Enhanced photocatalytic activity of zinc oxide synthesized by calcination of zinc sulfide precursor

ZnO nanoparticles were synthesized by calcination of ZnS precursor in an air atmosphere, in which ZnS had been firstly synthesized through precipitation with sodium sulfide (Na₂S) as the precipitator. Detailed structure and morphology of the samples were characterized by X-ray diffraction, energy dispersive spectroscopy, scanning electron microscopy, and transmission electronic microscopy. Optical properties were examined by UV–vis absorption spectroscopy. Photocatalytic activities of the samples were evaluated by degradation of Reactive Blue 14 (KGL). The results indicate that ZnS precursor converted into pure ZnO stepwise via calcination at a temperature range of 400–800 °C, and pure ZnO can be achieved above 700 °C. ZnO obtained by calcination at 700 °C had an average crystalline size around 45 nm and exhibited the highest photocatalytic activity, degrading KGL by almost 97.1% after 60 min under ultraviolet irradiation, which was superior to that of the directly synthesized and commercial ZnO. The inherent correlation between different samples and their photocatalytic activities was discussed. The phase, crystalline size, specific surface area and oxygen vacancy defects of the samples were proposed to affect their photocatalytic activity.     

Characterization of zinc sulfide (ZnS) nanoparticles Biosynthesized by Fusarium oxysporum

A variety of chemical and physical procedures could be used for the synthesis of metal sulfide nanoparticles. However, these methods suffer from some disadvantages including the use of toxic solvents, generation of hazardous by-products, and high energy consumption. In this work, zinc sulfide (ZnS) nanoparticles were synthesized through an environmentally and economically friendly method using the fungus Fusarium oxysporum. The ZnS nanoparticles were characterized using UV–visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Fluorescence spectroscopy. The obtained results demonstrated the presence of ZnS nanoparticles. Transmission electron microscopy (TEM), also determined their morphology as spherical, and their average size to be about 42 nm.     

Photocatalytic degradation of reactive black 5 azo dye by zinc sulfide quantum dots prepared by a sonochemical method

Zinc sulfide (ZnS) nanoparticles (NPs) with an average particle size of 2 nm were successfully synthesized under ultrasonic irradiation without any surfactant and high temperature treatment. Prepared NPs were characterized by powder X-ray diffraction, transmission electron microscopy, high resolution transmission electron microscopy, Fourier transform infrared spectroscopy, dynamic light scattering analysis, and UV–vis absorption spectroscopy. The energy band gap of ZnS NPs was measured by UV–vis absorption spectroscopy. The photocatalytic activity of semiconducting sulfide quantum dots for degradation of an azo dye called reactive black 5 (RB5) was investigated. Results showed that the dye can be photocatalytically degraded with high rate by ZnS NPs under UV light irradiation. The kinetics of removal of RB5 in aqueous solutions was studied in a series of experiments which were varied in the amount of ZnS NPs, contact time, pH, dye concentration, and temperature. The experimental data were fitted very well in the pseudo-second order kinetic model. 95% of dye was successfully removed in 10 min using 0.2 g ZnS NPs in a neutral pH. A possible molecular mechanism for photocatalytic degradation of dye by ZnS NPs was also given.     

Facile synthesis and photocatalytic activity of hollow micro-spherical zinc sulfide caps

Novel zinc sulfide (ZnS) hollow micro-spherical caps were produced via a facile thermal evaporation of ZnS and Zn powders without any types of templates. The samples are characterized by X-ray diffraction, scanning electron microscopy, Raman spectra and fluorescence spectra. The results demonstrate that the synthesized ZnS nanoparticles are hollow micro-spherical caps with the diameters ranging from 4 to 8 μm and a relatively homogeneous shell thickness of about 40 nm. Furthermore, the formation mechanism of ZnS hollow micro-spherical caps was also suggested. Moreover, the photocatalysis test shows that the ZnS hollow micro-spherical caps exhibit a high photocatalytic activity, thereby implying that the surface of ZnS can promote the separation of photogenerated electron–hole pairs and enhance the photocatalytic activity.     

