A low-temperature reactive sintering process for the 5Li2O–1Nb2O5–5TiO2 microwave dielectric ceramics

The B₂O₃-doped 5Li₂O–1Nb₂O₅–5TiO₂ composite microwave dielectric ceramics prepared by conventional and low-temperature single-step reactive sintering processes were investigated in the study. Without any calcinations involved, the Nb₂O₅ mixture of Li₂CO₃ and TiO₂ was pressed and sintered directly in the reactive sintering process. More uniform and finer grains could be obtained in the 5Li₂O–1Nb₂O₅–5TiO₂ ceramics by reactive sintering process, which could effectively save energy and manufacturing cost. And relatively good microwave dielectric properties of _r = 41, Q × f = 9885 GHz and τ_f = 43.6 ppm/°C could be obtained for the 1 wt.% B₂O₃-doped ceramics reactively sintered at 900 °C.     

Low cycle fatigue mechanism of René 80 at high temperature–high strain

The low cycle fatigue René 80, a Ni-base superalloy, was studied at temperature of 871 °C, R = (_min/_max) = 0 and strain rate of about 2 × 10⁻³ s⁻¹. The dislocation structure and failure surface observations were evaluated through TEM and SEM. TEM studies showed that at Δ_t = 0.8% during the first cycle the dislocations formed a hexagonal network in the γ-phase matrix. When the number of cycles increased, the density of dislocations increased as well. At N = N_f and Δ_t = 0.8% the cutting of γ′ precipitates took place. SEM studies at Δ_t = 0.8% and N = N_f showed that fatigue crack initiation generally occurred at the surface, where it is depleted of the γ′ phase as a result of oxidation by the high-temperature exposure. In addition to depleted zones, the grain boundary oxidation and oxide spikes were also considered as further crack initiation sites.     

Structure and mechanical properties of extruded Mg–Gd based alloy sheet

The Mg–8Gd–2Y–1Nd–0.3Zn–0.6Zr (wt.%) alloy sheet was prepared by hot extrusion technique, and the structure and mechanical properties of the extruded alloy were investigated. The results show that the alloy in different states is mainly composed of α-Mg solid solution and secondary phases of Mg₅RE and Mg₂₄RE₅ (RE = Gd, Y and Nd). At aging temperatures from 200 °C to 300 °C the alloy exhibits obvious age-hardening response. Great improvement of mechanical properties is observed in the peak-aged state alloy (aged at 200 °C for 60 h), the ultimate tensile strength (σ_b), tensile yield strength (σ_0.2) and elongation () are 376 MPa, 270 MPa and 14.2% at room temperature (RT), and 206 MPa, 153 MPa and 25.4% at 300 °C, respectively, the alloy exhibits high thermal stability.     

Microwave dielectric properties and sintering behavior of nano-scaled (α + θ)-Al2O3 ceramics

The dielectric properties at microwave frequencies and the microstructures of nano (α + θ)-Al₂O₃ ceramics were investigated. Using the high-purity nano (α + θ)-Al₂O₃ powders can effectively increase the value of the quality factor and lower the sintering temperature of the ceramic samples. Grain growth can be limited with θ-phase Al₂O₃ addition and high-density alumina ceramics can be obtained with smaller grain size comparing to pure α-Al₂O₃. Relative density of sintered samples can be as high as 99.49% at 1400 °C for 8 h. The unloaded quality factors Q × f are strongly dependent on the sintering time. Further improvement of the Q × f value can be achieved by extending the sintering time to 8 h. A dielectric constant (_r) of 10, a high Q × f value of 634,000 GHz (measured at 14 GHz) and a temperature coefficient of resonant frequency (τ_f) of −39.88 ppm/°C were obtained for specimen sintered at 1400 °C for 8 h. Sintered ceramic samples were also characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM).     

Steady state creep and creep recovery behaviours of pre-aging Al–Si alloys

The creep and creep recovery of pre-aging Al–1 wt.%Si and Al–1 wt.%Si–0.1 wt.%Zr–0.1 wt.%Ti alloys have been investigated at room temperature under different constant stresses. The aging temperature dependence of steady creep rate, _st, and the recovery strain rate, π, show that under the same test conditions first alloy yields creep or creep recovery rates much higher as compared with those of second alloy. The stress exponent n was found to change from 2.5 to 7.43 and 4.57 to 11.99 for two alloys, respectively, characterizing dislocation slipping mechanism. The activation energies of steady state creep of the two alloys were found to be 78.4 kJ/mol and 32.8 kJ/mol for Al–Si and Al–Si–Zr–Ti alloys, respectively. The microstructure of the samples studied was investigated by optical and transmission electron microscopy (TEM).     

