Fabrication of transparent silica glass by powder sintering

Transparent silica glasses were obtained by sintering a green compact (fabricated by slip-casting methods for high-purity silica glass powder) in diverse atmospheres. The relationships between sintering atmosphere and sintering temperature that result in transparent, sintered silica glass were shown. The results indicate that there are four forming phases for each sintering atmosphere and temperature: (1) nontransparent glass resulting from an overabundance of pores (2) crystal, such as cristobalite or β-quartz, (3) moganite, and (4) transparent glass. Optimum sintering temperature for fabricating transparent silica glass was above 1673 K in a high-vacuum (10^–4 Pa: p(O₂) = 10^–14) atmosphere. We investigate the fabrication of transparent and hydroxyl-free silica glass by a powder-sintered method. After studying the effect of sintering schedule on residual [OH^–] concentration for transparent, sintered silica glasses, we sintered a green compact prepared by silica powders with a mean particle size of 1.6 µm, first heating it to 1523 K for dehydration and then to 1873 K for densification. This typical fabricated condition resulted in a transparent, sintered silica glass with <1 ppm [OH^–] concentration.     

Influence of sintering atmosphere on the microstructure and water durability of SnO–MgO–P<Subscript>2</Subscript>O<Subscript>5</Subscript> glass

Effects of sintering atmosphere (Ar, air, and O₂) on the sinterability and crystallization at 380–470 °C of 60SnO, 10MgO, 30P₂O₅ (mol%) glass powder, and the water durability of the sintered glass were investigated. Increasing the oxygen partial pressure (P_\textO2 ) (P_{{{\text{O}}_{2} }} ) in the sintering atmosphere enhanced the oxidation tendency of Sn²⁺ to Sn⁴⁺ near the surface region of the glass particles. Therefore, the glass viscosity was increased, resulting in the increase in both the temperature of densification and the temperature at which crystalline phases developed. Phase assemblage and the amounts of crystalline phases were also affected by P_\textO2 . P_{{{\text{O}}_{2} }} . The water durability of the sintered glasses is discussed in terms of the above microstructural parameters.     

Microwave dielectric and elastic properties of glass-added Ba6−3xR8+2xTi18O54 (x = 2/3)

Microwave dielectric properties of Ba_6−3xSm_8+2xTi₁₈O₅₄ (x = 2/3) [BST] ceramics with the addition of 0–3 wt.% of various glasses have been studied. It has been found that the addition of 0.5 wt.% of the glasses decreases the sintering temperature by about 150 °C. In general, addition of 0.5 wt.% of Zn, Mg and Pb-based glasses deteriorate the quality factor, whereas aluminum and barium borosilicates do not decrease it considerably. The quality factor and dielectric constant decrease with increasing amount of glass. The temperature coefficient of resonant frequency shifts towards positive or negative depending on the composition of the glass. A glass–ceramic composite with a dielectric constant 64, Q × f nearly 8500 GHz and near to zero τ_f could be obtained at a sintering temperature of 1175 °C when 3–4 wt.% Al₂O₃–B₂O₃–SiO₂ glass was added to BST ceramic. The Young's modulus decreases with increasing amount of glass, irrespective of the composition of glass.     

Optimization of chalcogenide glass in the As–Se–S system for automotive applications

Infrared transmitting glasses in the As–Se–S system have been optimized by taking in account specifications for automotive application. The As₂Se₃ glass has been chosen as the starting composition and sulfur is introduced in order to improve some optical and mechanical properties. As expected, the Sulfur introduction decreases the refractive index as well as its change as function of temperature. The relationship between the refractive index and the glass composition has been established. The thermal coefficient of refractive index for sulfur containing glasses can be lower than 4 × 10⁻⁵ K⁻¹, which is considerably lower than that of germanium, the most used infrared transmitting materials. Influence of sulfur on other properties has also been studied.     