Tunable emission property of biotin capped Gd:ZnS nanoparticles and their antibacterial activity

Gd doped ZnS nanoparticles have been successfully fabricated by a microwave irradiation method whose surface was passivated with biotin at different concentration. The structural property was investigated by characterizing the samples with the help of X-ray diffraction (XRD), Fourier transform Infrared spectroscopy (FTIR) and Transmission electron microscopy (TEM). Energy dispersive spectroscopy (EDS) measurement showed the existence of Gd ion in the Gd-doped ZnS nanoparticles. Optical confirmation was done with the help of UV–visible and photoluminescence spectroscopy. Diffraction data confirmed the zinc blend structure for all the samples with grain size of 5.8 nm for uncapped and 3–4 nm for capped nanoparticles with varying concentration of biotin. Spherical shape with 7 nm (uncapped) and 4 nm (capped) were definite from TEM images. HRTEM images and SAED patterns with bright circular rings designated the cubical environment of these nanoparticles. Emission bands in the blue, green and red regions were observed for both the samples, which was blue shifted in case of capped nanoparticles with increased intensity. Enhanced luminescence property was observed in the case of capped Gd:ZnS nanoparticles when compared to uncapped and thus can be of biomedical uses. Notably these biotin capped Gd:ZnS nanoparticles proved to be a potential antibacterial agent against different pathogenic bacterial strains, which showed maximum zone of inhibition at concentration of 10 µg/ml. The bioactivity sums up that this surface passivated nanoparticle emerges as a new class of antibacterial agent.     

Optical properties of undoped and cobalt doped ZnS nanophosphor

In the present study, the optical properties of ZnS and cobalt (Co) doped ZnS nanoparticles were investigated at room temperature. ZnS and ZnS:Co nanophosphors were prepared through chemical route, namely the chemical precipitation method and the formation of the nanoparticles were confirmed by X-ray diffraction and field emission scanning electron microscope (FESEM). Band gap energy of the prepared samples is determined by using a UV–vis–NIR spectrophotometer. The photoluminescence property of ZnS and ZnS:Co sample is determined by fluorescence spectroscopy. The sizes of as prepared nanoparticles are found to be in the 8–9 nm range. The FESEM morphology shows the formation of nanostructure of ZnS samples. The value of optical band gap has been found to be in the range 4.30–4.03 eV. Room temperature photoluminescence (PL) spectrum of the undoped sample exhibits emission in the blue region with multiple peaks under UV excitation. On the other hand, Co²⁺ doped ZnS samples show enhanced visible light emissions under the same UV excitation wavelength of 310 nm.     

Enhanced photoluminescence properties of ZnS:Cu2+ nanoparticles using PMMA and CTAB surfactants

ZnS nanoparticles with Cu²⁺ doping have been synthesized at 80 °C through a soft chemical route, namely the chemical co-precipitation method at air atmosphere. The water soluble PMMA and CTAB were used as capping agents. The nanostructures of the synthesized nanoparticles have been analyzed using X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), Fourier transform infrared spectrometer (FT-IR), UV–vis and fluorescence spectrophotometer. The sizes of as-prepared nanoparticles are found to be below 3.4–5.2 nm range. Room temperature photoluminescence (PL) spectrum of the undoped sample exhibits emission in the blue region with multiple peaks under UV excitation. On the other hand, in the Cu²⁺ doped ZnS samples enhanced visible light emissions with emission intensities of ∼2 times larger than that of the undoped sample are observed for CTAB capped sample. The phase changes were observed in different temperatures by TG-DTA.     

Photocatalytic degradation of methyl orange and gas-sensing performance of nanosized ZnO

ZnO nanoparticles were synthesized by calcining composites of zinc nitrate and poly(vinyl pyrrolidone) (PVP, molecular weight 30 000) at a mass ratio of 1:2 at 500 °C for 2 h. X-Ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques were used to characterize the as-synthesized ZnO nanoparticles. The particles ranged in size from 30 to 50 nm. Infrared spectra of PVP and the PVP+Zn(NO₃)₂·6H₂O composite revealed coordination between the carbonyl (C=O) of PVP and Zn²⁺ of zinc nitrate, which led to a uniform nanoparticle morphology. The gas-sensing properties and photocatalytic performance of the final product were systematically investigated. The results show that the ZnO nanoparticles exhibit both a high response for ethanol detection and excellent photocatalytic activity for degradation of methyl orange under UV irradiation for 30 min.     