Emissions properties of Ho: I7 → I8 transition sensitized by Er and Yb in fluorophosphate glasses

Emission properties of Ho³⁺ at 2.0 μm and the energy transfer mechanism between Yb³⁺, Er³⁺ and Ho³⁺ ions in fluorophosphate glasses are investigated. The measured emission spectra show that the ⁵I₇ → ⁵I₈ transition of Ho³⁺ upon 980 nm laser diode excitation is strong. Judd–Ofelt intensity parameters (Ω_λ, λ = 2, 4, 6), spontaneous transition probability (A_rad), radiative lifetime (τ_r), absorption cross section (σ_a), stimulated emission cross section (σ_e) and FWHM ×  for the transition of Ho³⁺: ⁵I₇ → ⁵I₈ are calculated and discussed. The obtained results show that the present Yb³⁺/Er³⁺/Ho³⁺ triply-doped fluorophosphate glass can be identified to be a promising material at 2.0 μm emission.     

Optical bistability for ZnO–Nb2O5–TeO2 glasses

We examined the optical nonlinear properties of ZnO–Nb₂O₅–TeO₂. The absorption and Raman spectra were measured, the third-order nonlinear susceptibility was determined by degenerated four wave mixing technique. The magnitude of χ⁽³⁾ is about 1.0 × 10⁻¹² esu, larger than that of silica glasses, and the optical bistability was observed in a Fabry–Perot cavity.     

Spectral analysis of RE (RE = Sm, Dy, and Tm): P2O5–Al2O3–Na2O glasses

Phosphate glasses in the compositions of 70P₂O₅–15Al₂O₃–14Na₂O–1RE³⁺ (RE = Sm, Dy, and Tm) (mol%) were prepared by melt-quenching technique and characterized optically. The differential thermal analysis (DTA) profile of the host glass was carried out to confirm its thermal stability. For all the glasses absorption, photoluminescence and decay measurements have also been carried out. These glasses have shown strong emission and absorption bands in visible and near-infrared (NIR) region. From the measured absorption spectra, Judd–Ofelt (J–O) intensity parameters (Ω₂, Ω₄ and Ω₆) have been calculated for all the studied ions. For Sm³⁺ doped glass, four emission bands centered at 562 nm (⁴G_5/2 → ⁶H_5/2), 598 nm (⁴G_5/2 → ⁶H_7/2), 644 nm (⁴G_5/2 → ⁶H_9/2), and 704 nm (⁴G_5/2 → ⁶H_11/2) have been observed with 402 nm (⁶H_5/2 → ⁴F_7/2) excitation wavelength. Of them, 598 nm (⁴G_5/2 → ⁶H_7/2) has shown a bright orange emission. With regard to Dy³⁺ doped glass, a blue emission band centered at 486 nm (⁴F_9/2 → ⁶H_15/2) and a bright yellow emission at 575 nm (⁴F_9/2 → ⁶H_13/2) have been observed, apart from 662 nm (⁴F_9/2 → ⁶H_11/2) emission transition with an excitation at 388 nm (⁶H_15/2 → ⁴I_13/2,⁴F_7/2) wavelength. Emission bands of 650 nm (¹G₄ → ³F₄) and 785 nm (¹G₄ → ³H₅) transitions for the Tm³⁺ doped glass, with an excitation wavelength at 466 nm (³H₆ → ¹G₄), have also been observed. The stimulated emission cross-sections of all the emission bands of RE³⁺ glasses (RE = Sm, Dy, and Tm) have been computed based on their measured full-width at half maximum (FWHM, Δλ) and measured lifetimes (τ_m).     

