Preparation and characterization of N–I co-doped nanocrystal anatase TiO2 with enhanced photocatalytic activity under visible-light irradiation

N–I co-doped TiO₂ nanoparticles were prepared by hydrolysis method, using ammonia and iodic acid as the doping sources and Ti(OBu)₄ as the titanium source. The prepared catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and ultraviolet–visible diffuse reflection spectroscopy (UV–vis DRS). XRD spectra show that N–I–TiO₂ samples calcined at 673 K for 3 h are of anatase structure. XPS analysis of N–I–TiO₂samples indicates that some N atoms replace O atoms in TiO₂ lattice, and I exist in I⁷⁺, I⁻ and I⁵⁺ chemical states in the samples. UV–vis DRS results reveal that N–I–TiO₂ had significant optical absorption in the region of 400–600 nm. The photocatalytic activity of catalysts was evaluated by monitoring the photocatalytic degradation of methyl orange (MO). Compared with P25 and mono-doped TiO₂, N–I–TiO₂ powder shows higher photocatalytic activity under both visible-light (λ > 420 nm) and UV–vis light irradiation. Furthermore, N–I–TiO₂ also displays higher COD removal rate under UV–vis light irradiation.     

Effect of bismuth on the properties of Mn ferrite nanoparticles prepared by co-precipitation method

Nanoparticles of MnBi_xFe_2−xO₄(x = 0.0, 0.02, 0.04, 0.06) have been synthesized by a chemical co-precipitation method. X-ray diffraction analysis (XRD) reveals that bismuth exits in its Bi³⁺ and Bi⁵⁺ state. It was also observed that bismuth substitution enhances the grain growth and density. The dielectric constant (ε′) and the loss tangent (tan δ) increases with increase in bismuth content. Resistivity (ρ) and maximum magnetization (M) was found to decrease with increasing bismuth content.     

Intercalation of copper into bismuth telluride

The intercalation and leaching of copper into and out of bismuth telluride was investigated using aqueous and solid state electrochemical methods. It was found that copper intercalates up to a concentration of 3 mg/g bismuth telluride. Copper may also react with bismuth telluride to form copper telluride (Cu₂Te). Boiling hydrochloric acid leaches, or controlled potential electrochemical leaches, were effective at removing intercalated copper from bismuth telluride, returning the bismuth telluride to its original, undoped state. E.m.f. measurements using a solid, copper-ion conducting electrolyte resulted in copper activities of between 0.000 73 and 0.044 for intercalated bismuth telluride. An effective copper diffusion coefficient of 4×10^–5 cm²s^–1 was measured for a sintered polycrystalline bismuth telluride pellet at 483 K.This work was conducted at the Department of Materials Science and Metallurgy, University of Cambridge, Cambridge CB2 3Q2, UK     

Preparation of SrAl2O4: Eu, Dy nanometer phosphors by detonation method

SrAl₂O₄: Eu²⁺, Dy³⁺ nanometer phosphors were synthesized by detonation method. The particle morphology and optical properties of detonation soot that was heated at different temperatures (600–1100 °C) had been studied systematically by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Results indicated SrAl₂O₄: Eu²⁺, Dy³⁺ nanometer powders in monoclinic system (a = 8.442, b = 8.822, c = 5.160, β = 93.415) can be synthesized by detonation method, when detonation soot was heated at 600–800 °C. The particle size of SrAl₂O₄: Eu²⁺, Dy³⁺ is 35 ± 15 nm. Compared with the solid-state reaction and sol-gel method, synthesis temperature of the detonation method is lower about 500 and 200 °C respectively. After being excited under UN lights, detonation soot and that heated at 600–1100 °C can emit a green light.     

Preparation of double-doped BaCeO3 and its application in the synthesis of ammonia at atmospheric pressure

Perovskite-type oxides BaCe_0.90Sm_0.10O_3−δ (BCS) and BaCe_0.80Gd_0.10Sm_0.10O_3−δ (BCGS) were synthesized by the sol–gel method and characterized by thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Using the sintered samples as solid electrolytes and silver–palladium alloy as electrodes, ammonia was synthesized from nitrogen and hydrogen at atmospheric pressure in a solid-state proton-conducting cell reactor. The maximum rate of production of ammonia was 5.82×10⁻⁹ mol s⁻¹ cm⁻².     