Sintering, crystallization, and properties of a low-viscosity SnO–MgO–P2O5 glass

A lead-free, low-viscosity SnO–MgO–P₂O₅ glass powder was fabricated. Sinterability, wetting, flowability, crystallization, and the resulting properties of the glass powder were investigated. It is shown that the powder compact can be fully densified above 362 °C and show good wet to the substrate above 417 °C. The properties (coefficient of thermal expansion and chemical durability) of the sintered glass depend on the sintering temperature and are discussed in terms of the development of crystalline phases during sintering.     

Surface and grain-boundary energies as well as surface mass transport in polycrystalline CeO2

The multiphase equilibration technique for the determination of the equilibrium angles that develop at the interphase boundaries of a solid–liquid–vapor system, has been used to calculate the surface and interfacial energies in polycrystalline CeO₂ and CeO₂/Cu system in argon atmosphere at the temperature range 1473–1773 K. Linear temperature functions were obtained by extrapolation, for the surface energy γ_sv (J/m²) = 2.465–0.563 × 10⁻³ T and the grain-boundary energy γ_ss (J/m²) = 1.687–0.391 × 10⁻³ T of the ceramic, as well as for the interfacial energy γ_sl (J/m²) = 2.623–1.389 × 10⁻³(T −1356 K) of the CeO₂/Cu system. Grain-boundary grooving studied on polished surfaces of CeO₂ annealed in argon atmosphere at the same temperature range has shown that surface diffusion was the dominant mechanism for the mass transport. The surface diffusion coefficient can be expressed according to the equation D_s (m²/s) = 3.82 × 10⁻⁴ exp(−308,250/RT).     

Structural, dielectric, impedance and optical properties of CaBi2B2O7 glasses and glass-nanocrystal composites

Optically clear glasses were fabricated by quenching the melt of CaCO₃–Bi₂O₃–B₂O₃ (in equimolecular ratio). The amorphous and glassy characteristics of the as-quenched samples were confirmed via the X-ray powder diffraction (XRD) and differential scanning calorimetric (DSC) studies. These glasses were found to have high thermal stability parameter (S). The optical transmission studies carried out in the 200–2500 nm wavelength range confirmed both the as-quenched and heat-treated samples to be transparent between 400 nm and 2500 nm. The glass-plates that were heat-treated just above the glass transition temperature (723 K) for 6 h retained ≈60% transparency despite having nano-crystallites (≈50–100 nm) of CaBi₂B₂O₇ (CBBO) as confirmed by both the XRD and transmission electron microscopy (TEM) studies. The dielectric properties and impedance characteristics of the as-quenched and heat-treated (723 K/6 h) samples were studied as a function of frequency at different temperatures. Cole–Cole equation was employed to rationalize the impedance data.     

Microwave synthesis and properties of NaPO3–SnO–Nb2O5 glasses

Tin niobiophosphate glasses were produced using a domestic microwave oven under a nitrogen flow. The fast microwave melting method and the protective atmosphere prevent the oxidation of SnO. After 10 min of heating, the NaPO₃, SnO, and Nb₂O₅ mixtures are homogeneous and permit to obtain transparent glasses. Three series of glasses with different Sn/Nb ratio were studied to determine the influence of each oxide. The glass transition temperature increases linearly with the amount of Nb₂O₅ and SnO. These variations are more important for compositions with high metallic cation proportions and with a low Sn/Nb ratio. The same evolutions were observed for the density, Vickers hardness, and elastic modulus while the thermal expansion coefficient decreases monotonously. The simultaneous insertion of SnO and Nb₂O₅ in phosphate glass matrix leads to a progressive strengthening of the glass network. The chemical durability of the glasses also increases as a function of the amount of metal oxides. We prepared a bulk glass sample with a dissolution rate of about 3.3 × 10⁻⁸ g cm⁻² min⁻¹ in renewed water conditions at 95 °C. This durability is equivalent to those of the window glass whereas the glass transition temperature remains lower than 485 °C.     