Seebeck coefficient of V2O5-R2O3-TeO2 (R = Sb or Bi) glasses

The thermoelectric power of glasses in the systems V₂O₅-Sb₂O₃-TeO₂ and V₂O₅-Bi₂O₃-TeO₂ was measured at temperatures in the range 373–473 K. The glasses in both systems were found to be n-type semiconductors. The Seebeck coefficient, Q, at 473 K was determined as –192 to –151 VK^–1 for V₂O₅-Sb₂O₃-TeO₂ glasses, and –391 to –202 VK^–1 for V₂O₅-Bi₂O₃-TeO₂ glasses. For these glasses in both systems, Heikes' formula was satisfied adequately for the relationship between Q and In [C _v/(1-C_v)] (C _v = V⁴⁺/V_total, C _v is the ratio of the concentration of reduced vanadium ions), and discussions confirmed small polaron hopping conduction of the glasses in both systems. Mackenzie's formula relating to Q and V⁵⁺/V⁴⁺ was also applicable to the glasses in both systems, and it was concluded that the dominant factor determining Q was C _v.     

Cluster formation in Ag2O-P2O5-CdCl2 glass system

Ag₂O-P₂O₅ and Ag₂O-P₂O₅-20 wt% CdCl₂ glasses were prepared by melt quenching method and characterized with the help of several experimental techniques. Powder X-ray diffraction study indicated that the glasses are amorphous in nature. DSC studies showed that CdCl₂ doped glass is chemically more durable. Electrical conductivity and ionic transference number measurements have shown that both the glasses are ionic conductors with Ag⁺ ions as the charge carriers. The electrical conductivity of the doped glass is found to be higher than the undoped one. Structures of the glasses have been proposed on the basis of IR spectral analysis. From SEM studies it has been inferred that addition of 20 wt% CdCl₂ modifies the morphology of Ag₂O-P₂O₅ glass and in its presence formation of clusters composed of nanofibers occur.     

A study of tensile properties in Al–Si–Cu and Al–Si–Mg alloys: Effect of β-iron intermetallics and porosity

The effect of β-iron intermetallics and porosity on the tensile properties in cast Al–Si–Cu and Al–Si–Mg alloys were investigated for this research study, using experimental and industrial 319.2 alloys, and industrial A356.2 alloys. The results showed that the alloy ductility and ultimate tensile strength (UTS) were subject to deterioration as a result of an increase in the size of β-iron intermetallics, most noticeable up to β-iron intermetallic lengths of 100 μm in 319.2 alloys, or 70 μm in A356.2 alloys. An increase in the size of the porosity was also deleterious to alloy ductility and UTS. Although tensile properties are interpreted by means of UTS vs. log elongation plots in the present study, the properties for all sample conditions were best interpreted by means of log UTS vs. log elongation plots, where the properties increased linearly between conditions of low cooling rate–high Fe and high cooling rate–low Fe. The results are explained in terms of the β-Al₅FeSi platelet size and porosity values obtained.     

Compositional dependence of spectroscopic parameters of Dy ions in Ge–Ga–Se glasses

Dy³⁺ doped chalcogenide glasses from Ge–Ga–Se system were prepared and spectroscopic parameters of Dy³⁺ ions in these glasses were studied on the basis of Judd–Ofelt theory. We have found that the values of Judd–Ofelt intensity parameters Ω_t (t = 2, 4, 6) have maximal values at the GeSe₂–Ga₂Se₃ tie-line. Largest values of spectroscopic parameters of 1.3 µm Dy³⁺ transition (⁶F_11/2, ⁶H_9/2 → ⁶H_15/2), localized again at the GeSe₂–Ga₂Se₃ tie-line, confirm the importance of the stoichiometry of amorphous matrix for optical properties of doping rare-earth ions.     

Non-adiabatic polaron hopping conduction in semiconducting V2O5-Bi2O3 oxide glasses doped with BaTiO3

BaTiO₃-doped (5–40 wt %) 90V₂O₅-10Bi₂O₃ (VB) glasses have been prepared by a quick quenching technique. The d.c. electrical conductivities, _d.c., of these glasses have been reported in the temperature range 80–450 K. The electrical conductivity of these glasses, which arises due to the presence of V⁴⁺ and V⁵⁺ ions, has been analysed in the light of the small-polaron hopping conduction mechanism. The adiabatic hopping conduction valid for the undoped VB glasses (with 80–95 mol % V₂O₅), in the high-temperature region, is changed to a non-adiabatic hopping mechanism in the BaTiO₃-doped VB glasses. At lower temperatures, however, a variable range hopping (VRH) mechanism dominates the conduction mechanism in both the glass systems. Such a change-over from adiabatic to non-adiabatic conduction mechanism is a new feature in transition metal oxide glasses. Various parameters, such as density of states at the Fermi level N(E_F), electron wave-function decay constant, , polaron radius, r _p, and its effective mass, m _p ^* , etc., have been obtained for all the glass samples from a critical analysis of the electrical conductivity data satisfying the theory of polaron hopping conduction.     