Eddy current and total power loss separation in the iron–phosphate–polyepoxy soft magnetic composites

This work investigates the magnetic properties of iron–phosphate–polyepoxy soft magnetic composite materials. FTIR spectra, EDX analysis, distribution maps, X-ray diffraction pattern and density measurements show that the particles surface layer contains a thin layer of nanocrystalline/amorphous phosphate with high coverage of powders surface. In this paper, a formula for calculating the eddy current loss and total loss components by loss separation method is presented and finally the different parts of power losses are calculated. The results show that, the contribution of eddy current in the bulk material for single coating layer (k_b = 0.18) is higher in comparison with double coating layer (k_b = 0.09). Moreover, iron–phosphate–polyepoxy composites (P = 0.000004f²) have lower power loss in comparison with iron–phosphate composites (P = 0.00002f²).     

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.     

Electrospinning preparation and characterization of a new kind of composite nanomaterials: One-dimensional composite nanofibers doped with TiO2 nanoparticles and Ru(II) complex

One-dimensional composite nanomaterials, PVP (poly(vinylpyrrolidone)) fibers with diameters in the range of 300–500 nm doped with RuL₂(NCS)₂ (L = 4,4′-Dicarboxy-2,2′-bipyridine) complex and TiO₂ nanoparticles (NPs), were prepared by electrospinning technique. The morphology of the composite nanofibers was systemically studied when the diameters of TiO₂ NPs, the concentrations of TiO₂ NPs and RuL₂(NCS)₂ in the PVP matrix were changed. A new kind of organic–inorganic composite nanomaterials which combine the advantages of one-dimensional nanostructures, organic materials and inorganic materials was obtained and it is desirable for low-weight and flexible photovoltaic devices, especially for dye-sensitized TiO₂ solar cells.     

Irradiation induced effects on Ni3N/Si bilayer system

The irradiation effect in Ni₃N/Si bilayers induced by 100 MeV Au ions at fluence 1.5 × 10¹⁴ ions/cm² was investigated at room temperature. Grazing incidence X-ray diffraction determined the formation of Ni₂Si and Si₃N₄ phases at the interface. The roughness of the thin film was measured by atomic force microscopy. X-ray reflectivity was used to measure the thickness of thin films. X-ray photoelectron spectroscopy has provided the elemental binding energy of Ni₃N thin films. It was observed that after irradiation (Ni 2p_3/2) peak shifted towards a lower binding energy. Optical properties of nickel nitride films, which were deposited onto Si (100) by ion beam sputtering at vacuum 1.2 × 10⁻⁴ torr, were examined using Au ions. In-situ I–V measurements on Ni₃N/Si samples were also undertaken at room temperature which showed that there is an increase in current after irradiation.     

Novel fabrication of monodispersed peanut-type celestine particles using Sr-EDTA chelating precursors

Novel monodispersed peanut-type SrSO₄ (celestine) particles have been prepared using a facile precipitation reaction of Sr-EDTA chelating precursors at ambient temperature. The as-formed products were studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), nitrogen absorption–desorption and differential scanning calorimetry–thermogravimetry (DSC–TG) measurement. The monodispersed SrSO₄ particles with an average length of 1.7 μm and an aspect ratio of 1.4 appear unusual peanut-type morphology. These SrSO₄ particles have a relatively large Brunauer–Emmett–Teller (BET) surface area of about 20.9 m² g⁻¹ and contain mesopores with a mean pore size of about 34.3 nm. The SrSO₄ particles exhibit an excellent thermal stability from room temperature to 1400 °C with a structural transformation at 1158.3 °C. The growth mechanism of the monodispersed peanut-type celestine particles was discussed to obtain a better understanding on their formation process.     

Preparation and studies on surface modifications of calcium-silico-phosphate ferrimagnetic glass-ceramics in simulated body fluid

The structure and magnetic behaviour of 34SiO₂–(45 − x) CaO–16P₂O₅–4.5 MgO–0.5 CaF₂ − x Fe₂O₃ (where x = 5, 10, 15, 20 wt.%) glasses have been investigated. Ferrimagnetic glass-ceramics are prepared by melt quench followed by controlled crystallization. The surface modification and dissolution behaviour of these glass-ceramics in simulated body fluid (SBF) have also been studied. Phase formation and magnetic behaviour have been studied using XRD and SQUID magnetometer. The room temperature Mössbauer study has been done to monitor the local environment around Fe cations and valence state of Fe ions. X-ray photoelectron spectroscopy (XPS) was used to study the surface modification in glass-ceramics when immersed in simulated body fluid. Formation of bioactive layer in SBF has been ascertained using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The SBF solutions were analyzed using an absorption spectrophotometer. The magnetic measurements indicated that all these glasses possess paramagnetic character and the [Fe²⁺/Fe³⁺] ions ratio depends on the composition of glass and varied with Fe₂O₃ concentration in glass matrix. In glass-ceramics saturation magnetization increases with increase in amount of Fe₂O₃. The nanostructure of hematite and magnetite is formed in the glass-ceramics with 15 and 20 wt.% Fe₂O₃, which is responsible for the magnetic property of these glass-ceramics. Introduction of Fe₂O₃ induces several modifications at the glass-ceramics surface when immersed in SBF solution and thereby affecting the surface dissolution and the formation of the bioactive layer.     