Comparison of sintering behavior and piezoelectric properties of (K,Na)NbO3-based ceramics sintered in conventional and microwave furnace

In this study (1 − x) K_0.48Na_0.48Li_0.04Nb_0.96Ta_0.04O₃ − xSrTiO₃ (0.0 ≤ x ≤ 0.10) ceramics were fabricated by sintering in microwave furnace for first time as well as in conventional furnace (either via single step or two-step procedures). Sintering behavior and piezoelectric properties of sintered samples were studied and compared. It was found that two-step sintering decreases sintering temperature effectively and enhances densification compared to single step sintering. Microstructure analysis revealed that, two-step sintering suppresses grain growth and promotes densification. On the other hand, microwave sintering enhanced densification more effectively and reduced sintering time and temperature. The maximum piezoelectric constants of ceramics were measured for those sintered in microwave furnace. Piezoelectric constant of the sample containing 1 mol% SrTiO₃ which was sintered in microwave furnace was measured 310 pC N⁻¹ while by sintering in conventional furnace via single and two-step sintering it was obtained 208 and 278 pC N⁻¹, respectively.     

The effect of glass addition on the dielectric properties of barium strontium titanate

Ba_0.7Sr_0.3TiO₃ (BST) ceramics were prepared by the conventional solid state ceramic route. Different weight percentages of twelve different glasses were added to the calcined BST ceramics and sintered. The structure and microstructure of the sintered materials were investigated by X-ray diffraction and Scanning Electron Microscopic techniques. The low frequency dielectric properties of the glass-ceramic composites were measured using LCR meter. Some of the glasses improved the dielectric properties and considerably lowered the sintering temperature. The glasses were prepared and characterized under identical conditions. Among the different glasses, 1.5 wt% addition of 71ZnO–29B₂O₃ lowered the sintering temperature of BST to 975 °C with a dielectric loss of 9 × 10⁻³ and dielectric constant of 875 at 1 MHz. The curie temperature of BST ceramics was found to shift towards lower temperature with glass addition.     

Sintering studies on submicrometre-sized Y-Ba-Cu-oxide powder

The isothermal sintering behaviour of submicrometre-sized (<50 nm) powders of single-phase YBa₂Cu₃O _x (123) and unreacted stoichiometric mixture of submicrometre-sized (<50 nm) powders of BaCO₃, Y₂O₃ and CuO (which on calcination at 1173 K gives YBa₂Cu₃O _x ) was investigated through dilatometry under different sintering atmospheres. The sintering rate of the powder compacts was impeded by the presence of oxygen. The activation energies,Q, of sintering were determined to be 1218 kJ mol^–1 in argon, 1593 kJ mor^–1 in air and 2142 kJ mol^–1 in oxygen. A decrease in the apparent sintered density with increasing oxygen partial pressure was also observed. X-ray diffraction and thermal analyses (thermogravimetry and differential thermal analysis) showed no reaction during sintering of the single-phase product. Pellets fabricated from uncalcined powder exhibit two stages of sintering, one between 1073 and 1173 K having an activation energyQ=627kJ mol^–1, and a second one above 1173 K withQ=383.7 kJ mol^–1. A.c. susceptibility, resistivity and critical current density were determined as a function of the temperature of the sintered samples.     

Biosensor enhanced by glucose oxidase biomimetic membrane containing the platinum and silica nanoparticles

In this paper, glucose biosensor is fabricated with immobilization of glucose oxidase (GOx) in platinum and silica sol. The glucose biosensor combined with Pt and SiO₂ nanoparticles could make full use of the properties of nanoparticles. A set of experimental results indicates that the current response for the enzyme electrode containing platinum and silica nanoparticles increases from 0.32 µA cm^− 2 to 33 µA cm^− 2 in the solution of 10 mM β-D-glucose. The linear range is 3 × 10^− 5 to 3.8 × 10^− 3 M with a detection limit of 2 × 10^− 5 M at 3σ. The effects of the various volume ratios of Pt and SiO₂ sols with respect to the current response and the stability of the enzyme electrodes are studied.     

Dielectric Properties of Vitreous Silica with Various Hydroxyl Concentrations

We investigated the temperature dependence of the dielectric susceptibility of amorphous silica below 300 mK. The influence of glass matrix and hydroxyl concentration ( ^– >) was studied to investigate the suitability for thermometry. We obtained Suprasil samples with ^– > between 200 and 1000 ppm by annealing in vacuum. We also measured commercial Homosil glass. The sensitivity is proportional to ^– >, but saturation of the dielectric susceptibility occurs at the same temperature for all samples.     

