Anharmonic Effects in Germanium

A precise X-ray investigation is carried out to probe the lowest-order anharmonic contribution of the atomic potential of the germanium atom. A total number of 1052 reflections (h + k + l = 4n and 4n +/- 1) are precisely measured at room temperature using a spherical single crystal of germanium and using a Nonius CAD-4 X-ray diffractometer with crystal monochromatized MoKalpha radiation. A least-square refinement program is used to refine the harmonic and anharmonic thermal parameters of the crystal. The refinement gives beta(Ge) = (-0.749 +/- 1.79) x 10-(16) J nm-3 with B(Ge) = (0.528 +/- 0.004) x 10(-2) nm2. The reliability index (R) amounts to 1.71% for germanium.

Electrochemical preparation of few layer-graphene nanosheets via reduction of oriented exfoliated graphene oxide thin films in acetamide-urea-ammonium nitrate melt under ambient conditions

Electrochemical reduction of exfoliated graphene oxide, prepared from pre-exfoliated graphite, in acetamide-urea-ammonium nitrate ternary eutectic melt results in few layer-graphene thin films. Negatively charged exfoliated graphene oxide is attached to positively charged cystamine monolyer self-assembled on a gold surface. Electrochemical reduction of the oriented graphene oxide film is carried out in a room temperature, ternary molten electrolyte. The reduced film is characterized by atomic force microscopy (AFM), conductive AFM, Fourier-transform infrared spectroscopy and Raman spectroscopy. Ternary eutectic melt is found to be a suitable medium for the regulated reduction of graphene oxide to reduced graphene oxide-based sheets on conducting surfaces. (C) 2010 Elsevier B.V. All rights reserved.

A study of the reaction of divalent transition metal chlorides with pyridinium poly(hydrogen fluoride), ppht, and the effect of potassium hydrogen fluoride on fluorination and complexation

Studies of the reaction of metal chlorides, MCl2 (M = Mn, Co, Ni, Cu, Zn) with PPHF at room temperature have shown that Mn, Co and Zn form the corresponding metal fluorides, MF2, while Ni and Cu form their dipyridine metal(II) dichloride complexes. Nickel and copper complexes further undergo fluorination and complexation by potassium hydrogen fluoride in PPHF to form KNiF3 and KCuF3.

Varistors based on n-BaTiO3 ceramics

Stable and highly reproducible voltage-limiting characteristics have been observed at room temperature for polycrystalline ceramics prepared from donor-doped BaTiO3 solid solutions containing isovalent lattice substitute ions that lower the Curie point Tc. When the ambient temperature Ta is decreased such that Ta < Tc, the same ceramics show current-limiting behaviour. The leakage current, the breakdown voltage and the non-linear coefficient (α = 30−50) could be varied with grain-boundary layer (GBL) modifiers and postsintering annealing. The magnitude of the abnormally high dielectric constant (epsilon (Porson)r greater than, approximately 105) indicates the prevalence of GBL capacitance in these ceramics. Analyses of the current-voltage relations show that GBL conduction at Ta < Tc corresponds to tunnelling across asymmetric barriers formed under steady state Joule heating. At Ta > Tc, trap-related conduction gives way to tunnelling across symmetric barriers as the field strength increases.

Optical absorption and photoluminescence studies of Nd3 doped alkali boro germanate glasses

Optical absorption and photoluminescence studies have been carried out at room temperature in 25 R2O-25 GeO2-49.5 B2O3-0.5 Nd2O3 glass systems, (Composition in mol%, R= Li, Na, K and Rb). Judd Ofelt Intensity parameters and other parameters like Racah (E-1, E-2 and E-3), Slater-Condon-Shortley (F-2, F-4 and F-6) Spin-Orbit Coupling (xi(4f)) and Configuration Interaction (alpha,beta and gamma) for Nd3+ ion in the glass system are calculated. The variation of the 02 parameters are interpreted in terms of the covalency of the RE ion in the glass matrix. Further the hypersensitive transition I-4(9/2) -> (4)G(5/2), (2)G(7/2) is analyzed with respect to the intensity ratio I-L/I-S and is found to be dependent on the type of alkali in the glass matrix. The Photoluminescence studies do not show any appreciable shift in the peak emission wavelength of the F-4(3/2) to I-4(11/2) transition with the change in alkali type. (C) 2010 Elsevier B.V. All rights reserved.

