Rapid synthesis, characterization and optical properties of TiO2 coated ZnO nanocomposite particles by a novel microwave irradiation method

A novel and rapid microwave method was used to prepare TiO₂ coated ZnO nanocomposite particles. The resulted particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Results show that ZnO nanoparticles were coated with 6-10 nm amorphous TiO₂ layers. In addition, zeta potential analysis demonstrated the presence of TiO₂ layer on the surface of ZnO nanoparticles. Photoluminescence (PL) spectroscopy and UV-visible spectroscopy were used to investigate the optical properties of the nanoparticles. Compared to uncoated ZnO nanoparticles, the TiO₂ coated ZnO nanoparticles showed enhanced UV emission. The UV-visible diffuse reflectance study revealed the significant UV shielding characteristics of the nanocomposite particles. Moreover, amorphous TiO₂ coating effectively reduced the photocatalytic activity of ZnO nanoparticles as evidenced by the photodegradation of Orange G with uncoated and TiO₂ coated ZnO nanoparticles under UV radiation.     

Synthesis and enhanced light absorption of alumina matrix nanocomposites containing multilayer oxide nanorods and silver nanoparticles

In this paper, multilayer oxide nanorods were deposited in the nanopores of anodic aluminum oxide (AAO) via solution infiltration followed by heat treatment. The nanorods have a core–shell structure. First, the shell (nanotube) with the thickness of about 40 nm was made of TiO₂ through the hydrolysis of (NH₄)₂TiF₆. Second, silver nanoparticles with the diameter of about 3 nm were added into the TiO₂ layer through thermal decomposition of AgNO₃ at elevated temperatures. Then, cylindrical cores (nanorods) of CoO and ZnO with 200 nm diameter were prepared, respectively. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and composition of the nanorods. UV–vis light absorption measurements in the wavelength range from 350 to 1000 nm were performed to study the effect of nanorod and nanoparticle addition on the light absorption property of the alumina nanocomposites. It is found that CoO nanorods increase the light absorption of the alumina matrix composite in the wavelength range from 500 nm to 800 nm, but the TiO₂ shell does not increase the light absorption much. The ZnO nanorods do not change the light absorption either. However, the addition of silver nanoparticles significantly enhances light absorption of both AAO/TiO₂/Ag/CoO and AAO/TiO₂/Ag/ZnO nanocomposites. This increase in the visible light absorption reveals that there exists surface plasmon around the fine silver nanoparticles in the nanorods.     

Fabrication of TiO2 nanotube film by well-aligned ZnO nanorod array film and sol-gel process

High density TiO₂ nanotube film with hexagonal shape and narrow size distribution was fabricated by templating ZnO nanorod array film and sol-gel process. Well-aligned ZnO nanorod array films obtained by aqueous solution method were used as template to synthesize ZnO/TiO₂ core-shell structure through sol-gel process. Subsequently, TiO₂ nanotube array films survived by removing the ZnO nanorod cores using wet-chemical etching. Polycrystalline anatase TiO₂ nanotube films were ∼ 1.5 μm long and ∼ 100 nm in inter diameter with a wall thickness of ∼ 10 nm.     

Coating of TiO2 nanoparticles with PbS thin films and preparation of PbS nanoparticles using a one-pot sonochemical reaction under the multibubble sonoluminescence conditions

Preparations of PbS-coated titanium dioxide (TiO₂) and lead sulfide (PbS) nanoparticles under ultrasonic field at the multibubble sonoluminescence (MBSL) conditions were tested in water solutions. Under the optimal MBSL conditions (20 kHz and 220 W power input), PbS nanoparticles (diameter = 40-50 nm) were prepared by treating lead nitrate and thioacetamide for 20 min in water solutions. The size of PbS nanoparticles was found to be easily increased to about 90 nm in diameter by increasing the reactant concentration twice. A similar sonochemical reaction with TiO₂ nanoparticles (about 20-30 nm in diameter) gave rise to PbS-coated TiO₂ nanoparticles with a core/shell structure. The PbS thin film coating was quite uniform and the average coating depth of PbS on the TiO₂ nanoparticles was about 2-3 nm under the described conditions. It is interesting to note that the coating depth was found to be controlled to 2-10 nm range by increasing the amounts of reactants for Pb and S twice with a sonication time of 30 min.     