Preparation and rheological behavior of lead free silver conducting paste

The lead free silver conducting pastes were prepared by using silver powder, lead free low-melting glass and terpineol ethyl cellulose solution. By analyzing the sheet resistance, Vickers hardness as well as the adhesion strength of the fired film by the pastes formulated with different content of the glass, the desired glass weight percentage was determined as 4–6 wt%. The films, prepared by the pastes using the lead free glass with a glass transition temperature of 488 °C, were perfectly flat and compact after fired at a peak temperature within the range from 540 °C to 590 °C. The sheet resistance of the fired film with glass content of 5 wt% was 2.3 × 10⁻³ Ω mm⁻² at the thickness of 15 ± 3 μm, while the Vickers hardness was 61 MPa, and the adhesion strength was 28.5 MPa. In addition, the rheological, thixotropic, and viscoelasticity behaviors of the typical paste characterized by using an ARES (RFS-III) rheometer, were similar to that of the screen printing paste with high solid filler. The pastes are applicable for manufacturing electrical components on glass substrate.     

Microstructure and superplasticity of Mg–Al–Ca electromagnetic casting alloys after hot extrusion

Microstructure and superplastic properties of the plates extruded from the Ca containing Mg alloy (1 wt.% Ca–AZ31) billets fabricated by electromagnetic casting (EMC) without and with electromagnetic stirring (EMS) were examined. The linear intercept grain sizes of the extruded materials were 3.7 μm and 2.1 μm, respectively. The material extruded from the EMC + EMS billet exhibited good superplasticity at low temperatures as well as at high strain rates, including the tensile elongations of 370% at 1 × 10⁻³ s⁻¹, −523 K and 550% at 1 × 10⁻² s⁻¹, −673 K. These values largely exceeded those of the AZ31 alloys with the similar grain sizes. The superior superplasticity of the extruded EMC + EMS billet could be attributed to fine grains and high grain stability at elevated temperatures by the presence of finely dispersed particles of thermally stable (Al,Mg)₂Ca phase. The constitutive equations were developed for describing the high-temperature deformation behavior of the fine-grained 1 wt.% Ca–AZ31 alloys with different grain sizes in wide range of temperature and strain rate.     

The structural and electrical property of CuCr1 − xNixO2 delafossite compounds

A series of CuCr_1 − xNi_xO₂ (0 ≤ x ≤ 0.06) polycrystalline samples was prepared. The electrical conductivity was measured in the temperature range of 160–300 K. It was found that the electrical conductivity (σ) increases rapidly with the doping of Ni²⁺ ions. At room temperature, the σ is 0.047 S cm^− 1 for the sample with x = 0.06, which is two orders of magnitude larger than that of the CuCrO₂ sample (9.49E− 4 S cm^− 1). The Seebeck coefficients are positive for all samples, which indicate p-type conducting of the samples. The experimental results imply that it is possible to get higher electrical conductivity p-type transparent conducting oxides (TCO) from CuMO₂ by doping with divalent ions.     

Deformability enhancement in ultra-fine grained, Ar-contained W compacts by TiC additions up to 1.1%

Nano-sized Ar bubbles give negative influence on the fracture resistance and occurrence of superplasticity in ultra-fine grained (UFG) W–TiC compacts. In order to enhance deformability in UFG, Ar-contained W–TiC compacts, effects of TiC addition on the high-temperature deformation behavior were examined. W–TiC compacts with TiC additions of 0, 0.25, 0.5, 0.8 and 1.1 wt% were fabricated by mechanical alloying in a purified Ar atmosphere and hot isostatic pressing. Tensile tests were conducted at 1673–1973 K (0.45–0.54 T_m, T_m: melting point of W) at initial strain rates from 5 × 10⁻⁵ to 5 × 10⁻³ s⁻¹. It is found that as TiC addition increases, the elongation to fracture significantly increases, e.g., from 3 to 7% for W–0 and 0.25TiC/Ar to above 160% for W–1.1TiC/Ar when tested at 1873 and 1973 K at 5 × 10⁻⁴ s⁻¹. The flow stress takes a peak at 0.25%TiC and decreases to a nearly constant level at 0.5–1.1%TiC. The ranges of the strain rate sensitivity of flow stress, m, and the activation energy for deformation, Q, with TiC additions are 0.17–0.30 and 310–600 kJ/mol, respectively. The observed effects of the TiC additions on the tensile properties are discussed.     

