Synthesis,structural, thermal and optical properties of TeO2–Bi2O3–GeO2–Li2O glasses

In this study, synthesis and characterization of novel quaternary tellurite glass system TeO₂–Bi₂O₃–GeO₂–Li₂O is presented. The compositions include TeO₂ and GeO₂ as glass formers while different proportion of Bi₂O₃ and Li₂O act as network modifiers. Differential thermal analysis, X-ray diffraction, scanning electron microscopy energy dispersive X-ray spectroscopy, laser ablation inductively coupled plasma mass spectrometry, UV–Vis and Raman spectroscopy are applied to study the structural, thermal and optical properties of the studied glasses. Obtained glasses possess a relatively low glass transition temperature (around 300 °C) if compared to other tellurite glasses, show good thermal transparency in the visible and near infra-red (from 2.4 to 0.4 μm) and can double the frequency of laser light from its original wavelength of 1064 nm to its second-harmonic at 532 nm (i.e. second harmonic generation).     

Sintering and crystallization of off-stoichiometric BaO·Al2O3·2SiO2 glasses

Glass-ceramics with off-stoichiometric celsian composition of 50 wt% BaO·2SiO₂ – 50 wt% BaO·Al₂O₃·2SiO₂, (B2S-BA2S) were fabricated and investigated for their sintering and crystallization characteristics. (B2S-BA2S) glass powder showed a melting temperature much lowered compared to that of stoichiometric BaO·Al₂O₃·2SiO₂ (BA2S) glass powder and high sintering ability. (B2S-BA2S) glass powder containing B₂O₃, (B2S-BA2S)B and that containing B₂O₃ and TiO₂, (B2S-BA2S)BT revealed much lowered crystallization peak temperatures, but rather low sintered density. By applying Kissiger analysis to differential thermal analysis (DTA) data activation energy values for crystallization were determined as 265, 195 and 242 kJ/mol, respectively for (B2S-BA2S), (B2S-BA2S)B and (B2S-BA2S)BT glasses. X-ray diffraction (XRD) patterns from all the glass-ceramics crystallized at 1100°C for 4 h revealed formation of crystalline phases of -BaO·2SiO₂, monocelsian and hexacelsian. (B2S-BA2S) glass-ceramics crystallized at 1400°C for 4 h showed formation of -BaO·2SiO₂ and monocelsian phases with only trace of metastable hexacelsian phase.     

Sintering and crystallization of off-stoichiometric SrO·Al2O3·2SiO2 glasses

Glass-ceramics with the celsian-corundum binary join composition of 88.8 wt% SrO·Al₂O₃·2SiO₂ – 11.2 wt% Al₂O₃, (SA2S-A), were fabricated by pressureless sintering and investigated for their sintering and crystallization behaviors. The (SA2S-A) glass powder showed crystallization peak and melting temperatures of 1059 and 1550 °C, respectively and high sintering ability. The (SA2S-A) glass powders containing B₂O₃, (SA2S-A)B and those containing B₂O₃ and TiO₂, (SA2S-A)BT showed lowered crystallization peak temperatures of 1033 and 997 °C, respectively. By applying Kissiger analyses to the DTA data of the (SA2S-A), (SA2S-A)B and (SA2S-A)BT glass powders, the activation energy values for crystallization were determined as 488, 370 and 333 kJ/mol, respectively. The Ozawa analyses on the DTA data gave the Avrami parameter values at 1.2, 1.1 and 1.9, respectively for the (SA2S-A), (SA2S-A)B and (SA2S-A)BT glass powders. The x-ray diffraction (XRD) patterns of the (SA2S-A) glass-ceramics, crystallized at 1100 °C for 4 h, showed formation of both the monocelsian and hexacelsian phases. The (SA2S-A)B and (SA2S-A)BT glass-ceramics crystallized at 1100 °C for 1 h, showed formation of the phase-pure monocelsian and did not show any evidence of the hexacelsian formation prior to the monocelsian formation.     