Facile preparation of Ag/ZnO nanoparticles via photoreduction

Ag/ZnO nanoparticles can be obtained via photocatalytic reduction of silver nitrate at ZnO nanorods when a solution of AgNO₃ and nanorods ZnO suspended in ethyleneglycol is exposed to daylight. The mean size of the deposited sphere like Ag particles is about 5 nm. However, some of the particles can be as large as 20 nm. The ZnO nanorods were pre-prepared by basic precipitation from zinc acetate di-hydrate in the ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide. They are about 50–300 nm in length and 10–50 nm in width. Transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDS), X-ray powder diffraction (XRD), UV–Vis spectroscopy, X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) were used to characterize the resulting Ag/ZnO nanocomposites.     

Decolorization of beads-milled TiO2 nanoparticles suspension in an organic solvent

In this paper, a new method is proposed for the decolorization of a yellow-hued suspension of rutile TiO₂ nanoparticles in an organic solvent (diethylene glycol dimethylether). The presence of color has always been undesirable in a suspension of nanoparticles filler used for industrial needs, particularly for optical applications.A colorless suspension was achieved by irradiating well-dispersed TiO₂ nanoparticles in an organic solvent with UV-light (λ = 254 nm) for 5 h. TiO₂ nanoparticles of 1 and 5 wt.% were dispersed using a beads mill method. Trimethoxytrifluor(propyl) silane was used as a dispersant to achieve stability. The effect of the UV-light irradiation on the TiO₂ nanosuspension was investigated by means of a Fourier transform nuclear magnetic resonance analyzer (FT-NMR). The dispersant was partially desorbed due to the interaction of UV light and the TiO₂/dispersant complex. Thus, an enhanced transparency and the absence of color were obtained for well-dispersed TiO₂ nanoparticles in an organic solvent.     

Plasmonic Metal Mediated Charge Transfer in Stacked Core–Shell Semiconductor Heterojunction for Significantly Enhanced CO2 Photoreduction

Construction of core–shell semiconductor heterojunctions and plasmonic metal/semiconductor heterostructures represents two promising routes to improved light harvesting and promoted charge separation, but their photocatalytic activities are respectively limited by sluggish consumption of charge carriers confined in the cores, and contradictory migration directions of plasmon-induced hot electrons and semiconductor-generated electrons. Herein, a semiconductor/metal/semiconductor stacked core–shell design is demonstrated to overcome these limitations and significantly boost the photoactivity in CO₂ reduction. In this smart design, sandwiched Au serves as a “stone”, which “kills two birds” by inducing localized surface plasmon resonance for hot electron generation and mediating unidirectional transmission of conduction band electrons and hot electrons from TiO₂ core to MoS₂ shell. Meanwhile, upward band bending of TiO₂ drives core-to-shell migration of holes through TiO₂–MoS₂ interface. The co-existence of TiO₂ → Au → MoS₂ electron flow and TiO₂ → MoS₂ hole flow contributes to spatial charge separation on different locations of MoS₂ outer layer for overall redox reactions. Additionally, reduction potential of photoelectrons participating in the CO₂ reduction is elaborately adjusted by tuning the thickness of MoS₂ shell, and thus the product selectivity is delicately regulated. This work provides fresh hints for rationally controlling the charge transfer pathways toward high-efficiency CO₂ photoreduction.     

Adsorption and solar light activity of transition-metal doped TiO<Subscript>2</Subscript> nanoparticles as semiconductor photocatalyst

There is an eminent interest to improve the photoactivity of TiO₂ nanostructures via doping with mid-band gap donors or acceptors to achieve a high solar absorption. In the present work, Cr- and V-doped TiO₂ nanoparticles were prepared via a facile chemical vapor synthesis method. The effect of the transition metals (TM) on the solar light activity of the semiconductor nanoparticles as photocatalyst was examined by degradation of methylene blue and acid red 27. Induced coupled plasma and X-ray photoelectron spectroscopy analyses indicated high efficiency of the doping process in the hot wall reactor without surface covering of the TiO₂ nanoparticles by the dopants. Diffuse reflectance spectroscopy also revealed a red shift of the absorption edge of the TiO₂ nanoparticles with increasing dopant concentration. Analysis of the photoactivity of the synthesized nanoparticles under sun light showed an increase in the primary absorption of dye molecules on the surface of Cr- and V-doped TiO₂ nanoparticles whereas the degradation rate was found to depend on the type and concentration of the dopants. A high photoactivity is obtained at 0.2 at% V concentration. The mechanism of photoactivity is discussed based on the effect of TM on the absorption edge of the semiconductor.     

