Low-temperature synthesis,structural and magnetic properties of self-dopant LaMnO3+δ nanoparticles from a metal-organic polymeric precursor

Self-dopant LaMnO_3+δ nanoparticles have been successfully synthesized by metal citrate complex method based on Pechini-type reaction route, at low temperature (773 K). Powder X-ray diffraction and transmission electron microscope revealed pure and nanostructured phase of LaMnO_3+δ (δ = 0.125) with an average grain size of ∼72 nm (773 K) and ∼80 nm (1173 K). DC-magnetization measurements under an applied magnetic field of H = ±60 kOe showed an increase in the magnetization with the increase of calcination temperature. Ferromagnetic nature shown by non-stoichiometric LaMnO_3+δ was verified by well-defined hysteresis loop with large remanent magnetization (M_r) and coercive field (H_c). Surface areas of LaMnO_3+δ nanoparticles were found to be 157.4 and 153 m² g⁻¹ for the samples annealed at 773 K and 1173 K, respectively.     

MoS2 nanosheet functionalized with Cu nanoparticles and its application for glucose detection

For the first time, Cu nanoparticles were evenly decorated on MoS₂ nanosheet by chemical reduction. The as-prepared Cu-MoS₂ hybrid was characterized by atomic force microscope (AFM), Raman spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and then used to fabricate a non-enzymatic glucose sensor. The performance of our sensor was investigated by cyclic voltammetry and amperometric measurement in alkaline media. Electrochemical tests showed that Cu-MoS₂ hybrid exhibited synergistic electrocatalytic activity on the oxidation of glucose with a high sensitivity of 1055 μA mM⁻¹ cm⁻² and a linear range up to 4 mM.     

Spectroscopic properties of B2O3–PbO–Bi2O3–GeO2 glass doped with Sm3+ and gold nanoparticles

Heavy metal oxide B₂O₃–PbO–Bi₂O₃–GeO₂ transparent glass doped with Sm³⁺ was synthesized and implanted with Au⁺ using energy of 300 keV and fluence of 1 × 10¹⁶ cm⁻². The annealing of the implanted glass at moderate temperature below the glass transition temperature induced the nucleation of gold nanoparticles, confirmed by the characteristic absorption band in the visible range and by transmission electron microscopy. Using Miés and Doylés theories for the surface plasmon resonance, the average size of the gold nanoparticles was about 4.6 nm, similar to the values observed by transmission electron microscopy. It was also observed the crystallization of a thin layer of the glass at the implanted surface after annealing, detected by X-ray diffraction and scanning electron microscope. Visible and near-infrared emission of Sm³⁺ was enhanced after annealing of the glass implanted with gold. Judd–Ofelt parameters and radiative parameters were calculated for the glass doped with Sm³⁺ with and without gold nanoparticles.     

Cu doped ZnO nanoparticle sheets

Cu doped ZnO nanoparticle sheets were synthesized via a proposed solution route with mixed Zn(NO₃)₂ and Cu(NO₃)₂ precursors at a low temperature of 95 °C. Scanning electron microscopy, transmission electron microscopy, and X-ray energy dispersive spectrometry results demonstrate that the nanostructues synthesized by solutions with higher Cu(NO₃)₂ concentration are nanoparticle sheets comprised of uniform Cu doped ZnO nanoparticles with diameters around 20 nm. Room-temperature photoluminescence spectra of the nanoparticle sheets show tunable near band emissions centered at 390–405 nm and strong yellow emissions at 585–600 nm. Absorbance spectra show gradual redshift in the UV range with the increase of Cu concentrations in the ZnO nanomaterials. The study provides a simple and efficient route to prepare Cu doped ZnO nanomaterials at low temperature. The as-synthesized products with both violet and yellow emissions are promising for white light-emitting diode applications.     