Synthesis and characterization of ZnS/ZnO/CdS nanocomposites

Water-soluble ZnS/ZnO/CdS (0.1–0.5 M) nanocomposites were successfully synthesized by the chemical precipitation method in air. X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet–visible (UV–vis), photoluminescence (PL) and thermo gravimetric-differential thermal analysis (TG-DTA) were used to characterize the synthesized products. It is found that the ZnS/ZnO/CdS (0.1–0.5 M) core–shell nanocomposite is cubic and hexagonal mixed structure. TEM results showed the prepared nanocomposites are monodispersed and uniform in size. It is confined within 4.3–5.6 nm range. UV–vis absorption spectra were confined growth process of multi shells on ZnS. It showed a red shift with respect to the shells thickness. Fluorescence measurement showed the emission band which exists in the visible region. Stability and phase transition were identified by TG-DTA analysis. The results show an improved florescence property, indicating their potential applications in biological labeling.     

Red luminescence of spherical CuxZn1−xS semiconductor nanoparticles using 2-mercaptoethanol as capping agent

Cu²⁺-doped (0–2 at%) ZnS nanoparticles stabilized by 2-mercaptoethanol (2-ME) were successfully prepared using wet precipitation route in aqueous solution. The structural and optical characteristics were studied by various techniques. XRD pattern showed zinc blende cubic structure of Cu²⁺-doped ZnS with grain size of 4±0.5 nm. Spherical shape and well distribution of particles is confirmed by TEM, SEM and STM microscopy. Copper doping were identified by elemental dispersive (EDS) spectrometry. UV–vis spectroscopy revealed strong confinement effect due to blue shift in absorption shoulder peak as compared to bulk ZnS. Red luminescence band at～657 nm on Cu²⁺ doping may be arising from recombination of electrons at sulfur vacancies (V_s) and Cu(t₂) states formed at ZnS band gap. Optimum concentration of 0.25 at% (red band) of Cu²⁺ doping was selected by the observed enhanced PL emission.     

Effect of Cu concentration on the photoconductivity properties of ZnS nanoparticles synthesized by co-precipitation method

In the present work, solution based co-precipitation method has been used to prepare Cu-doped ZnS nanoparticles and characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), UV–vis absorption spectroscopy and photoconductivity (PC). XRD analysis shows the cubical zinc blende structure while for higher doping concentration extra peaks of CuS have been observed. The estimated crystallite sizes of Cu-doped ZnS lies in the range of 2–4 nm. SEM micrographs show spherical shape of nanoparticles. UV–vis absorption study shows blue shift of absorption shoulder for un-doped and Cu-doped ZnS NPs as compared to the bulk counterpart. In photoconductivity study, the enhancement of photosensitivity has been observed in 4% Cu-doped sample while the maximum current is found in 1% Cu-doped sample. The substitution of Cu is found to affect the photoconductivity properties owing to the CuS phase. The variation of darkcurrent and photocurrent with applied voltages exhibits super-linear nature (r>1). Negative photoconductivity (NPC) is observed in all the samples in which the photocurrent decreases during steady illumination.     

Absence of photocatalytic activity in the presence of the photoluminescence property of Mn–ZnS nanoparticles prepared by a facile wet chemical method at room temperature

Mn-doped ZnS nanoparticles (NPs) were prepared with dopants at various concentrations using a facile, simple and inexpensive wet chemical method at room temperature. The physicochemical properties of NPs were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible absorption spectroscopy (UV–vis) and photoluminescence (PL). XRD analysis confirmed formation of ZnS with zinc blende structure and average crystallite size of about 2 nm. TEM analysis revealed formation of hyperfine NPs with rather good uniformity. The room temperature photoluminescence (PL) spectrum of ZnS:Mn²⁺ exhibited an orange-red emission around 600 nm. The maximum PL intensity was observed for 7.5% Mn doped ZnS. The photocatalytic performance of ZnS:Mn²⁺ was successfully demonstrated for degradation of three different model dyes (i.e. Rhodimine B (Rh. B), Bromocresol Green (BCG) and Bromochlorophenol Blue (BCB)). The results revealed that not only was there a remarkable difference in photocatalytic performance of Mn doped ZnS for all three different dyes at different dopant concentrations but also photocatalytic activity was decreased by Mn doping.     