Effect of Bi2O3 on structural and optical properties of Li2O·PbO·Bi2O3·B2O3 glasses

Journal of Materials Science: Materials in Electronics - The quaternary glass system has a composition of 30Li2O·20PbO·xBi2O3·(50-x)B2O3 (where x?=?0, 10, 20, 30, and...     

Structural and physical characterization of the Li2O∶P2O5∶CrO1.5 ion-conducting glasses

Li₂OP₂O₅CrO_1.5 glasses containing 40, 50 and 60 mol% Li₂O and a varying P₂O₅-to-CrO_1.5 ratio have been synthesized. The glass-transition temperature and density increase as P₂O₅ is progressively replaced by CrO_1.5. The glasses, being green in colour and showing strong optical absorption at 450 nm and 660 nm, contain predominantly Cr^{3 +} ions and a relatively small amount of Cr^{6 +} ions. The proportions of phosphate species with one, two, and three non-bridging oxygen atoms are determined from Raman spectroscopy results. From X-ray photoelectron spectroscopy (XPS) binding energies of the Li 1s, P 2p, Cr 2p and O 1s core levels are determined. The O 1s spectrum is found to consist of two peaks which are attributed to the P=O, P-O-P, P-O, P-O-Cr, and Cr-O oxygen species. Conductivity of these glasses increases with increasing Li₂O content and with progressive replacement of P₂O₅ by CrO_1.5. The 0.60Li₂O O.32P₂O₅0.08 CrO_1.5 glass is found to have the highest conductivity, 3.2×10^–6–1 cm^–1 at 25 °C. Compositional dependence of the conductivity is discussed in relation to variations in the glass structure.     

Synthesis and characterization of barium borosilicate glass–Al2O3 composites

Barium borosilicate glass with composition 30BaO–60B₂O₃–10SiO₂ glass was prepared by melt-quenching technique. Different weight % of crystalline Al₂O₃ was mixed with the glass powder and sintered at optimum temperature. The changes in the structure and thermal properties of the glass with alumina content were investigated by X-ray powder diffraction, FT-IR spectroscopy and differential thermal analysis. The variations in the coefficient of thermal expansion and dielectric properties with composition were also studied and correlated with the structural changes.     

D.c. conductivity of V2O5–MnO–TeO2 glasses

Semiconductive oxide glasses in the system V2O5–MnO–TeO2 were prepared, and the mechanism of d.c. conduction was studied. The Seebeck coefficient measurements at temperatures from 375–475 K indicated the glasses to be n-type semiconducting. The d.c. conductivity ranged from 5×10–5 to 1.9×10–6 S cm–1 at 405 K for V2O5=60 mol% and MnO=0–20 mol%, and decreased with increasing MnO content. The conduction was confirmed to obey the adiabatic small polaron hopping model, and was due to mainly hopping between V-ions in the glasses. The polaron band width J was estimated to be J=0.10–0.20 eV. The electron–phonon interaction coefficient p was very large (21–26). The hopping mobility evaluated as 2.3×10–7–2.7×10–6 cm2 V–1 s–1 increased with increasing V2O5 content. The estimated carrier concentration was the order of 1019 cm–3. The principal factor determining conductivity was the polaron hopping mobility in these glasses. © 1998 Chapman & Hall     

Structural verification and optical characterization of SiO2–Au–Cu2O nanoparticles

In this paper, SiO₂–Au–Cu₂O core/shell/shell nanoparticles were synthesized by reducing gold chloride on 3-amino-propyl-triethoxysilane molecules attached silica nanoparticle cores for several stages. Cu₂O nanoparticles were synthesized readily with the size of 4–5 nm using a simple route of sol–gel method Then, they were clung to the surface of Au seeds. The morphology of the resultant particles was studied using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Transmission electron microscopy images demonstrate growth of monodispersed gold seeds and Cu₂O nanoparticles in narrow size up to 10 nm and 5 nm, respectively. The presence of gold and Cu₂O coating was confirmed by X-ray diffraction, Fourier transform infrared spectroscopy and UV–Vis spectroscopy. Absorption spectroscopy shows considerably 40 nm blue shift in absorption edge for SiO₂–Au–Cu₂O nanostructure rather than SiO₂–Au core/shell nanoparticles.     

