Size-controllable synthesis of spherical ZnO nanoparticles: Size- and concentration-dependent resonant light scattering

A new and simple direct precipitation method assisted with ultrasonic agitation was proposed for the preparation of spherical ZnO nanoparticles. The size of the ZnO nanoparticles, 10 nm to 85 nm, was tuned through controlling the calcination temperature and changing the ratio of the reactants. The resonant light scattering (RLS) of the ZnO nanoparticles dispersed/suspended in aqueous solution of Triton X-100 was studied under room temperature. It was found that the ZnO nanoparticles of different size or concentration all have a characteristic RLS peak at 387 nm. Under optimal conditions, the RLS intensity was proportional to the ZnO concentration in the range of 7.3 × 10^?8–1 × 10^?4 mol L^?1, while the cubic root of the RLS intensity was found to be proportional to the size of ZnO nanoparticles. Further, the quantitative relationship of the size of the ZnO nanoparticles versus the calcination temperature was derived, and this could be used to forecast/control the nano-size in the nano-ZnO preparation.     

Biosynthesized CuO nano-platelets: Physical properties & enhanced thermal conductivity nanofluidics

This contribution reports for the first time, room temperature biosynthesis of p-type CuO nanoparticles carried out using Callistemon viminalis’ flower extracts as a chelating agent in a process that is entirely green. Room temperature X-ray diffraction, attenuated IR total reflection spectroscopy, X-ray photoelectron and Raman spectroscopy investigations confirmed the formation of single phase Tenorite bcc monoclinic CuO nanocrystals post annealing in air, at 500 °C. Photoluminescence spectroscopy with UV emissions at 356 nm (3.47 eV) and broad visible emissions at 418 nm, 561 nm, and 664 nm, support the formation in air, at 200 °C, of CuO nanoparticles with high surface-to-volume ratios and defects. As a direct application, the biosynthesized CuO nanoplatelet-containing powder dispersed in de-ionized water showed an enhancement of the thermal conductivity from 6% to 34% and a significant stability of the PVP stabilized CuO-water nanofluid.     

Annealing effects on the morphology and luminescence of cubic boron nitride based ceramics

Cubic boron nitride based ceramics with silicon were sintered at 1350 °C under a pressure of 5.0 GPa. The effects of post-annealing on grain morphology, surface morphology, and photoluminescence of Si–cBN ceramics were investigated by scanning electron microscope and room temperature photoluminescence measurements. The results showed that the annealing treatment had great influence on cBN grain morphology, rather than the surface morphology. The luminescence intensity increased with annealing temperature and annealing time. The void-net structure formed by continuous distribution of SiO_x particulate on the ceramic surface resulted in the emission band peaking at about 701.2 nm, and the tense passivation of Si by SiO_x led to the peak's low intensity. The near ultraviolet emission band peaking at about 317 nm was attributed to the oxygen vacancies formed in cBN grain surface, caused by the scavenging of oxygen from the cBN grain surface by the added Si.     

Nb2O5 nanobelts: A lithium intercalation host with large capacity and high rate capability

In this study, Nb₂O₅ nanobelts, with a ca. ∼15 nm in thickness, ca. ∼60 nm in width and several tens of mircrometers in length, have first been used as the electrode material for lithium intercalation over the potential window of 3.0–1.2 V (vs. Li⁺/Li). It delivers an initial intercalation capacity of 250 mA hg⁻¹ at 0.1 Ag⁻¹ current density, corresponding to x = 2.5 for L_xNb₂O₅, and can still keep relative stable and reaches as large as 180 mA hg⁻¹ after 50 cycles. Surprisingly, the electrodes composed of Nb₂O₅ nanobelts can work smoothly even at high current density of 10 Ag⁻¹, and shows higher specific capacity and excellent cycling stable, as well as sloped feature in voltage profile. Cycling test indicates Nb₂O₅ nanobelts electrode shows a high reversible charge/discharge capacity, high rate capability with excellent cycling stability.     

Electrochemical impedance spectroscopy of ZnO nanostructures

The paper reports on the use of electrochemical impedance spectroscopy to determine the doping character and carrier density of freshly prepared and annealed ZnO nanostructures. The ZnO nanostructures were obtained by chemical oxidation of metallic Zn in a 5% N,N-dimethylformamide (DMF) aqueous solution at 95 °C for 24 h. The as-grown nanostructured ZnO samples display a high donor density of 3.71 ± 0.88 × 10²¹ cm^?3. Annealing at 100 and 200 °C did not have any effect on the donor density while thermal annealing at 300 °C in air for 1 h induced a decrease in the doping concentration without affecting the surface morphology.     