Effect of temperature on crystallite sizes of copper sulfide nanocrystals prepared from copper(II) dithiocarbamate single source precursor

We report the synthesis of CuS nanoparticles using [Cu(butdtc)₂] as single source precursor thermolysed at two different temperatures. The products were characterized by UV–vis absorption spectroscopy, X-ray diffraction, Transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray analysis and atomic force microscopy. The absorption spectra of the CuS nanocrystals are blue shifted and the XRD were indexed to the hexagonal phase of CuS with nanoparticles obtained at 120 °C showing well defined crystalline structure compared to those obtained at 180 °C. Transmission electron microscopy images showed particles that are almost spherical in shapes with average crystallite sizes of 21–38 nm for CuS1 prepared at 180 °C and 3–7 nm for CuS2 prepared at 120 °C and confirms that the chosen reaction temperature determine the crystallite sizes of the nanoparticles.     

Biologically synthesized copper sulfide nanoparticles: Production and characterization

In the present research, copper sulfide nanoparticles were synthesized through a low-cost and environmentally friendly method using the fungus Fusarium oxysporum for the first time. The extracellularly generated nanoparticles were characterized by UV–vis, Florescence Spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR), and Transmission Electron Microscopy (TEM). According to the UV–vis, Florescence and FTIR analysis, it was confirmed that the biosynthesized nanoparticles were created of copper sulfide composition. Moreover, from the morphological point of view, TEM images demonstrated that spherical particles having the size of 2–5 nm were entangled in spherical peptide shells which were about 20 nm in diameter.     

Synthesis,characterization, and measurement of structural,optical, and phtotoluminescent properties of zinc sulfide quantum dots

A facile and rapid microwave irradiation method was developed to prepare ZnS nanoparticles (NPs) using a set of ionic liquids (ILs) based on the bis(trifluoromethylsulfonyl) imide anion and different cations of 1-alkyl-3-methyl-imidazolium. The phases, structures, and optical absorption properties of the NPs were determined in depth with X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, UV–vis absorption spectroscopy (UV–vis), diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). The average crystallite size of the ZnS NPs calculated from the XRD pattern was of the order of 2.8 nm which exhibits cubic zinc blende structure. The energy band gap measurements of NPs were carried out by UV and DRS. The results revealed that the ZnS NPs exhibit strong quantum confinement effect. The optical band gap energy increases significantly compared with those of the bulk ZnS. The refractive indices for different ZnS nanosamples and different concentrations of ZnS NPs for a typical sample suspended in deionized water were also measured.     

Studies on structural,morphological, magnetic and optical properties of chromium sesquioxide (Cr2O3) nanoparticles: Synthesized via facile solvothermal process by different solvents

Chromium sesquioxide (Cr₂O₃) nanoparticles have been successfully synthesized via the facile solvothermal process, by using CrO₃ in different solvents. The as-synthesized nanoparticle sizes are calculated and confirmed to be 25–45 nm, by using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The functional groups of the samples were tested by the Fourier transform infrared (FTIR) spectroscopy. Fine and spherical-like morphologies and compositional elements of the products were observed by the scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. A weak ferromagnetic (WFM) property was observed for sample by the vibrating sample magnetometer (VSM). The observed band gap values (E_g=4.33–3.54 eV) higher than that of bulk Cr₂O₃ (~3.4 eV) indicated that the particles had been successfully synthesized in the nano region, and measured by ultra-violet visible (UV–vis) absorption spectroscopy. The broad visible emission at ~399 nm, in the photoluminescence spectroscopy revealed the high purity and perfect crystallinity of the samples.     

Strong blue luminescence of O2−-doped ZnS nanoparticles synthesized by a low temperature solid state reaction method

O^2?-doped ZnS(ZnS:O) nanoparticles with strong blue emission were successfully synthesized using a facile low temperature solid state reaction method. X-ray powder diffraction, scanning electron microscopy, and transmission electron microscopy were used to characterize their crystal structures, sizes, morphologies, and photoluminescence. The ZnS:O nanoparticles were quasi-spherical particles with a cubic zincblende crystal structure, and their average crystallite diameter was about 8.35–13.50 nm. Dependence of the photoluminescence properties of the ZnS:O nanoparticles on the Zn/O ratio in the source materials was studied, and an optimal O^2? doping condition was found to be Zn/O=10:5.3. The ZnS:O (Zn/O=10:5.3) nanoparticles exhibited strong blue emission with an intensity 9 times higher than the undoped nanoparticles.     