Evolution of Transformation Texture in a Metastable B - Titanium Alloy

Texture evolution in h. c. p. (alpha) phase derived from aging of a differently processed metastable b.c.c. (beta) titanium alloy was investigated. The study was aimed at examining (i) the effect of different b. c. c. cold rolling textures and (ii) the effect of different defect structures on the h. c. p transformation texture. The alloy metastable beta alloy Ti-10V-4.5Fe-1.5Al was rolled at room temperature by unidirectional (UDR) and multi-step cross rolling (MSCR). A piece of the as-rolled materials were subjected to aging in order to derive the h. c. p. (alpha) phase. In the other route, the as-rolled materials were recrystallized and then aged. Textures were measured using X-ray as well as Electron Back Scatter Diffraction. Rolling texture of beta phase, as characterized by the presence of a strong gamma fibre, was found stronger in M S C R compared to UDR, although they were qualitatively similar. The stronger texture of MSCR sample could be attributed to the inhomogeneous deformation taking place in the sample that might contribute to weakening of texture. Upon recrystallization in beta phase field close to beta-transus. the textures qualitatively resembled the corresponding beta deformation textures; however, they got strengthed. The aging of differently beta rolled samples resulted in the product alpha-phase with different textures. The (UDR + Aged) sample had a stronger texture than (MSCR + Aged) sample, which could be due to continuation of defect accumulation in UDR sample, thus providing more potential sites for the nucleation of alpha phase. The trend was reversed in samples recrystallized prior to aging. The (MSCR + Recrystallized + Aged) sample showed stronger texture of alpha phase than the (UDR + Recrystallized + Aged) sample. This could be attributed to extensive defect annihilation in the UDR sample on recrystallization prior to aging. The (MSCR + Aged) sample exhibited more alpha variants when compared to (MSCR + Recrystallized + Aged) sample. This has been attributed to the availability of more potential sites for nucleation of alpha phase in the former. It could be concluded that alpha transformation texture depends mainly on the defect structure of the parent phase.

Linear electro‐optic dispersion in (‐)‐2‐(α‐methylbenzylamino)‐5‐nitropyridine single crystals

The variation of the linear electro-optic effect in (-)-2-(alpha-methylbenzylamino)-5-nitropyridine with the wavelength of the incident light at room temperature has been measured. The reduced half-wave voltages have been found to have the values 2.1, 2.8, and 6.0 kV at 488, 514.5, and 632.8 nm respectively and the corresponding values of the linear electro-optic coefficient have been evaluated.;The interpretation of the results in terms of the structures of the molecule and the crystal is discussed. The thermal variation of the birefringence has also been investigated and the coefficient for the temperature variation of the refractive index difference is found to have the value (d Delta n/dT)=9.3X10(-5) K-1.

Role of lattice defects and crystallite morphology in the UV and visible-light-induced photo-catalytic properties of combustion-prepared TiO2

The physico-chemical, photo-physical and micro-structural properties responsible for the strikingly different photocatalytic behavior of combustion-prepared TiO2 (c.TiO2) and Degussa P25 (d.TiO2) samples are elucidated in this study. Electron microscopy and selected area electron diffraction micrographs revealed that the two samples exhibited different morphologies. The grains of c.TiO2 were spherical and comprised of 5-6 nm size primary particle. On the other hand, d.TiO2 consisted of large (0.5-3.0 mu m) size and irregular shape aggregates having primary particles of 15-40 nm cross-sectional diameter. The ESR study revealed that the presence of certain defect states in c.TiO2 helped in stabilization of O-. and Ti3+-OH type species during room-temperature UV-irradiation. No such paramagnetic species were however formed over d.TiO2 under similar conditions. C1s and Ti 2p XPS spectra provide evidence for the presence of some lattice vacancies in c.TiO2 and also for the bulk Ti4+ -> Ti3+ conversion during its UV-irradiation. Compared to d.TiO2, c.TiO2 displayed considerably higher activity for discoloration of methyl orange but very poor activity for splitting of water, both under UV and visible light radiations. This is attributed to enhanced surface adsorption of dye molecules over c.TiO2, because of its textural features and also the presence of photo-active ion-radicals. On the other hand, the poor activity of c.TiO2 for water splitting is related to certain defect-induced inter-band charge trapping states in the close vicinity of valence and conduction bands of c.TiO2, as revealed by thermoluminescence spectroscopy. Further, the dispersion of nanosize gold particles gave rise to augmented activity of both the catalysts, particularly for water splitting. This is explained by the promotional role of Au-0 or Au-0/TiO2 interfacial sites in the adsorption and charge-adsorbate interaction processes. (C) 2011 Elsevier B.V. All rights reserved.

