg) 39, 865–870 (May 1997)     

Negative thermal expansion and phase transition behaviour in Ag2O

The structure of Ag₂O has been studied between 5 and 300 K using both high resolution synchrotron X-ray and neutron powder diffraction methods. Ag₂O exhibits strong negative thermal expansion below 200 K and the cell volume is only weakly temperature dependent between 200 and 300 K. There is evidence for a first order phase transition below 35 K in Ag₂O and this is apparently related to displacive disorder of the Ag cations. This disorder contributes to the observed NTE.     

Temperature variation of the Debye-Waller factors of Ba++ and F− ions in BaF2 powder by x-ray diffraction

The temperature variation of the Debye-Waller factors of Ba⁺⁺ and F⁻ ions in BaF₂ powder has been studied using x-ray powder diffraction over the temperature range 77°–298°K. A continuous flow cryostat has been specially fabricated for this purpose for the YPC 50 NM powder diffractometer available in the department. The Debye-Waller factors of Ba⁺⁺ and F⁻ between room temperature and 879°K have been measured using single crystal neutron diffraction by Cooperet al. Theoretical lattice dynamics shell model calculations using a 7-parameter model in a quasiharmonic approximation have been done over a temperature range 77° to 879°K. The theoretical values have been compared with the present x-ray measurements and the single crystal neutron diffraction values and the results are discussed.     

The characteristics of Au:VO2 nanocomposite thin film for photo-electricity applications

Au nanoparticles have been fabricated on normal glass substrates using nanosphere lithography (NSL) method. Vanadium dioxide has been deposited on Au/glass by reactive radio frequency (rf) magnetron sputtering. The structure and composition were determined by X-ray diffraction and X-ray photoelectron spectroscope. Electrical and optical properties of bare VO₂ and Au:VO₂ nanocomposite thin films were measured. Typical hysteresis behavior and sharp phase transition were observed. Nanopartical Au could effectively reduce the transition temperature to 40 °C. The transmittance spectrum for both Au:VO₂ nanocomposite thin film shows high transmittance under transition temperature and low transmittance above transition temperature. The characteristics present the Au:VO₂ nanocomposite thin film can be used for applications, such as “smart window” or “laser protector”.     

Structural and optical characterization of Ce-doped Gd2SiO5 films by sol-gel technique

Cerium-doped Gd₂SiO₅ (GSO:Ce) films have been prepared on (1 1 1) silicon substrates by the sol-gel technique. Annealing was performed in the temperature range from 400 to 1000 °C. X-ray diffraction (XRD), and atomic force microscopy (AFM) were used to investigate the structure and morphology of GSO:Ce films. Results showed that GSO:Ce film starts to crystallize at about 600 °C, GSO:Ce films have a preferential (0 2 1) orientation, as the annealing temperature increase, the (0 2 1) peak intensity increases, the full width of half maximum (FWHM) decreases, and the grain size of GSO:Ce films increases. Emission spectra of GSO:Ce films were measured, results exhibit the characteristic blue emission peak at 427 nm.     

In situ high-pressure X-ray diffraction study of densification of a molecular chalcogenide glass

Structural mechanisms of densification of a molecular chalcogenide glass of composition Ge_2.5As_51.25S_46.25 have been studied in situ at pressures ranging from 1 atm to 11 GPa at ambient temperature as well as ex situ on a sample quenched from 12 GPa and ambient temperature using high-energy X-ray diffraction. The X-ray structure factors display a reduction in height of the first sharp diffraction peak and a growth of the principal diffraction peak with a concomitant shift to higher Q-values with increasing pressure. At low pressures of at least up to 5 GPa the densification of the structure primarily involves an increase in the packing of the As₄S₃ molecules. At higher pressures the As₄S₃ molecules break up and reconnect to form a high-density network with increased extended-range ordering at the highest pressure of 11 GPa indicating a structural transition. This high-density network structure relaxes only slightly on decompression indicating that the pressure-induced structural changes are quenchable.     

Decomposition of the hexagonal copper hydride at high pressure

The process of decomposition of hexagonal copper hydride has been observed in situ in a diamond anvil cell (DAC) using the energy dispersive X-ray diffraction (EDXRD) method. The presence and intensity of diffraction lines of the hexagonal CuH_0.8 phase have been taken as a probe for the decomposition process. The intensity of diffraction lines decreases abruptly in the vicinity of 8.4 GPa, indicating complete decomposition of the hydride. The determined value of decomposition pressure is equal to 8.4±0.6 GPa. The standard Gibbs energy of formation of 54.0±1.3 kJ mol⁻¹ (H₂) calculated for copper hydride has been compared with the result obtained from calorimetric studies. The large discrepancy between the two values suggests that the decomposition pressure does not describe ‘true’ equilibrium conditions in this system.