Improved microstructure and flux pinning properties of Gd-substituted (Bi,Pb)-2212 superconductor sintered between 846 and 860 °C

The influence of sintering temperature on microstructural and superconducting properties of Gd-substituted (Bi,Pb)-2212 superconductor was investigated. It is found that the microstructure of the system can be tailored and refined so as to yield the best superconducting properties in terms of critical current density (J_C) and flux pinning by heat treating at a temperature in the range 846-860 °C. The samples sintered at 858 °C show the maximum self-field J_C of 31,960 kA m^{− 2} and those sintered at 846 °C show the maximum flux pinning force [F_P = 1698 kN m^{− 3}] as against 1860 kA m^{− 2} and 16 kN m^{− 3}, respectively for the undoped sample sintered at its optimum sintering temperature. The changes in microstructure followed by very high enhancement of J_C, J_C-B characteristics and F_P due to Gd-substitution within a small temperature range, is of great scientific and technological significance.     

Electrical and optical properties of 12CaO·7Al2O3 electride doped indium tin oxide thin film deposited by RF magnetron co-sputtering

12CaO·7Al₂O₃ electride (C12A7:e⁻) doped indium tin oxide (ITO) (ITO:C12A7:e⁻) thin films were fabricated on a glass substrate by an RF magnetron co-sputtering system with increasing number of C12A7:e⁻ chips (from 1 to 7) and at various oxygen partial pressure ratios. The optical transmittance of the ITO:C12A7:e⁻ thin film was higher than 70% in the visible wavelength region. In the electrical properties of the thin film, a decrease of the carrier concentration from 2.6 × 10²⁰ cm^− 3 to 2.1 × 10¹⁸ cm^− 3 and increase of the resistivity from 1.4 × 10^− 3 Ω cm to 4.1 × 10^− 1 Ω cm were observed with increasing number of C12A7:e⁻ chips and oxygen partial pressure ratios. It was also observed that the Hall mobility was decreased from 17.27 cm²·V^− 1·s^− 1 to 5.13 cm²·V^− 1·s^− 1. The work function of the ITO thin film was reduced by doping it with C12A7:e⁻.     

Alkaline aluminum phosphate glasses for thermal ion-exchanged optical waveguide

Alkaline aluminum phosphate glasses (NMAP) with excellent chemical durability for thermal ion-exchanged optical waveguide have been designed and investigated. The transition temperature Tg (470 °C) is higher than the ion-exchange temperature (390 °C), which is favorable to sustain the stability of the glass structure for planar waveguide fabrication. The effective diffusion coefficient D_e of K⁺–Na⁺ ion exchange in NMAP glasses is 0.110 μm²/min, indicating that ion exchange can be achieved efficiently in the optical glasses. Single-mode channel waveguide has been fabricated on Er³⁺/Yb³⁺ doped NMAP glass substrate by standard micro-fabrication and K⁺–Na⁺ ion exchange. The mode field diameter is 9.6 μm in the horizontal direction and 6.0 μm in the vertical direction, respectively, indicating an excellent overlap with a standard single-mode fiber. Judd–Ofelt intensity parameter Ω₂ is 5.47 × 10⁻²⁰ cm², implying a strong asymmetrical and covalent environment around Er³⁺ in the optical glasses. The full width at half maximum and maximum stimulated emission cross section of the ⁴I_13/2 → ⁴I_15/2 are 30 nm and 6.80 × 10⁻²¹ cm², respectively, demonstrating that the phosphate glasses are potential glass candidates in developing compact optoelectronic devices. Pr³⁺, Tm³⁺ and Ho³⁺ doped NMAP glasses are promising candidates to fabricate waveguide amplifiers and lasers operating at special telecommunication windows.