Preparation of fatigue-free SrBi2Ta2O9 thin films by r.f. magnetron sputtering and their ferroelectric properties

Fatigue-free bismuth-layered SrBi₂Ta₂O₉ (SBT) films were deposited on Pt/Ti/SiO₂/Si substrates by r.f. magnetron sputtering at room temperature. The variation of structure and electrical properties were studied as a function of annealing temperatures from 750–850 °C. The films annealed at 800 °C had a composition ratio of Sr:Br:Ta = 0.7:2.0:2.0. X-ray photoelectron spectroscopy signals of bismuth show an oxygen-deficient state within the SBT films. The films annealed at 800 °C have a thickness of 200 nm and a relatively dense microstructure. The remanent polarization (2P _r), and the coercive field (2E _c), obtained for the SIBT films, were 9.1 C cm^–2 and 85 kV cm^–1 at an applied voltage of 3 V, respectively. The films showed fatigue-free characteristics up to 10¹⁰ cycles under 5 V bipolar square pulses. The leakage current density was about 7 × 10^–7 A cm^–2 at 150 kV cm^–1. The SBT films prepared by r.f. magnetron sputtering were attractive for application to non-volatile memories.     

Synthesis of layered Li1.2+x[Ni0.25Mn0.75]0.8−xO2 materials (0 ≤ x ≤ 4/55) via a new simple microwave heating method and their electrochemical properties

Li_1.2+x[Ni_0.25Mn_0.75]_0.8−xO₂ (0 ≤ x ≤ 4/55) was prepared by a new simple microwave heating method and the effect of extra Li⁺ content on electrochemistry of Li_1.2Ni_0.2Mn_0.6O₂ (x = 0) was firstly revealed. X-ray diffraction identified that they had layered α-NaFeO₂ structure (space group R-3m). Linear variation of lattice constant as a function of x value supported the formation of solid solution, that is, extra Li⁺ is possibly incorporated in structure of layered Li_1.2Ni_0.2Mn_0.6O₂ (x = 0), accompanying oxidization of Ni²⁺ to Ni³⁺ to form Li_1.2+x[Ni_0.25Mn_0.75]_0.8−xO₂ (0 ≤ x ≤ 4/55). This was confirmed by X-ray photoelectron spectroscopy that Ni³⁺ appeared and increased in content with increasing x value. Charge–discharge tests showed that Li_1.2+x[Ni_0.25Mn_0.75]_0.8−xO₂ (0 ≤ x ≤ 4/55) truly displayed different electrochemical properties (different initial charge–discharge plots, capacities and cycleability). Li_1.2Ni_0.2Mn_0.6O₂ (x = 0) in this work delivered the highest discharge capacity of 219 mAh g⁻¹ between 4.8 and 2.0 V. Increasing Li content (x value in Li_1.2+x[Ni_0.25Mn_0.75]_0.8−xO₂) reduced charge–discharge capacities, but significantly enhancing cycleability.     

Yellow-emitting phosphor of Sr3B2O6:Eu for application to white light-emitting diodes

This work focuses on the development of Eu²⁺-doped strontium (Sr)-borate as a yellow-emitting phosphor and its application to the fabrication of white light-emitting diodes (LEDs). Synthesis of Eu²⁺-doped Sr-borate phosphors was finely tuned for obtaining the efficient yellow luminescence through varying host composition, Eu concentration, and firing temperature. The 1300 °C-fired Eu²⁺-doped Sr₃B₂O₆, which was found to be the most efficient candidate to date, was used for white LED fabrication. Their optical properties were evaluated, resulting in warm white lights with CIE chromaticity coordinates of (0.340–0.372, 0.287–0.314) and color rendering indices of 75–77 under the forward currents of 5–40 mA.     