Grain growth kinetic in xTiO2–6 wt.% Bi2O3–(94 − x) ZnO (x=0, 2, 4) ceramic system

The grain growth kinetics in the 0, 2 and 4 wt.% TiO₂ added ZnO–6 wt.% Bi₂O₃ system was studied using the simplified phenomenological grain growth kinetics equation together with the physical properties of the sintered samples. The grain growth exponent value (n) and the apparent activation energy for the ZnO–6 wt.% Bi₂O₃ system was 5 and 218 kJ/ mol, respectively. The addition of the TiO₂ to the ZnO–6 wt.% Bi₂O₃ system inhibited the ZnO grain growth. At 2 and 4 wt.% TiO₂ additions, the apparent activation energies were calculated as 467 and 346 kJ/ mol, respectively. The addition of TiO₂ to the system inhibited the grain growth of ZnO ceramics.     

Optical,morphological, electrical properties of ZnO-TiO2-SnO2/CeO2 semiconducting ternary nanocomposite

Low dielectric constant and low dielectric loss with moderate wide bandgap, novel semiconducting metal oxide composites are useful materials for applying optoelectronic, microwave dielectric ceramics. A less dielectric constant is required for wireless communication to reduce the cross pairing between conductors and also for fast signal transmission. In the present study, the structural, optical, and dielectric properties of ternary ZnO - TiO₂ added with SnO₂/CeO₂ semiconducting nanocomposite materials were investigated and synthesized by the solid-state gelation method. The samples were sintered at a temperature of 450 ⁰C. The X-ray diffraction patterns of composites revealed the existence of TiO₂ anatase phase, SnO_2, and CeO₂. The average crystallite size at d₁₀₁ was measured using the Scherer method, ranging from 6.18 nm to 9.13 nm. The overall crystallite size was calculated using the Size-strain plot method, and it is in the range of 14.8 nm to 17.16 nm. The surface morphology of all samples appears uniform in size and spherical shape. The average particle size of grains was 35 nm. The absorbance properties studied by UV–Visible spectroscopy and bandwidth were 2.6 eV calculated using Tauc’s plot method, and it reveals the formation of new energy levels. The dielectric properties of pellet dimensions of 1 mm thickness and 10 mm diameter, measured from the LCR meter, are indicated at 1 kHz frequency. The most significant dielectric constant (ε_r) and lowest loss tangent (Tan δ) are 53.89 and 0.25 for pure ZnO - TiO₂, and the lowest dielectric constant (ε_r) and less loss tangent (Tan δ) are 9.69 and 0.38 for 1 wt% CeO₂ doped to ZnO - TiO₂. The conductivity of the composite is in the range of 10^-7 S/cm. With additive concentration to ZnO - TiO₂, both SnO₂ and CeO₂ are equally potential and modifies the parameters due to the similar bandgaps and more oxygen availability.     

Synthesis of tapered TiO2 tubes by replication of ZnO

Micrometer-long tapered TiO₂ tubes have been successfully prepared by a vapor phase method, using tetrapodlike ZnO as template and tetrabutyl titanate (TBT) as titanium source. A very homogeneous TiO₂ coating layer was first prepared on tetrapodlike ZnO and the ZnO core was removed by hydrochloric acid solution. It was found that the obtained tubes were uniform and composed of anatase TiO₂ nanocrystallites. The wall thickness of the TiO₂ tubes varies from 20 to 60 nm by adjusting the amount of TBT. The BET surface area reaches 95 m² g^− 1. The combination of the tubular structure and special morphology may improve the mass transport and benefit to the recovery of the TiO₂ tubes photocatalyst from treated waste water.     