Effect of calcination temperature on Cu doped NiO nanoparticles prepared via wet-chemical method: Structural,optical and morphological studies

In the present study, NiO and Cu-doped NiO nanoparticles were successfully synthesized by wet chemical method at room temperature using sodium hydroxide (NaOH) as precipitating agent. The as-prepared Cu-doped NiO powder samples were subjected to three different calcination temperatures such as, 350 °C, 450 °C and 550 °C in order to investigate the impact of calcined temperatures on the phase formation, particle size and band gap evolution. The phase formation and crystal structure information of the prepared nanomaterials were examined by X-ray powder diffraction (XRD). XRD revealed the face-centered cubic (FCC) structure. Average crystalline size of pure and doped samples estimated using Scherer formula was found to be 15 nm and 9 nm respectively. With increase in the calcination temperature from 350 °C to 550 °C for the Cu doped NiO samples the particle size of the nanoparticles was found to increase from 4 nm to 9 nm respectively. The optical study for both pure and doped NiO nanoparticles was performed using an UV–Vis spectrophotometer in the wavelength range of 200–800 nm. The strong absorption in the UV region confirms the band gap absorption in NiO and was estimated from the UV–Vis diffuse reflectance spectra via Tauc plot. Systematic studies were also carried out to study the effect of calcination on the optical transmittance. Samples were also investigated using Raman and Fourier Transform Infrared Spectroscopy (FTIR). Furthermore, morphology of the pure NiO and Cu-doped NiO Nanoparticles were examined by scanning electron microscope (SEM).     

Biosynthesis of zinc oxide nanoparticles from Azadirachta indica for antibacterial and photocatalytic applications

Green synthesis of nanoparticles is gaining importance and has been suggested as possible alternatives to chemical and physical methods. The present work reports low-cost, green synthesis of zinc oxide (ZnO) nanoparticles using 25% (w/v) of Azadirachta indica (Neem) leaf extract. The biosynthesized nanoparticles were characterized by transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), UV–visible spectroscopy (UV–vis), X-ray diffraction (XRD) and fourier transform infrared spectroscopy (FTIR). The synthesized ZnO nanoparticles were pure, predominantly spherical in shape with size ranging from 9.6 to 25.5 nm. In the present work, the biosynthesized ZnO nanoparticles have been used for antibacterial and photocatalytic applications. The antibacterial activity of characterized samples was determined using different concentrations of biosynthesized ZnO nanoparticles (20 µg/mL, 40 µg/mL, 60 µg/mL, 80 µg/mL and 100 µg/mL) against Gram-positive and Gram-negative bacteria: Staphylococcus aureus, Streptococcus pyogenes and Escherichia coli using shake flask method. The obtained results revealed that the bacterial growth decreases with increase in concentration of biosynthesized ZnO nanoparticles. In Addition, Gram-positive bacteria seemed to be more sensitive to ZnO nanoparticles than Gram-negative bacteria. The biosynthesized ZnO nanoparticles showed photocatalytic activity under the UV light enhancing the degradation rate of methylene blue (MB), which is one of the main water-pollutant released by textile industries.     

Thin films of silica imbedded silicon and germanium quantum dots by solution processing

Hydrophilic silicon (0.9 nm) and germanium (2.7 nm) quantum dots (QDs), synthesized utilizing micelles to control particle size, were coated with silica using liquid phase deposition. The use of dodecyltrimethylammonium bromide as a surfactant yielded uniform spheres (Si@SiO₂=57 nm; Ge@SiO₂=32 nm), which could then be arrayed in three dimensions using a vertical deposition method on quartz plates. The silica coated QDs were characterized by UV–visible spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy, and transmission electron microscopy. The thin films were characterized by UV–visible spectroscopy, scanning electron microscopy, and the measurement of a photocurrent.