Influence of Cu addition on the self-propagating high-temperature synthesis of Ti5Si3 in Cu–Ti–Si system

The self-propagating high-temperature synthesis (SHS) reactions can take place in Cu–Ti–Si systems with Cu additions of 10–50 wt.%, and the products only consist of Ti₅Si₃ and Cu phases, without any transient phase. In Ti–Si system, most of the Ti₅Si₃ grains synthesized exhibit the polygon-shaped coarse appearance with an obviously sintered morphology. When Cu content increases from 10 to 50 wt.%, however, the Ti₅Si₃ exhibits cobblestone-like shape with a relatively smooth surface, and its average size decreases significantly from 15 to 2 μm or less. The formation mechanism of Ti₅Si₃ in Cu–Ti–Si system is characterized by the solution, reaction and precipitation processes. Furthermore, the addition of Cu has a great influence on the volume change between green and reacted preforms. The volume change increases with Cu content increasing from 0 to 20 wt.%, and then decreases with the content further increasing from 20 to 50 wt.%. The addition of Cu to Ti–Si system significantly decreases the onset temperature of the reaction during differential scanning calorimetry process, which is even much lower than the α → β transition temperature of Ti (882 °C), suggesting that the reaction could be greatly facilitated by Cu addition. As a result, the role of Cu serves not only as a diluent but also as a reactant and participates in the self-propagating high-temperature synthesis reaction process.     

Ultrafast third-order optical non-linearity of 0.56GeS2–0.24Ga2S3–0.2KX(X = Cl, Br, I) chalcohalide glasses by femtosecond Optical Kerr Effect

0.56GeS₂–0.24Ga₂S₃–0.2KX(X = Cl, Br, I) chalcohalide glasses were prepared and their third-order optical non-linearities χ⁽³⁾ have been studied systematically using the femtosecond time-resolved Optical Kerr Effect technique at wavelength of 800 nm. In this system, 0.56GeS₂–0.24Ga₂S₃–0.2KCl glass shows the largest χ⁽³⁾ (1.82 × 10⁻¹³ esu), but 0.56GeS₂–0.24Ga₂S₃–0.2KBr glass has the fastest optical non-linear response time in subpicosecond domain (about 340 fs), which is due to the ultrafast distortion of the electron clouds surrounding the balanced position of Ge, Ga, S, K and Br atoms. The local hyperpolarizability determining non-linear optical response are determined by the partially ionic bonds originating from Ge(Ga)–S bonds and halogen valence bonds. They show great potential applications on the glass-based optoelectronic devices like optical switching.     

Raman spectroscopic study of structure of WO3La2O3B2O3 glasses with no color and crystallization of LaBWO6

Glasses with the nominal compositions of xWO₃25La₂O₃(75 − x)B₂O₃ (mol%) with x = 15, 25, and 50 were prepared using a conventional melt quenching method, and their structure and crystallization behavior were examined from Raman scattering spectra and X-ray diffraction analyses. The glasses are colorless in the visible light region and give the optical band gap energy of 3.49-3.61 eV. The glass transition and crystallization temperatures and the thermal stability against crystallization decrease with increasing WO₃ content. The strong Raman bands at 840 and 940-960 cm⁻¹ suggest that the main coordination state of W⁶⁺ ions in the glasses is isolated (WO₄)²⁻ tetrahedral units. The formation of WO₆ octahedral units is also suggested in the glasses with high WO₃ contents. The main crystallization mechanism in the glasses is the surface crystallization, and the glass of 50WO₃25La₂O₃25B₂O₃ shows the crystallization of LaBWO₆ single phase. The present study proposes that WO₃La₂O₃B₂O₃ glasses and crystallized glasses are very interesting as optical functional materials.     

