Thermal evaporation and condensation synthesis of metallic Zn layered polyhedral microparticles

Metallic zinc layered polyhedral microparticles have been fabricated by thermal evaporation and condensation technique using zinc as precursor at 750 °C for 120 min and NH₃ as a carrier gas. The zinc polyhedral microparticles with oblate spherical shape are observed to be 2-9 μm in diameter along major axes and 1-7 μm in thickness along minor axes. The structural, compositional and morphological characterizations were performed by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). A vapour-solid (VS) mechanism based growth model has been proposed for the formation of Zn microparticles. Room temperature photoluminescence (PL) emission spectrum of the product exhibited a strong emission band at 369 nm attributed to the radiative recombination of electrons in the s, p conduction band near Fermi surface and the holes in the d bands generated by the optical excitation.     

Synthesis of metallic Zn microprisms, their growth mechanism and PL properties

Novel metallic Zn hexagonal hollow microprisms have been synthesized by a simple thermal evaporation technique using NH₃ as a carrier gas under atmospheric pressure. As-prepared hollow microprisms were characterized using X-ray diffraction, energy dispersive X-ray spectroscopy, scanning electron microscopy and transmission electron microscopy. The hollow microprisms collected on silicon substrate are found to be 3-7 μm long with diameter in the range 900-950 nm. A vapour-solid (VS) process based growth mechanism has been proposed for the formation of hexagonal Zn microprisms grown along (0001) basal plane in [0001] direction. Photoluminescence (PL) emission spectrum of zinc microprisms at room temperature exhibited a very prominent peak at 384 nm owing to the radiative recombination of electrons in s, p conduction band near Fermi surface and the holes in the d bands generated by optical excitation.     

Synthesis and optical properties of single-crystalline GaN nanorods

Single-crystalline GaN nanorods were successfully synthesized on Si(1 1 1) substrates through ammoniating Ga₂O₃/Mo films deposited on the Si(1 1 1) substrate by radio frequency magnetron sputtering technique. The as-synthesized nanorods are confirmed as single-crystalline GaN with wurtzite structure by X-ray diffraction (XRD), selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM). Scanning electron microscopy (SEM) displays that the GaN nanorods are straight and smooth with diameters in the range of 100-200 nm and lengths typically up to several micrometers. X-ray photoelectron spectroscopy (XPS) confirms the formation of bonding between Ga and N. The representative photoluminescence spectrum at room temperature exhibits a strong and broad emission band centered at 371.1 nm, attributed to GaN band-edge emission. The growth process of GaN nanorod may be dominated by vapor-solid (VS) mechanism.     

Green hydrothermal synthesis and photoluminescence property of ZnO2 nanoparticles

ZnO₂ nanoparticles were synthesized via a green hydrothermal method using ZnO powder and 30% H₂O₂ aqueous solution as the starting materials, and characterized by X-ray diffraction (XRD), Raman spectra, energy dispersive X-ray (EDX) spectra, field emission scanning electron microscope (FESEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and room temperature photoluminescence (RTPL) spectra. It was found that suitable reaction temperature (e.g., 80-140 °C) played an important role in obtaining pure cubic phase ZnO₂ nanoparticles. The RTPL spectra disclosed that the as-synthesized ZnO₂ nanoparticles exhibit one strong emission band centered at around 400 nm and one very weak emission band at around 474 nm, which may have originated from the band edge emission and the oxygen vacancy, respectively.     

Optical properties of nanocrystalline SnS2 thin films

Thin films of nanocrystalline SnS₂ on glass substrates were prepared from solution by dip coating and then sulfurized in H₂S (H₂S:Ar = 1:10) atmosphere. The films had an average thickness of 60 nm and were characterized by X-ray diffraction studies, scanning electron microscopy, EDAX, transmission electron microscopy, UV-vis spectroscopy, and Raman spectroscopy. The influence of annealing temperature (150-300 °C) on the crystallinity and particle size was studied. The effect of CTAB as a capping agent has been tested. X-ray diffraction analysis revealed the polycrystalline nature of the films with a preferential orientation along the c-axis. Optical transmission spectra indicated a marked blue shift of the absorption edge due to quantum confinement and optical band gap was found to vary from 3.5 to 3.0 eV with annealing temperature. Raman studies indicated a prominent broad peak at ∼314 cm⁻¹, which confirmed the presence of nanocrystalline SnS₂ phase.     