Growth and characterization of naphthalene single crystals grown by modified vertical Bridgman method

The large size 20 mm diameter naphthalene single crystals were grown by modified vertical Bridgman method. The optical quality of the grown crystal was analyzed by photoluminescence and ultraviolet visible absorption spectral measurements. Photoluminescence spectrum indicated violet emission at 410 nm. The UV–vis absorption spectrum shows the maximum at 219.32 nm. The microhardness measurements and differential thermal analysis performed to analyze the mechanical and thermal stability of the as grown crystals. The dielectric measurements were carried out at five frequencies, viz., 100 Hz, 1 kHz, 10 kHz, 100 kHz and 1 MHz and at various temperatures, ranging from 308 K to 348 K indicate an increase of the dielectric parameters with the increase of temperature at all the five frequencies. The conductivity of the material is understood to be more of electronic in nature. Also, the increase in the dielectric parameters with that of temperature is due to the temperature variation of electronic polarizability.     

Al-doped ZnO powdered materials: Al solubility limit and IR absorption properties

Al-doped ZnO powder was synthesized via the Pechini route with a doping rate varying from 1 to 4 mol.%. A solubility limit has been estimated under 0.3 mol.% of Al using X-ray diffraction refinements. The incorporation of aluminium into the ZnO lattice was investigated by ²⁷Al NMR, which suggests an extremely low amount of Al in a distribution of sites in ZnO. In order to assess the impact of such a low dopant amount, diffuse reflection experiments were performed for a wavelength range from 200 to 2500 nm. If the effect of doping was negligible for samples prepared at 850 °C, annealing at 1200 °C clearly reveals enhanced IR absorption properties for the doped samples, which are similar whatever be the nominal Al content.     

Formation of nano-crystalline quartz crystals from ZnO/MgO/Al2O3/TiO2/ZrO2/SiO2 glasses

Glasses with the compositions 50.9 SiO₂ · 20.8 Al₂O₃ · (20.8 ? x) MgO· × ZnO · 3.7 TiO₂ · 3.7 ZrO₂ with x = 0, 2.3, 4.6 and 9.3 were annealed at temperatures in the range from 850 to 1100 °C. Depending on temperature, high- or low-quartz solid solutions, magnesium aluminosilicate, mullit and spinel precipitated. These glass–ceramics exhibit excellent mechanical properties and are potential candidates for applications in micromechanics or as hard disc substrate.The larger the ZnO concentration, the lower is the glass transition temperature. Also microhardnesses and Young’s moduli increased with increasing ZnO concentration. The nucleation temperature was of minor importance. To achieve good mechanical properties, the initially formed high-quartz phase must transform to the corresponding low-quartz phase. This occurs if the quartz phase contains only minor MgO or ZnO concentrations, which can be achieved by increasing the annealing times or temperature. Then MgO, ZnO and Al₂O₃ occur as separate spinel or gahnite phase.     

A new photoanode architecture of dye sensitized solar cell based on ZnO nanotetrapods with no need for calcination

We introduce a photoanode architecture in dye sensitized solar cell comprising building blocks of ZnO nanotetrapods with a mean arm diameter of 40 nm and arm lengths of 500–800 nm. This photoanode features a decent roughness factor up to 400, good network forming ability and limited electron-hopping interjunctions. Even without calcination, a power conversion efficiency up to 3.27% (under 100 mW cm^?2) has been achieved at a film thickness of 31.2 μm. The avoidance of the calcination step is an outstanding feat for flexible solar cells. We have also employed impedance spectroscopy to interpret the solar cell performance features.     

LixV2O5 nanobelts for high capacity lithium-ion battery cathodes

5–10 μm long, typically 200–300 nm wide, and several nanometers thick Li_xV₂O₅ (× ～ 0.8) nanobelts with the δ-type crystal structure were synthesized by a hydrothermal treatment of Li⁺-exchanged V₂O₅ gel. When dried at 200 °C under vacuum prior to electrochemical testing, the as-prepared nanobelts underwent the well-known δ → ε → γ-phase transition giving a mixture of ε and γ phases as a nanocomposite electrode material. Such a simple preparation procedure guarantees a yield of material with drastically enhanced initial discharge specific capacity of 490 mAh/g and great cyclability. The enhanced electrochemical performance is attributed to the complex of experimental procedures including post-synthesis treatment of the single-crystalline Li_xV₂O₅ nanobelts.     