Preparation and characterization of copper nanoparticles/zinc oxide composite modified electrode and its application to glucose sensing

We report a new method for selective detection of d(+)-glucose using a copper nanoparticles (Cu-NPs) attached zinc oxide (ZnO) film coated electrode. The ZnO and Cu-NPs were electrochemically deposited onto indium tin oxide (ITO) coated glass electrode and glassy carbon electrode (GCE) by layer-by-layer. In result, Cu-NPs/ZnO composite film topography was characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM), respectively. SEM and AFM confirmed the presence of nanometer sized Cu-NPs/ZnO composite particles on the electrode surface. In addition, X-ray diffraction pattern revealed that Cu-NPs and ZnO films were attached onto the electrode surface. Indeed, the Cu-NPs/ZnO composite modified electrode showed excellent electrocatalytic activity for glucose oxidation in alkaline (0.1 M NaOH) solution. Further, we utilized the Cu-NPs/ZnO composite modified electrode as an electrochemical sensor for detection of glucose. This glucose sensor showed a linear relationship in the range from 1 × 10^? 6 M to 1.53 × 10^? 3 M and the detection limit (S/N = 3) was found to be 2 × 10^? 7 M. The Cu-NPs/ZnO composite as a non-enzymatic glucose sensor presents a number of attractive features such as high sensitivity, stability, reproducibility, selectivity and fast response. The applicability of the proposed method to the determination of glucose in human urine samples was demonstrated with satisfactory results.     

Performance evaluation of ZnO–CuO hetero junction solid state room temperature ethanol sensor

A semiconductor ethanol sensor was developed using ZnO–CuO and its performance was evaluated at room temperature. Hetero-junction sensor was made of ZnO–CuO nanoparticles for sensing alcohol at room temperature. Nanoparticles were prepared by hydrothermal method and optimized with different weight ratios. Sensor characteristics were linear for the concentration range of 150–250 ppm. Composite materials of ZnO–CuO were characterized using X-ray diffraction (XRD), temperature-programmed reduction (TPR) and high-resolution transmission electron microscopy (HR-TEM). ZnO–CuO (1:1) material showed maximum sensor response (S = R_air/R_alcohol) of 3.32 ± 0.1 toward 200 ppm of alcohol vapor at room temperature. The response and recovery times were measured to be 62 and 83 s, respectively. The linearity R² of the sensor response was 0.9026. The sensing materials ZnO–CuO (1:1) provide a simple, rapid and highly sensitive alcohol gas sensor operating at room temperature.     

Microwave-assisted method for preparation of Zn1−xMgxO nanostructures and their activities for photodegradation of methylene blue

Nanostructures of Zn_1−xMg_xO (0 ⩽ x ⩽ 0.2) were prepared in water by one-pot method under microwave irradiation for 5 min. In this method, zinc acetate, magnesium nitrate and sodium hydroxide were used as starting materials without using any additive and post preparation treatment. The nanostructures were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS), diffuse reflectance spectroscopy (DRS), electrochemical impedance spectroscopy (EIS), Fourier transform-infrared (FT-IR), and the Brunauer–Emmett–Teller (BET) techniques. The nanostructures have wurtzite hexagonal crystalline phase and doping of Mg²⁺ ions does not change the phase of ZnO. The SEM and TEM images show that morphology of the samples is changing by doping of Mg²⁺ ions. The EIS data show that by doping the ion, interfacial charge transfer resistance of the nanostructures decreases. Photocatalytic activity of the nanostructures was evaluated by degradation of methylene blue (MB) under UV irradiation. The degradation rate constant on the nanostructures with 0.15 mol fraction of Mg²⁺ ions is about 2-fold greater than for ZnO. Moreover, influence of various operational parameters such as microwave irradiation time, calcination temperature, weight of catalyst, concentration of MB, pH of solution and scavengers of reactive species on the degradation rate constant was investigated and the results were discussed.     