Large-scale synthesis of highly pure Cd metal hexagonal nanosheets

Highly pure and large-scale single crystalline cadmium (Cd) metal hexagonal nanosheets with 10-12 nm thickness were obtained by catalyst-free thermal decomposition of cadmium oxide (CdO) powder under nitrogen gas at 1000 °C. The as-prepared product was characterized by X-ray diffraction, energy dispersive X-ray spectroscopy, scanning electron microscopy, transmission electron microscopy and selected area electron diffraction. Room temperature photoluminescence (PL) spectrum for Cd nanosheets exhibited three very distinct emission bands at 360 nm, 402 nm and 426 nm. UV emission band at 360 nm is attributed to radiative recombination of electrons in the s, p conduction band near the Fermi surface and the holes in the d bands generated by xenon light excitation whereas visible emission bands at 402 nm and 426 nm may be due to surface oxidation effects or induced defects in the nanosheets. The growth mechanism for the formation of Cd metal hexagonal nanosheets is also proposed and discussed briefly.     

Structure and optical spectrum of GaN nanorods produced on Si(111) substrates

A novel method is applied to prepare nanorods. In this method, nanorods have been successfully synthesized on Si(111) substrates through annealing sputtered Ga₂O₃/Nb films under flowing ammonia at 950 °C in a quartz tube. The as-synthesized nanorods are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectra. The results show that the nanorod is single-crystalline GaN. It has a diameter of about 200 nm and lengths typically up to several micrometers. Photoluminescence spectrum under excitation at 325 nm only exhibits a UV light emission peak is located at about 368.5 nm. Finally, the growth mechanism of nanorods is also briefly discussed.     

Synthesis and luminescent properties of ZnNb2O6 nanocrystals for solar cell

The phase formation, morphology and luminescent properties of ZnNb₂O₆ nanocrystals by the sol-gel method were investigated at a lower temperature than that of the traditional solid-state reaction method. The products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), photoluminescence spectroscopy (PL) and absorption spectra. The activation energy of ZnNb₂O₆ grain growth is obtained about 18.4 kJ/mol. The diameters of the nanocrystals are in the range of 20-40 nm. The PL spectra excited at 276 nm have a broad and strong blue emission band maximum at 450 nm, corresponding to the self-activated luminescence of the niobate octahedra group [NbO₆]⁷⁻. The optical absorption spectrum of the sample at a calcination temperature of 800 °C has a band gap energy of 3.68 eV.     

Fabrication of metallic Cd multifarious prismatic microcrystals (CMPMCs) under NH3 gas ambient

We report here highly dense and pure metallic cadmium (Cd) multifarious prismatic microcrystals (CMPMCs) fabricated by thermal decomposition of cadmium oxide (CdO) powder at 700 °C for 60 min under NH₃ gas ambient inside horizontal tube furnace. CMPMCs were observed to be 1-1.5 μm in size with interesting morphologies of various cross sections such as triangular, trapezoidal, pentagonal and hexagonal etc. having solid, hollow/semi-hollow appearances. The as-synthesized CMPMCS were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) and selected area electron diffraction (SAED). Room temperature photoluminescence (PL) spectrum for Cd metal microcrystals exhibited a prominent emission band at 365 along with a shoulder peak at 404 nm. The UV main emission band is ascribed to radiative recombination of the electrons in the s, p conduction band near the Fermi surface and holes in the d bands generated under xenon light excitation whereas shoulder peak may be owing to surface oxidation effects or induced defects. This study shows the potential of CMPMCs for applications in optical devices. Based on vapour-solid (VS) process, growth mechanism for the formation of CMPMCs is also proposed and discussed briefly.     

Synthesis of ZnO flowers and their photoluminescence properties

Flower-like ZnO nano/microstructures have been synthesized by thermal treatment of Zn(NH₃)₄²⁺ precursor in aqueous solvent, using ammonia as the structure directing agent. A number of techniques, including X-ray diffraction (XRD), field emission scan electron microscopy (FESEM), transmission electron microscopy (TEM), thermal analysis, and photoluminescence (PL) were used to characterize the obtained ZnO structures. The photoluminescence (PL) measurements indicated that the as-synthesized ZnO structures showed UV (∼375 nm), blue (∼465 nm), and yellow (∼585 nm) emission bands when they were excited by a He-Gd laser using 320 nm as the excitation source. Furthermore, it has been interestingly found that the intensity of light emission at ∼585 nm remarkably decreased when the obtained ZnO nanocrystals were annealed at 600 °C for 3 h in air. The reason might be the possible oxygen vacancies and interstitials in the sample decreased at high temperature.     