Role of laser pre-pulse wavelength and inter-pulse delay on signal enhancement in collinear double-pulse laser-induced breakdown spectroscopy

Dual-pulse (DP) laser-induced breakdown spectroscopy (LIBS) provides significant improvement in signal intensity as compared to conventional single-pulse LIBS. We investigated collinear DPLIBS experimental performance using various laser wavelength combinations employing 1064 nm, 532 nm, and 266 nm Nd:YAG lasers. In particular, the role of the pre-pulse laser wavelength, inter-pulse delay times, and energies of the reheating pulses on LIBS sensitivity improvements is studied. Wavelengths of 1064 nm, 532 nm, and 266 nm pulses were used for generating pre-pulse plasma while 1064 nm pulse was used for reheating the pre-formed plasma generated by the pre-pulse. Significant emission intensity enhancement is noticed for all reheated plasma regardless of the pre-pulse excitation beam wavelength compared to single pulse LIBS. A dual peak in signal enhancement was observed for different inter-pulse delays, especially for 1064:1064 nm combinations, which is explained based on temperature measurement and shockwave expansion phenomenon. Our results also show that 266 nm:1064 nm combination provided maximum absolute signal intensity as compared to 1064 nm:1064 nm or 532 nm:1064 nm.     

Polyvinylpyrrolidone-assisted growth and optical properties of ZnO hexagonal bilayer disk-like microstructures

ZnO hexagonal bilayer disk-like microstructures are successfully prepared assisted with polyvinylpyrrolidone (PVP), and the photoluminescence (PL) spectrum of as-prepared ZnO samples showed a very strong ultraviolet (UV) emission at the UV region.     

Morphology of nanoporous carbon-binder domains in Li-ion batteries—A FIB-SEM study

FIB-SEM tomography is used to reconstruct the carbon-binder domain (CBD) of a LiCoO₂ battery cathode (3.9 × 5 × 2.3 μm³) with contrast enhancement by ZnO infiltration via atomic layer deposition. We calculate the porosity inside the CBD (57.6%), the cluster-size distribution with a peak at 54 nm, and the pore-size distribution with a peak at 64 nm. The tortuosities of the pore space (1.6–2.0) and the CBD (2.3–3.5) show a mild anisotropy, which is attributed to the fabrication process. A comparison to a modeled homogenous CBD reveals that clustering in the CBD decreases its electronic conductivity while increasing the ionic diffusivity. To account for the higher calculated diffusivity compared to experimental values from literature, a simple binder swelling model is implemented, suggesting a swelling of 75 vol%. The prevention of both clustering and swelling could increase the volume available for active material and therefore the energy density.     

Low temperature synthesis and characterization of rosette-like nanostructures of ZnO using solution process

Rosette-like structures of ZnO were synthesized at low temperature (60 °C) using solution process over 20 min of time. Hydroxylamine hydrochloride was used as capping agent with zinc nitrate hexahydrate and sodium hydroxide. Transition from triangular shaped plate like particles to rosette-like structure and to individual nanorods is observed with increasing refluxing temperature. Single-crystalline nature with wurtzite hexagonal phase is confirmed from transmission electron microscopic observations. Photoelectron spectroscopic measurement presented spectra close to the standard bulk ZnO, with an O 1s peak composed of surface adsorbed O–H group, O^2? in the oxygen vacancies on ZnO structure and ZnO.     

Effect of Hg2+doping and of the annealing temperature on the nanostructural properties of TiO2 thin films obtained by sol–gel method

This work is a study of Hg²⁺-doped TiO₂ thin films deposited on silicon substrates prepared by sol–gel method and treated at temperatures ranging between 600 to 1000 °C for 2 h. The structural and optical properties of thin films have been studied using different techniques. We analyzed the vibrations of the chemical bands by Fourier transform infrared (FTIR) spectroscopy and the optical properties by UV–Visible spectrophotometry (reflection mode) and photoluminescence (PL). The X-ray diffraction and Raman spectra of TiO₂ thin films confirmed the crystallization of the structure under the form of anatase, rutile, mercury titanate (HgTiO₃) as a function of the annealing temperature. The observation by scanning electron microscopy (SEM) showed the changing morphology, with respect to nanostructures, nanosheets, nanotubes, with the annealing temperature. The diameters of nanotubes ranged from 50 nm to 400 nm. The photoluminescence and reflectance spectra indicated that these structures should enhance photocatalytic activity.     