Strong quantum confinement effect in nanocrystalline cerium oxide

Highly uniform and well-dispersed cerium oxide quantum dots were successfully synthesized by simple precipitation method by using cerium ammonium nitrate and ammonium hydroxide as precursor materials with suitable conditions. The X-ray diffraction pattern indicates the formation of cubic phase CeO₂. The average particle size of cerium oxide from high resolution transmission electron microscopy (HRTEM) was found to be 3 nm. The X-ray photoelectron (XPS) spectrum confirms the presence of Ce³⁺ in CeO₂. Optical studies by UV–vis spectroscopy for the synthesized CeO₂ nanoparticles exhibit a blue shift (E_g = 3.78 eV) with respect to the bulk material (E_g = 3.15 eV) due to quantum confined exciton absorption.     

Luminescence and energy transfer in Er3+/Nd3+ ion-codoped Ge–In–S–CsBr chalcohalide glasses

This study investigates the emission properties of the Er³⁺/Nd³⁺ ions codoped 70GeS₂–10In₂S₃–20CsBr chalcohalide glasses. The vacuumed melt-quenching technique is employed to synthesize the glasses. The absorption spectra, upconversion and near-IR emission spectra as well as fluorescence decay curves are collected. With the increasing concentration of Er³⁺ ions, the lifetimes at 1073 nm for Nd³⁺ ions decrease from 538 to 420 μs under 808 nm excitation. Meanwhile, the lifetimes at 1540 nm for Er³⁺ ions decrease from 245 to 214 μs with the increasing concentration of Nd³⁺ ions. The emission spectra and lifetimes show that energy transfer exists between the Nd³⁺ and Er³⁺ ions. The luminescence and detailed energy transfer mechanisms are schematically proposed.     

One step synthesis of Bi@Bi2O3@carboxylate-rich carbon spheres with enhanced photocatalytic performance

Bi@Bi₂O₃@carboxylate-rich carbon core-shell nanosturctures (Bi@Bi₂O₃@CRCSs) have been synthesized via a one-step method. The core–shell nanosturctures of the as-prepared samples were confirmed by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and Raman spectroscopy. The formation of Bi@Bi₂O₃@CRCSs core–shell nanosturctures should attribute to the synergetic roles of different functional groups of sodium gluconate. Bi@Bi₂O₃@CRCSs exhibits significant enhanced photocatalytic activity under visible light irradiation (λ > 420 nm) and shows an O₂-dependent feature. According to trapping experiments of radicals and holes, hydroxyl radicals were not the main active oxidative species in the photocatalytic degradation of MB, but O₂⁻ are the main active oxidative species.     

The 1.53 μm spectroscopic properties of Er3+/Ce3+/Yb3+ tri-doped tellurite glasses containing silver nanoparticles

The metallic silver nanoparticles (NPs) was introduced into the Er³⁺/Ce³⁺/Yb³⁺ tri-doped tellurite glasses with composition TeO₂–ZnO–La₂O₃ to improve the 1.53 μm band fluorescence. The UV/Vis/NIR absorption spectra, 1.53 μm band fluorescence spectra, fluorescence lifetimes, X-ray diffraction (XRD) curves, differential scanning calorimeter (DSC) curves and transmission electron microscopy (TEM) image of tri-doped tellurite glasses were measured, together with the Judd–Ofelt intensity parameters, emission cross-sections, absorption cross-sections and radiative quantum efficiencies were calculated to investigate the effects of silver NPs on the 1.53 μm band spectroscopic properties of Er³⁺ ions, structural nature and thermal stability of glass hosts. It is shown that Er³⁺/Ce³⁺/Yb³⁺ tri-doped tellurite glasses can emit intense 1.53 μm band fluorescence through the combined energy transfer (ET) processes from Yb³⁺ to Er³⁺ ions and Er³⁺ to Ce³⁺ ions under the 980 nm excitation. At the same time, the introduction of an appropriate amount of silver NPs can further improve the 1.53 μm band fluorescence owing to the enhanced local electric field effect induced by localized surface Plasmon resonance (LSPR) of silver NPs and the possible energy transfer from silver NPs to Er³⁺ ions, and an improvement by about 120% of fluorescence intensity is found in the studied Er³⁺/Ce³⁺/Yb³⁺ tri-doped tellurite glass containing 0.5 mol% amount of silver NPs with average diameter of ∼15 nm. The energy transfer mechanisms from Yb³⁺ to Er³⁺ ions and Er³⁺ to Ce³⁺ ions were also quantitatively investigated by calculating energy transfer microparameters and phonon contribution ratios. Furthermore, the thermal stability of glass host increases slightly with the introduction of silver NPs while the glass structure maintains the amorphous nature. The results indicate that the prepared Er³⁺/Ce³⁺/Yb³⁺ tri-doped tellurite glass with an appropriate amount of silver NPs is an excellent gain medium applied for 1.53 μm band EDFA pumped with a 980 nm laser diode (LD).     