Dependence of optical properties on the composition in Er-doped xNaPO3–(80 − x)TeO2–10ZnO–10Na2O glasses

Transparent and uniform tellurite–phosphate glasses were prepared and the reason why the substitution of NaPO₃ for P₂O₅ can eliminate the coloration of tellurite–phosphate was discussed. The result of TDA indicated that introducing NaPO₃ into tellurite glasses can improve thermal stability of glass hosts. The compositional dependence of absorption cross-sections of ⁴I_13/2, ⁴I_11/2 and ²H_11/2 level, emission cross-section of ⁴I_13/2 level, host phonon energy, up-conversion and 1.5 μm optical emission intensity as well as and quantum yield for ⁴I_13/2 level in PTEr glasses were investigated too. By analyzing obtained data, authors believe that tellurite–phosphate glasses can be used as potential host material for developing optical amplifiers.     

Non-linear concentration-dependent electrical properties of some semiconducting vanadate glasses

Characterizations of (50 – x) P₂O₅-x M-50V₂O₅ (M = Bi₂O₃, Sb₂O₃, and GeO₂ and x=0 to 45 mol% M) and P₂O₅-Bi₂O₃ semiconducting oxide glasses have been made from studies of electrical conductivities (both a.c. and d.c.) in the temperature range 77 to 400 K. All these glasses showed some interesting non-linear variation of d.c. and a.c. conductivity, together with other properties for particular values of M (between 20 and 30 mol% M). Because the non-vanadate (1–x) P₂O₅-x Bi₂O₃ glasses also showed similar conductivity anomaly (minimum) around 25 mol% Bi₂O₃ with a corresponding maximum in the activation energy (W), it is concluded (in contradiction to earlier suggestions) that not only the ratio (= V⁵⁺/V⁴⁺) but also the network-former ions in the vanadate glasses make a substantial contribution to the anomalous concentration variation of the physical properties of these glasses. The electrical conduction in these glasses is found to be mainly due to hopping of polarons in the adiabatic approximation. At low temperature, the d.c. conductivity obeys Mott's T ^–1/4 behaviour. The a.c. conductivity obeying the general ^s law (exponent s lying between 0.85 and 0.98) supports the theory based on the hopping over the barrier model.     

Analysis of the air flow in a cold store by means of computational fluid dynamicsAnalyse du débit d'air dans un entrepôt frigorifique à l'aide de la dynamique des fluides informatisée

Airflow inside a cold store is investigated using computational fluid dynamics. The airflow model is based on the steady state incompressible, Reynolds-averaged Navier–Stokes equations. The turbulence is taken into account using a k− model. The standard as well as the Renormalisation-Group (RNG) version of the k− model is investigated. The forced-circulation air cooler unit is modelled with an appropriate body force and resistance, corresponding to the characteristics of the fan and the tube-bank evaporator. The finite volume method of discretisation is used. The validation of the model has been performed by a comparison of the calculated time-averaged velocity magnitudes with the mean velocities measured by means of a hot-film type omni-directional velocity sensor. A relative error on the calculated air velocities of 26% was observed. The RNG k− model does not help to improve the prediction of the recirculation. Both a finer grid and enhanced turbulence models are needed to improve the predictions.     

Effect of Ni-modified α-Al2O3 prepared by sol–gel and solvothermal methods on the characteristics and catalytic properties of Pd/α-Al2O3 catalysts

In the present study, Ni-modified α-Al₂O₃ with Ni/Al ratios of 0.3 and 0.5 were prepared by sol–gel and solvothermal method and then were impregnated with 0.3 wt.% Pd. Due to different crystallization mechanism of the two preparation methods used, addition of nickel during preparation of α-Al₂O₃ resulted in various species such as NiAl₂O₄, mixed phases between NiAl₂O₄ and α-Al₂O₃, and mixed phases between NiAl₂O₄ and NiO. As revealed by NH₃-temperature programmed desorption, formation of NiAl₂O₄ drastically reduced acidity of alumina, hence lower amounts of coke deposited during acetylene hydrogenation was found for the Ni-modified α-Al₂O₃ supported catalysts. For any given method, ethylene selectivity was improved in the order of Pd/Ni–Al₂O₃-0.5 > Pd/Ni–Al₂O₃-0.3 > Pd/Ni–Al₂O₃-0  Pd/α–Al₂O₃-commercial. When comparing the samples prepared by different techniques, the sol–gel-made samples showed better performances than the solvothermal-derived ones.