Synthesis and characterization of γ-Bi2O3 based solid electrolyte doped with Nb2O5

γ-phase bismuth oxide is a well known high oxygen ion conductor and can be used as an electrolyte for intermediate temperature solid oxide fuel cells (IT-SOFCs). This study aims to determine new phases of Bi₂O₃-Nb₂O₅ binary system and the temperature dependence of the electrical transport properties. The reaction products obtained in open air atmosphere were characterized by X-ray powder diffractions (XRD). The unit cell parameters were defined from the indexes of the powder diffraction patterns. The γ-Bi₂O₃ crystal system were obtained by doping 0.01 < mole% Nb₂O₅ < 0.04 at 750 °C for 48 and 96 h. Thermal behaviour and thermal stability of the phases were investigated by thermal analysis techniques. Surface and grain properties of the related phases were determined by SEM analysis. The temperature dependence of the electrical properties of γ-Bi₂O₃ solid solution was measured by four-point probe d.c. conductivity method. In the investigated system, the highest value of conductivity was observed for σ _T = 0.016 ohm^?1 cm^?1 at 650 °C on 4 mole% Nb₂O₅ addition. The electrical conductivity curves of studied materials revealed regular increase with temperature in the form of the Arrhenius type conductivity behaviour.     

Small polaron transport in V2O5–NiO–TeO2 glasses

Semiconducting glasses of the V₂O₅–NiO–TeO₂ system were prepared by the press-quenching method and their d.c. conductivities in the temperature range 300–450 K were measured. The d.c. conductivities at 395 K for the present glasses were determined to be 10^–7 to 10^–1 S m^–1, indicating that the conductivity increased with increasing V₂O₅ concentration. A glass of composition 67.5V₂O₅–2.5NiO–30TeO₂ (mol %) having a conductivity of 2.47×10^–2 S m^–1 at a temperature of 395 K was found to be the most conductive glass among the vanadium-tellurite glasses. From the conductivity–temperature relation, it was found that a small polaron hopping model was applicable at the temperature above _D/2 (_D: the Debye temperature); the electrical conduction at T>_D/2 was due to adiabatic small polaron hopping of electrons between vanadium ions. The polaron bandwidth ranged from 0.06 to 0.21 eV. The hopping carrier mobility varied from 1.1×10^–7 to 5.48×10^–5 cm² V^–1 s^–1 at 400 K. The carrier density is evaluated to be 1.85×10¹⁹–5.50×10¹⁹ cm^–3. The conductivity of the present glasses was primarily determined by hopping carrier mobility. In the low-temperature (below _D/2) regime, however, both Mott's variable-range hopping and Greaves intermediate range hopping models are found to be applicable.     

Nanocrystallization as a method of improvement of electrical properties of Fe2O3–PbO2–TeO2 glasses

Selected glasses of Fe₂O₃–PbO₂–TeO₂ system have been transformed into nanomaterials by annealing at a temperature close to the crystallization temperature (T_c). The effects of the annealing of the present samples on the structural and electrical properties were studied by transmission electron micrograph (TEM), X-ray diffraction (XRD), differential scanning calorimeter, density (d) and dc conductivity (σ). TEM and XRD of glass–ceramic naocrystals indicated nanocrystals embedded in the glassy matrix with average particle size of 20–35 nm. The glass–ceramic naocrystals obtained by annealing at T_c exhibit improvement of electrical conductivity up to four orders of magnitude than the starting glasses. This considerable improvement of electrical conductivity after nanocrystallization is attributed to formation of extensive and dense network of electronic conduction paths which are situated between Fe₂O₃ nanocrystals and on their surface. The conduction is attributed to non-adiabatic hopping of small polaron.     