Effect of oxygen partial pressure on microstructural and optical properties of titanium oxide thin films prepared by pulsed laser deposition

Nanocrystalline titanium oxide (TiO₂) thin films were deposited on silicon (1 0 0) and quartz substrates at various oxygen partial pressures (1 × 10⁻⁵ to 3.5 × 10⁻¹ mbar) with a substrate temperature of 973 K by pulsed laser deposition. The microstructural and optical properties were characterized using Grazing incidence X-ray diffraction, atomic force microscopy, UV–visible spectroscopy and photoluminescence. The X-ray diffraction studies indicated the formation of mixed phases (anatase and rutile) at higher oxygen partial pressures (3.5 × 10⁻² to 3.5 × 10⁻¹ mbar) and strong rutile phase at lower oxygen partial pressures (1 × 10⁻⁵ to 3.5 × 10⁻³ mbar). The atomic force microscopy studies showed the dense and uniform distribution of nanocrystallites. The root mean square surface roughness of the films increased with increasing oxygen partial pressures. The UV–visible studies showed that the bandgap of the films increased from 3.20 eV to 3.60 eV with the increase of oxygen partial pressures. The refractive index was found to decrease from 2.73 to 2.06 (at 550 nm) as the oxygen partial pressure increased from 1.5 × 10⁻⁴ mbar to 3.5 × 10⁻¹ mbar. The photoluminescence peaks were fitted to Gaussian function and the bandgap was found to be in the range ∼3.28–3.40 eV for anatase and 2.98–3.13 eV for rutile phases with increasing oxygen partial pressure from 1 × 10⁻⁵ to 3.5 × 10⁻¹ mbar.     

Effect of annealing on the magnetic properties of solution synthesized Zn1−xMnxO nanorods

Mn-doped ZnO nanorods with ～30 nm in diameter and ～200 nm in length were synthesized by a seed-mediated solution method. The structures, magnetic properties, as well as the annealing effect were characterized by transmission electron microscopy, electron energy loss spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectrum and physical properties measurement system. Magnetic properties measurement revealed that the Zn_0.97Mn_0.03O nanorods exhibited ferromagnetism with a saturation magnetization of 0.005 emu g^?1 and a coercivity of 110 Oe at 305 K. After annealing the samples at 900 °C for 2 h in air, the nanorods were transformed into nanoparticle aggregates. The coercivity and saturation magnetization increased obviously. Detailed analyses proved that a phase-separation process was happened at the high temperature. In this process, most of the particles preserved the wurtzite ZnO structure, while a few small ones evolved into spinel-structured particles. The increasing of the ferromagnetism of the annealed sample is attributed to the formation of secondary phase Zn_xMn_3?xO_4.     