Silver nanoparticles: Large scale solvothermal synthesis and optical properties

Silver nanoparticles have been successfully synthesized by a simple and modified solvothermal method at large scale using ethanol as the refluxing solvent and NaBH₄ as reducing agent. The nanopowder was investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), dynamic light scattering (DLS), UV-visible and BET surface area studies. XRD studies reveal the monophasic nature of these highly crystalline silver nanoparticles. Transmission electron microscopic studies show the monodisperse and highly uniform nanoparticles of silver of the particle size of 5 nm, however, the size is found to be 7 nm using dynamic light scattering which is in good agreement with the TEM and X-ray line broadening studies. The surface area was found to be 34.5 m²/g. UV-visible studies show the absorption band at ∼425 nm due to surface plasmon resonance. The percentage yield of silver nanoparticles was found to be as high as 98.5%.     

CuSn(OH)6 submicrospheres: Room-temperature synthesis and weak antiferromagnetic behavior

CuSn(OH)₆ submicrospheres with a diameter of 400-900 nm, which are composed of nanoparticles with a size of about 27.8 nm, have been successfully synthesized for the first time via a simple liquid approach at room temperature in 15 min. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were used to characterize the products. Standard magnetization measurements at low temperature reveal that the as-obtained CuSn(OH)₆ submicrospheres are antiferromagnetic and have a weak spin-Peierls transition at about 78 K.     

Green hydrothermal synthesis and optical absorption properties of ZnO2 nanocrystals and ZnO nanorods

A green hydrothermal method was proposed for the controllable synthesis of ZnO₂ nanocrystals and ZnO nanorods, using the common and cost-effective 2ZnCO₃·3Zn(OH)₂ powder and 30 mass% H₂O₂ aqueous solution as the raw materials. The characterization results from X-ray diffraction, high resolution transmission electron microscopy, transmission electron microscopy and energy dispersive X-ray spectroscopy indicated that the products synthesized at 100-120 °C for 6 h or at 170 °C for 0 h were cubic phase ZnO₂ nanocrystals; while those synthesized at 170 °C for 3-6 h were hexagonal phase ZnO nanorods. The UV-vis absorption spectra showed that the as-synthesized ZnO₂ nanocrystals and ZnO nanorods had optical band gaps of about 4.1 and 3.3 eV, respectively.     

Synthesis of AgBr/ZnO nanocomposite with visible light-driven photocatalytic activity

AgBr/ZnO nanocomposite was synthesized via chemical precipitation from pure ZnO nanowires, AgNO₃, and NaBr. Inductively coupled plasma optical emission spectroscopy, X-ray diffraction, and high resolution transmission electron microscopy results confirmed the forming of AgBr/ZnO nanocomposite. High resolution transmission electron microscopy results of the as-synthesized AgBr/ZnO nanocomposite revealed that AgBr nanoparticles were attached to the surface of ZnO nanowires. UV-vis diffuse reflectance spectra of both pure ZnO and AgBr/ZnO nanocomposite displayed a band gap edge at about 350-380 nm. However, compared with pure ZnO, an additional broad tail from approximately 400 nm to 700 nm appeared in the UV-vis diffuse reflectance spectrum of AgBr/ZnO nanocomposite. The photocatalytic studies indicated that the as-synthesized AgBr/ZnO nanocomposite was a kind of promising photocatalyst in remediation of water polluted by some chemically stable azo dyes under visible light.     

Monodisperse ceria nanospheres: Synthesis,characterization, optical properties,and applications in wastewater treatment

Monodisperse ceria nanospheres have been synthesized by a facile solvothermal method, and their morphology and microstructures have been revealed by a combination of X-ray diffraction (XRD), scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy and N₂ adsorption. It is demonstrated that the as-synthesized powders are highly uniform CeO₂ in spherical shape with cubic fluorite structure. HRTEM and XRD studies show that each ceria nanosphere is composed of dozens of nanocrystals with the average size of 8.5 nm. The direct optical band gap of the ceria nanospheres estimated from the ultraviolet–visible absorption spectrum is 2.7 eV, which is evidently red-shifted with respect to the bulk material (E_g = 3.19 eV); the reduced band gap could be resulted from the high concentration of grain boundaries and defects present in the ceria nanospheres. In addition, the ceria nanospheres exhibit a strong blue luminescence at 504 nm and a broad orange luminescence centered at 645 nm. As a result of the large specific surface area, ceria nanospheres are revealed to be an excellent sorbent for the removal of poisonous pollutants present in water, such as chromium ions and rhodamine B. The removal efficiency of chromium ions is as high as ∼94%.     