Synthesis and characterization of SiO2–La2O3 gels obtained in a water-free environment

SiO₂–La₂O₃ binary oxide system was prepared by the sol–gel method without addition of strong polar solvents (e.g. water, alcohol) to the initial system. Changes in the surface and gel network structure were described as a function of the type and concentration of the second component that is lanthanum oxide. A series of samples with Si to La molar ratios of 1:0.1, 1:0.25, 1:0.5, and 1:1 were characterised by XRD, TG–TA, FTIR, and low-temperature nitrogen adsorption measurements. Results of the investigation showed that higher amounts of the lanthanum component in the binary oxide gel system led to a completely changed morphology of the porous structure of the surface gels obtained in a non-aqueous medium.     

Synthesis and characterization of γ-zirconium arsenate

The hydrothermal synthesis of a novel layered zirconium arsenate, Zr( AsO₄) (H₂AsO₄) · 2H₂O, with γ-type structure and preliminary data on its characterization by chemical and thermal analysis, X-ray diffraction (XRD) and ion exchange are reported. This XRD powder pattern is indexed on a monoclinic cell: a = 5.5699(2) Å, b = 6.8175(4) Å, c= 12.1203(6) Å and β= 103.15(1)°.     

The role of fluorine in the devitrification of SiO2·Al2O3·P2O5·CaO·CaF2 glasses

A series of eight glasses based on a glass system with the generic composition 1.5(5–Z)SiO₂·(5–Z) Al₂O₃·1.5P₂O₅·(5–Z)CaO·ZCaF₂ were studied where Z = 2, 1.75, 1.5, 1.25, 1, 0.5, 0.25, 0. These glasses were characterised using differential scanning calorimetry (DSC) and x-ray powder diffraction (XRD). Glasses with high fluorine contents were found to crystallise readily to fluorapatite via a homogeneous nucleation route probably involving prior amorphous phase separation. These results are explained in terms of an approach which views glasses as being inorganic polymers where the presence of fluorine disrupts the glass network and thereby reduces the energy barrier to homogeneous nucleation and crystallisation of fluorapatite.     

Synthesis,characterization and crystal structure of a novel Strandberg-type polyoxoselenomolybdate Rb4[Se2Mo5O21]·2H2O

An inorganic compound formulated as Rb₄[Se₂Mo₅O₂₁]·2H₂O (1) has been isolated by conventional solution method and structurally characterized by single-crystal X-ray diffraction methods, scanning electron microscopy (SEM), powder XRD, IR, UV–vis spectra, and cyclic voltammetry measurements. This compound crystallizes in the monoclinic system, space group C2 with unit a = 19.701 (3) Å, b = 10.296 (2) Å, c = 12.134 (4) Å, β = 106.96 (2)° and Z = 4. The crystal structure of (1) is built up from a Strandberg clusters connected through hydrogen-bonding interactions into a three-dimensional supramolecular network.     

Synthesis and characterization of nanosize CoxNi1−xFe2O4 powders by glycothermal process

Nanosized Co_xNi_1−xFe₂O₄ powders were prepared in ethylene glycol solution under mild temperature and pressure conditions by precipitation from metal nitrates. The average size and distribution of the synthesized Co_xNi_1−xFe₂O₄ powders was about 15 nm and narrow, respectively. The magnetic property of the synthesized Co_xNi_1−xFe₂O₄ powder was about 60 (emu/g) with superparamagnetic character at room temperature.     

Synthesis and Study of Sr[HSiUO6]2·2H2O and Ba[HSiUO6]2·2H2O

Uranosilicates of the general formula M^{I I}[HSiUO₆]₂·2H₂O (M^{I I} = Sr, Ba) were prepared by hydrothermal synthesis. Previously unknown intermediate crystal hydrates were separated and studied by X-ray diffraction (XRD), IR spectroscopy, and thermal analysis. Polymorphic transitions -Sr[HSiUO₆]₂ -Sr[HSiUO₆]₂ and -Ba[HSiUO₆]₂ -Ba[HSiUO₆]₂ were revealed at 700 and 780°C, respectively.