Microwave-assisted hydrothermal synthesis of zinc oxide particles starting from chloride precursor

Zinc oxide (ZnO) was synthesized using a microwave assisted hydrothermal (MAH) process based on chloride/urea/water solution and under 800 W irradiation for 5 min. In the bath, Zn²⁺ ions reacted with the complex carbonate and hydroxide ions to form zinc carbonate hydroxide hydrate (Zn₄CO₃(OH)₆·H₂O), and the conversion from Zn₄CO₃(OH)₆·H₂O to ZnO was synchronously achieved by a MAH process. The as-prepared ZnO has a sponge-like morphology. However, the initial sponge-like morphology of ZnO could change to a net-like structure after thermal treatment, and compact nano-scale ZnO particles were finally obtained when the period of thermal treatment increased to 30 min. Pure ZnO nanoparticles was obtained from calcination of loose sponge-like ZnO particles at 500 °C. The analysis of optical properties of these ZnO nanoparticles showed that the intensity of 393 nm emission increased with the calcination temperature because the defects were reduced and the crystallinity was improved.     

Effects of deposition temperature and chemical composition on the ZnO crystal growth on the surface of Pd catalyst through electroless chemical reaction

Zinc oxide (ZnO) was site-selectively grown on the palladium (Pd) catalyst through the electroless deposition process under mild conditions, and the effects of deposition temperature and chemical composition on the ZnO crystal growth were investigated. ZnO crystals were synthesized on the UV-patterned Pd catalysts in the aqueous solutions of various dimethylamine borane (DMAB)/Zn(NO₃)₂ ratio at 30–70 °C. The site-selective deposition was confirmed by X-ray photoelectron spectroscopy (XPS) data and elemental maps of Pd, Zn and oxygen in energy-filtering transmission electron microscopy (EFTEM), and the crystal morphology was observed by scanning electron microscopy (SEM). A strong near band emission at around 390 nm and a weak green emission at around 470 nm were observed in the photoluminescence (PL) spectrum. The ZnO crystals were grown in the following three steps: (1) ZnO fibrils were generated on the Pd catalysts and became sphere-like particles, (2) hexagonal wurtzite crystals initiated to grow from the sphere-like particles, and (3) the crystals grew in two directions—longitudinal and lateral growths giving rod-type or needle-type hexagonal crystals. It was found that longitudinal growth rate increased with increasing deposition temperature or DMAB/Zn(NO₃)₂ ratio.     

Hydrothermal synthesis and luminescence properties of hierarchical SrF2 and SrF2:Ln3+ (Ln = Er,Nd, Yb,Eu, Tb) micro/nanocomposite architectures

Highly uniform SrF₂ and SrF₂:Ln³⁺ (Ln = Er, Nd, Yb, Eu, Tb) hierarchical microspheres assembled by 2D nanoplates have been successfully synthesized by a facile and friendly hydrothermal route. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and photoluminescence (PL) spectra were used to characterize the samples. The experimental results indicate that reaction time and chelating reagent play a key role in forming the hierarchical microspheres. The formation mechanism was proposed based on the evolution of this morphology as a function of hydrothermal time. The near-infrared luminescence of lanthanide ions (Er, Nd, and Yb) doped SrF₂ microspheres were discussed in detail. In addition, the as-obtained SrF₂:Eu³⁺ sample exhibits orange-red emission centered at 590 nm under excitation at 393 nm, while the SrF₂:Tb³⁺ exhibits a strong green emission at 540 nm. The as-synthesized SrF₂:Ln³⁺ luminescent microspheres might find some potential applications in areas of photoluminescence, telecommunication and laser emission.     

Fluorescence properties and relaxation processes of Tb3+ ions in ZnCl2-based glasses

60ZnCl₂–20KCl–20BaCl₂–xTbCl₃ glasses (x = 0.10, 0.25, 0.50, 0.75, 1.00, and 1.25) were prepared by melt-quenching method, and Tb³⁺ fluorescence properties were investigated under 355 nm excitation. Regardless of x values, the electrons that were relaxed from the ⁵D₃ to ⁵D₄ level of Tb³⁺ ions by the multiphonon relaxation, were repressed to 28% of all the excited electrons because the ZnCl₂-based glass had much lower phonon energy than oxide glasses. For 0 < x ≤ 0.34, the cross relaxation, (⁵D₃ → ⁵D₄) → (⁷F₀ ← ⁷F₆), was repressed, and consequently 72% and 28% of all the excited electrons were radiatively relaxed by the ⁵D₃ → ⁷F_J (J = 6, 5, 4, 3, and 2) and ⁵D₄ → ⁷F_J (J = 6, 5, 4, and 3) transitions, respectively. The lifetimes of the ⁵D₃ and ⁵D₄ initial levels were obtained to be 1.1 and 2.1 ms, respectively.     