Electrolytic in situ STM investigation of h-BN-Nanomesh

Single sheet boron nitride layers on thin rhodium (1 1 1) films were formed upon thermal decomposition of borazine under ultra-high vacuum (UHV) conditions. They were transferred and investigated in an electrolytic environment. In 0.1 M HClO₄, the presence and stability of the so-called nanomesh super structure with a lattice constant of 3.2 nm is established with electrochemical impedance spectroscopy, cyclic voltammetry and subsequent imaging with in situ scanning tunneling microscopy (STM) under potential control. In the electrolyte, the BN nanomesh acts as a dielectric layer with an unusual behaviour of the impedance, where the capacitive component is larger than on a Rh(1 1 1) reference sample. It exhibits reversible hydrogen adsorption and desorption at a potential of −600 mV vs. a saturated mercury sulphate reference electrode (MSE). The unit cell of the nanomesh is imaged by STM and shows hexagonally arranged two-dimensional pores with a diameter of 2 nm. At a fixed potential, the nanomesh was stable for long time, but after repeated potential sweeps between +260 and −540 mV vs. MSE, STM indicates roughening, though a 12 × 12 superstructure was recovered after annealing in UHV.     

Synthesis and characterization of ZnO nanoparticles by thermal decomposition of a curcumin zinc complex

ZnO nanoparticles were generated by thermal decomposition of a binuclear zinc (II) curcumin complex as single source precursor. Thermal behavior of the precursor showed a considerable weight loss at about 374 °C by an exothermic reaction with a maximum weight loss rate of 14%/min. Complete decomposition of precursor was observed within 49 min with a heating rate of 10 °C/min. Synthesized nanoparticles have been characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and selected area electron diffraction microscopy. Results revealed monodispersed hexagonal zincite structure with an average size of 117 ± 4 nm.     

Electrochemical synthesis of orientation-ordered ZnO nanorod bundles

The high density and orientation-ordered ZnO nanorod bundles with wurtzite structures were prepared on Cu substrates by electrochemical deposition in solution of ZnCl₂ + tartaric acid at a temperature of 90 °C. This approach is a unique and size controlled synthetic method for the large-scale preparation of ZnO nanorod bundles. Cyclic voltammogram measured in solution of the mixture of ZnCl₂ and tartaric acid shows a restraining role of tartaric acid for the electro-reduction of Zn(II). The formation mechanism of ZnO on the surface of the cathode can be explained that the high temperature (⩾90 °C) promotes the corrosion of electrodeposited Zn via reacting with H₂O and O₂ to form the stable passive phase of ZnO. The compositions of the nanorod bundles can be entirely ZnO or Zn and ZnO composites determined by the temperature and deposition rate. The photoluminescence (PL) properties indicate that these ZnO deposits are highly crystallized and of excellent optical quality.     

Optical and Structural Properties of Zn2SiO4:Mn2+ from SLS Waste Bottle Obtained by a Solid State Method

In this studies, 2 wt.% Mn-doped Zn₂SiO₄ were synthesized from SLS waste glass, ZnO and MnO using conventional solid-state method. Structural and optical properties were examined as functions of sintering temperature. Density and linear shrinkage of samples increased with increasing in sintering temperature. X-Ray Diffraction pattern revealed that sintering temperature play an important role in enhancing crystallization of Zn₂SiO₄. It was found that the phase formation changed from amorphous to ȕ- Zn₂SiO₄ and then to α-Zn₂SiO₄ with the unsintered to sinter at 600 °C and 700 °C respectively. The morphology under FESEM characterization shows that the samples become more uniform with rectangular shape like as the sintering temperature increased. From UV-Vis spectroscopy, the results obtained showed that the intensive absorption occurred in the UV region, in the range of 250-γλ0 nm. Prominent green emission colours of α-Zn₂SiO₄ were observed centred at 527 nm while the yellow emission centred at η8η nm resulted from ȕ-Zn₂SiO at an excitation of 260 nm. However, red emission centred at 600 nm was observed for glass samples. These emissions come from the Mn-dopant and correspond to the ⁴T₁ – ⁶A₁ transition.