Sorption behavior of nano-TiO2 for the removal of selenium ions from aqueous solution

Titanium dioxide nanoparticles were employed for the sorption of selenium ions from aqueous solution. The process was studied in detail by varying the sorption time, pH, and temperature. The sorption was found to be fast, and to reach equilibrium basically within 5.0 min. The sorption has been optimized with respect to the pH, maximum sorption has been achieved from solution of pH 2–6. Sorbed Se(IV) and Se(VI) were desorbed with 2.0 mL 0.1 mol L⁻¹ NaOH. The kinetics and thermodynamics of the sorption of Se(IV) onto Nano-TiO₂ have been studied. The kinetic experimental data properly correlate with the second-order kinetic model (k₂ = 0.69 g mg⁻¹ min⁻¹, 293 K). The overall rate process appears to be influenced by both boundary layer diffusion and intraparticle diffusion. The sorption data could be well interpreted by the Langmuir sorption isotherm. The mean energy of adsorption (14.46 kJ mol⁻¹) was calculated from the Dubinin–Radushkevich (D–R) adsorption isotherm at room temperature. The thermodynamic parameters for the sorption were also determined, and the ΔH⁰ and ΔG⁰ values indicate exothermic behavior.     

Up-conversion luminescence properties of Y2O2S:Yb,Er nanophosphors

Up-converting yttrium oxysulfide nanomaterials doped with ytterbium and erbium (Y₂O₂S:Yb³⁺,Er³⁺) were prepared with the flux method. The precursor oxide materials were prepared using the combustion synthesis. The morphology of the oxysulfides was characterized with transmission electron microscopy (TEM). The particle size distribution was 10–110 nm, depending on the heating temperature. According to the X-ray powder diffraction (XPD), the crystal structure was found hexagonal and the particle sizes estimated with the Scherrer equation agreeded with the TEM images. Upon the 970 nm infrared (IR) laser excitation, the materials yield moderate green ((²H_11/2, ⁴S_3/2) → ⁴I_15/2 transition) and strong red (⁴F_9/2 → ⁴I_15/2) luminescence. The green luminescence was enhanced with respect to the red one by an increase in both the crystallite size and erbium concentration due to the cross-relaxation (CR) processes. The most intense up-conversion luminescence was achieved with x_Yb and x_Er equal to 0.10 and 0.005, respectively. Above these concentrations, concentration quenching occurred.     

Self-assembly of monodisperse SiO2-zinc borate core-shell nanospheres for lubrication

Spherical SiO₂ particles have been successfully coated with zinc borate layers through a self-assembly process. The resulted SiO₂-Zn₅B₄O₁₁ core-shell nanospheres were characterized by X-ray diffraction (XRD), infrared spectra (IR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) equipped with an energy-dispersive X-ray spectrometer (EDS). The obtained SiO₂-Zn₅B₄O₁₁ core-shell nanospheres have perfect spherical shape with narrow size distribution (average diameters 50 nm), i.e., the cores with mean diameters of 40 nm and the shells with an average thickness of 5 nm, monodisperse and smooth surface. Moreover, the friction coefficient of the base oil was decreased by the addition of SiO₂-Zn₅B₄O₁₁ core-shell nanospheres.     

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).     

Synthesis and characterization of nanocrystalline manganese pyrophosphate Mn2P2O7

Mn₂P₂O₇ polyhedral particles were synthesized by simple and cost-effective method using manganese nitrate hydrate and phosphoric acid in the presence of nitric acid with further calcinations at the temperature of 800 °C. The crystallite size obtained from X-ray line broadening is 31 ± 13 nm for the Mn₂P₂O₇. The X-ray diffraction and SEM results indicated that the synthesized nanoparticles have only the structure without the presence of any other phase impurities. The FT-IR and FT-Raman spectra show characteristic bands of the P₂O₇⁴⁻ anion. The UV–Vis–NIR spectrum confirms the octahedral coordination of Mn²⁺ ion.     

Stored energy of a severely deformed interstitial free steel

A Ti-stabilised IF steel subjected to room temperature equal channel angular pressing (ECAP) for 8 passes, route B_C was further cold rolled to 25, 50 and 95% thickness reductions. The evolution of bulk stored energy (350–600 J mol⁻¹) and the associated thermal behaviour was investigated by differential scanning calorimetry (DSC). Local stored energy (5–140 J mol⁻¹) was measured using microhardness, electron back-scattering diffraction (EBSD) and X-ray line profile analysis. The higher stored energy values via calorimetry correspond to energy release from all sources of strain in the material volume as well as Ti precipitation during annealing. An apparent activation energy of 500–550 J mol⁻¹ suggests sluggish recrystallisation due to excess Ti in solid solution.