Studies on pyridinium hexafluorostannate and its derivatives

Pyridinium hexafluorostannate, (C5H5NH)2SnF6, has been prepared by the reaction of stannous chloride or tin metal with pyridinium poly(hydrogen fluoride), PPHF, and identified by chemical analysis, IR and NMR (H-1, F-19, C-13). Making use of (C5H5NH)2SnF6 as a precursor, the following important hexafluorostannate salts have been synthesized in high yields at room temperature by ionic exchange: M2SnF6 (M = NH4, Na, K, Rb, Cs) and BaSnF6. These salts have been characterised by chemical analysis and infrared spectroscopy. Indexed powder X-ray diffraction data for Na2SnF6, Rb2SnF6 and Cs2SnF6 have been reported.

Syntheses and studies on pyridinium pxofluorocomplexes of molybdenum, tungsten andiodine

(C5H5NH)2MO2F4 (M = Mo and W) and C5H5NHIO2F2 have been synthesized at room temperature by the reaction of molybdic, tungstic or iodic acid, respectively, with pyridinium poly(hydrogen fluoride). These complexes have been characterized by chemical analyses, H-1 nmr and infrared spectroscopy.

Solvothermal synthesis of Hg1-xCdxTe nanostructures-Their structural and optical properties

This article describes a facile, low-cost, solution-phase approach to the large-scale preparation of Hg1-xCdxTe nanostructures of different shapes such as nanorods, quantum dots, hexagonal cubes of different sizes and different compositions at a growth temperature of 180 degrees C using an air stable Te source by solvothermal technique. The XRD spectrum shows that the crystals are cubic in their basic structure and reveals the variation in lattice constant as a function of composition. The size and morphology of the products were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The formation of irregular shaped particles and few nano-rods in the present synthesis is attributed to the cetyl trimethylammonium bromide (CTAB). The room temperature FTIR absorption and PL studies for a compositon of x = 0.8 gives a band gap of 1.1 eV and a broad emission in NIR region (0.5-0.9 eV) with all bands attributed to surface defects.

Lanthanide Sulfate Frameworks: Synthesis, Structure, and Optical Properties

Layered lanthanide sulfate compounds with three different structures have been prepared and characterized. The compounds C10H10N2] La(SO4)(2)]center dot 2H(2)O (I), C10H10N2] La(SO4)(2)(H2O)(2)](2) (Ha), C10H10N2]Pr(SO4)(2)(H2O)(2)](2) (IIb), C10H10N2]Nd-2(SO4)(4)(H2O)(2)](2) (IIIa), C10H10N2]Sm-2(SO4)(4)(H2O)(2)](2) (IIIb), and C10H10N2]Eu-2(SO4)(4)(H2O)(2)] 2 (IIIC) have anionic lanthanide sulfate layers separated by protonated bipyridine molecules. The layers are formed by the connectivity between the lanthanide polyhedra and sulfate tetrahedra. The formation of a two-dimensional La-O-La layer (la), Pr-O-Pr chains (IIb), and a tetramer cluster (IIIa) is noteworthy. The compounds exhibit honeycomb (I), square (IIa, IIb), and honeycomb (IIIa-IIIc) net arrangements, when the connectivity between the lanthanide ions is considered. Optical studies indicate the observation of characteristic metal-centered emission at room temperature. The Nd compound (IIIa) exhibits a two-photon upconversion behavior.

Wet chemical syntheses of ultrafine multicomponent ceramic powders through gel to crystallite conversion

Coarse (BOn/2)-O-n+/xH(2)O (10

Chemical Degradation of Poly(styrene disulfide) and Poly(styrene tetrasulfide) by Triphenylphosphine

The chemical degradation of polysulfide polymers, viz., poly(styrene disulfide), PSD, and poly(styrene tetrasulfide), PST, has been achieved using triphenylphosphine, TPP. The reaction was monitored using P-31 NMR spectroscopy. The solubility analysis of the reaction residues reveals that while PSD degrades completely, PST on the other hand, undergoes complete degradation only when the concentration of TPP is increased. Moreover, the reaction of PST with TPP occurs at room temperature whereas PSD requires a higher temperature. The reaction products were analyzed using the direct pyrolysis mass spectrometric (DP-MS) technique, and their formation has been explained through an ionic mechanism.

H-1 MAS NMR study of protonic conduction in layered HNbWO6 center dot xH(2)O (x=1.5, 0.5)

H-1 Magic Angle Spinning (MAS) NMR of layered HNbWO6 . xH(2)O (x = 1.5, 0.5) is carried out at room temperature and at various spinning speeds (1-12 kHz). Results on the fully hydrated sample (x = 1.5) are consistent with the model of diffusion of H3O+ ions within the layers. In the partially dehydrated sample (x = 0.5) an exchange between the distinctly present cage protons and H3O+ protons leads to protonic conduction.