Synthesis, characterization and optical properties of sheet-like ZnO

Sheet-like ZnO with regular hexagon shape and uniform diameter has been successfully synthesized through a two-step method without any metal catalyst. First, the sheet-like ZnO precursor was synthesized in a weak alkaline carbamide environment with stirring in a constant temperature water-bath by the homogeneous precipitation method, then sheet-like ZnO was obtained by calcining at 600 °C for 2 h. The structures and optical properties of sheet-like ZnO have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), photoluminescence (PL) and UV-vis-NIR spectrophotometer. The results reveal that the product is highly crystalline with hexagonal wurtzite phase and has appearance of hexagon at (0 0 0 1) plane. The HRTEM images confirm that the individual sheet-like ZnO is single crystal. The PL spectrum exhibits a narrow ultraviolet emission at 397 nm and a broad visible emission centering at 502 nm. The band gap of sheet-like ZnO is about 3.15 eV.     

Sub-2 nm SnO2 nanocrystals: A reduction/oxidation chemical reaction synthesis and optical properties

A simple reduction/oxidation chemical solution approach at room temperature has been developed to synthesize ultrafine SnO₂ nanocrystals, in which NaBH₄ is used as a reducing agent instead of mineralizers such as sodium hydroxide, ammonia, and alcohol. The morphology, structure, and optical property of the ultrafine SnO₂ nanocrystals have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD), differential scanning calorimetry and thermogravimetric analysis (DSC-TGA), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy. It is indicated that the uniform tetragonal ultrafine SnO₂ nanocrystals with the size below 2 nm have been fabricated at room temperature. The band gap of the ultrafine SnO₂ nanocrystals is about 4.1 eV, exhibiting 0.5 eV blue shift from that of the bulk SnO₂ (3.6 eV). Furthermore, the mechanism for the reduction/oxidation chemical reaction synthesis of the ultrafine SnO₂ nanocrystals has been preliminary presented.     

Synthesis and characterization of tin disulfide hexagonal nanoflakes via solvothermal decomposition

Tin disulfide (SnS₂) hexagonal flakes with diameters in the range of 50−150 nm are synthesized by using SnCl₂.2H₂O and sodium diethyldithiocabamate as source materials via a solvothermal decomposition route. As-prepared SnS₂ hexagonal nanoflakes are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS) and ultraviolet-visible (UV-vis) spectroscopy. The band gap energy of the SnS₂ nanoflakes is measured to be 2.17 eV, and the conduction band (CB) and valence band (VB) levels of the SnS₂ nanoflakes are calculated to be − 4.34 eV and − 6.55 eV respectively, showing them to be suitable for optional and electronic applications.     

Green hydrothermal synthesis and characterization of CdO2 nanoparticles

A green hydrothermal method has been developed for the synthesis of CdO₂ nanoparticles from Cd(OH)₂ powder and 6 vol.% H₂O₂ aqueous solution at 80-150 °C. The characterization results from X-ray diffraction, transmission electron microscopy, and thermal gravimetric and differential scanning calorimetry analysis disclosed that the resultant products were pure cubic phase CdO₂ nanoparticles with the sizes in the range of about 11-13 nm. The UV-vis absorption spectra revealed that the as-synthesized CdO₂ nanoparticles had similar optical band gaps of about 3.85 eV. The Raman spectra of the as-synthesized CdO₂ nanoparticles displayed two obvious peaks at about 348 and 830/833 cm^-1, a characteristic of pyrite-type IIB-peroxides.     

Hot-injection synthesis and characterization of quaternary Cu2ZnSnSe4 nanocrystals

Cu₂ZnSnSe₄ (CZTSe) is one of promising materials in the use of absorber layers of solar cells. It contains earth-abundant elements of zinc and tin, a near-optimal direct band gap of ∼ 1.5 eV, as well as a large absorption coefficient ∼ 10⁴ cm-1. The CZTSe nanocrystals in oleylamine (OLA) was successfully prepared via hot-injection method. The characterization of its structure, composition, morphology and absorption spectra were done using powder X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) and UV-vis absorption spectra. The results revealed that the monodispersed nanocrystals were single phase polycrystalline within the range of 15-20 nm. Optical measurements showed a direct band gap of 1.52 eV, which was optimal for low cost solar cells. The capping property of OLA was also demonstrated by examining Fourier Transform Infrared Spectroscopy (FTIR) feature peaks of CZTSe and OLA, respectively.