Structural and photoluminescent properties of Al2O3: Cr3+ nanoparticles via solution combustion synthesis method

In the present work, we have discussed the structural and photoluminescent properties of Al₂O₃ nanoparticles doped with Cr³⁺ ion prepared through solution combustion synthesis (SCS) technique. SCS is a well-known method for the production of different metal oxides and composite materials such as metal matrix composites and for producing this need an extra reduction step. The set of samples differing in activator concentration were studied carefully by means of structural and optical characterization methods. In particular, the transmission electron microscopy (TEM) has been deployed together with X-ray diffraction (XRD) technique to determine fundamental structural properties of nanoparticles. XRD results showed that pure α-Al₂O₃ single phase was obtained and TEM result indicates that nanoparticles are spherical in shape. The selected area electron diffraction (SAED) and Energy dispersive analysis by X-rays (EDAX) analysis suggested the crystallinity and chemical composition of the Cr³⁺ doped Al₂O₃. The change in crystal structure parameters was obtained by Rietveld refinement method. The optical characterization focused mainly on the basic excitation and emission features and their sensitivity to the dopant concentrations. The excitation spectrum of Cr³⁺-doped Al₂O₃ nanopowders consist of two bands peaking at 406 nm and 570 nm and the emission spectrum consist of two bands peaking at 694 nm and 670 nm.     

Effect of Nd3+ incorporation on the microstructure and chemical structure of RF sputtered ZnO thin films

The present work aims at investigating the effects that different levels of Nd atoms incorporation can have on the microstructure and chemical structure of ZnO thin films. Undoped and Nd-doped ZnO films were deposited by RF co-sputtering from pure ZnO and metallic Nd targets in Ar plasma onto Si, quartz and glass substrates. The Nd concentration in the ZnO host matrix was varied in the range 0–26 at.% by varying the bias applied to the Nd target. A comprehensive characterization of the films properties was performed by X-ray photoelectron and Auger electron spectroscopies, X-ray fluorescence analysis, X-ray diffraction and scanning electron microscopy. At low Nd atomic concentration (Nd/Zn < 0.07) Nd atoms were successfully incorporated into the ZnO matrix, whose crystalline structure was preserved. A deterioration of the ZnO würtzite phase was observed on the contrary with increasing Nd content in the films together with the precipitation of a second phase, identified as Nd₂O₃.     

Effect of processing parameters on structural,morphological and optical Y2O3:Yb3+/Ho3+ powders characteristics

Rod-like and flake-like up-converting Y₂O₃:Yb³⁺/Ho³⁺ particles which are composed of nanoparticles with size less than 100 nm, are prepared by a simple hydrothermal processing at 473 K (3 h) followed by additional thermal treatment at 1373 K (3 and 12 h). The effect of precursor pH value on the formation of Y₂O₃:Yb³⁺/Ho³⁺ is followed through X-ray powder diffractometry (XRPD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Structural refinement confirms formation of the cubic bixbyte structure (S.G. Ia-3) with the non-uniform accommodation of dopants at C₂ and S₆ cationic sites. Under 978 nm laser excitation, strong green (530–570 nm) up-conversion is observed in all samples. The emission shows a decrease in intensity with an increase in external temperature, indicating FIR (fluorescence intensity ratio) based temperature sensing behavior of 0.52% for the ⁵F₄ → ⁵I₈/⁵S₂ → ⁵I₈ transitions.