ZnO sputter coating on SnO2 nanowires: Effects of thin coating and subsequent thermal annealing

The structural and optical properties of SnO₂–ZnO core–shell nanowires were studied and the effects of thermal annealing were investigated. As-prepared SnO₂–ZnO core–shell nanowires exhibited a smooth and continuous shell layer along the nanowire, with a thickness in the range of 5–10 nm. While the thin ZnO shell layer disappeared after annealing at 800 °C, this did not occur after annealing at 600 °C. The as-fabricated SnO₂–ZnO core–shell nanowires exhibited yellow emission, presumably from the core SnO₂ nanowires. The UV emission from ZnO shell layer was obtained by annealing at 600 °C, whereas it was removed by annealing at 800 °C.     

Synthesis and characterization of ZnO/SiO2 core/shell nanocomposites and hollow SiO2 nanostructures

In this paper, we prepared the ZnO nanoparticles by a simple hydrothermal method and fabricated the ZnO/SiO₂ core/shell nanostructures through a sol-gel chemistry process successfully. The hollow SiO₂ nanostructures were obtained by selective removal of the ZnO cores. The structure, morphology and composition of the products were determined by the techniques of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). The results indicated that the ZnO nanoparticles were sphere-like shape with the average size of 60 nm and belonged to hexagonal wurtzite crystal structure. With the coating of SiO₂, the vibration modes of Si-O-Si and Si-OH were found. Furthermore, the measurement results of optical properties showed that spectra of bare ZnO nanoparticles and ZnO/SiO₂ core/shell nanocomposites exhibited similar emission features, including a blue emission peak and an orange emission band.     

Synthesis and characterization of pure anatase TiO<Subscript>2</Subscript> nanoparticles

Pure anatase TiO₂ nanoparticles were synthesized by microwave assisted sol–gel method and further characterized by powder X-ray diffraction (XRD), energy dispersive x-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV–Visible spectrophotometer, SEM images showed that TiO₂ nanoparticles were porous structure. The XRD patterns indicated that TiO₂ after annealed at 300 °C for 3 h was mainly pure anatase phase. The crystallite size was in the range of 20–25 nm, which is consistent with the results obtained from TEM images. Microwave heating offers several potential advantages over conventional heating for inducing or enhancing chemical reactions.     

Characterization and photoactivity of TiO2 sols prepared with triethylamine

Using triethylamine as a surface protective agent, a transparent and pale yellowish TiO₂ sol had been prepared at 90 °C. This method was very different from the traditional methods, which produced titanium dioxide nanoparticles with anatase crystalline structure either at high acid condition or high temperature. X-ray diffraction (XRD) and transmission electron spectroscopy (TEM) demonstrated that the as-prepared TiO₂ sol nanoparticles with anatase crystalline structure were uniformly distributed, and the average size was 3 nm. X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectra showed that triethylamine was adsorbed on TiO₂ sol particles surface. FTIR spectroscopy noted that TiO₂ sol particles had the similar spectra with Degussa P25. Photoactivity of the as-prepared TiO₂ sol was studied by investigating the photodegradation of methyl violet in hydrosol reaction system under visible light irradiation.     

Rapid synthesis of TiO2 hollow nanostructures with crystallized walls by using CuO as template and microwave heating

In this paper, TiO₂ hollow nanostructures with anatase walls have been rapidly fabricated by using CuO as template and microwave heating. These TiO₂ hollow nanostructures have been characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Experimental results showed that the TiO₂ shell transformed from amorphous to anatase phase in 3 min, induced by the hot CuO core under microwave irradiation. The diameter of TiO₂ hollow nanostructures is about 50-80 nm, and the length is about 200-300 nm. The thickness of the shell is about 3 nm. This method is promising to be used to synthesize other nanomaterials with a hollow nanostructure.     

Co-emission of UV, violet and green photoluminescence of ZnO/TiO2 thin film

ZnO/TiO₂ thin films were fabricated on quartz glass substrates by E-beam evaporation. The structural and optical properties were investigated by X-ray diffraction (XRD), Raman spectra, optical transmittance and photoluminescence. XRD analysis indicates that the TiO₂ buffer layer can increase the preferential orientation along the (002) plane of the ZnO film. PL measurements suggest that co-emission of strong UV peak at 378 nm, violet peak at 423 nm and weak green luminescence at 544 nm is observed in the ZnO/TiO₂ thin film. The violet luminescence emission at 423 nm is attributed to the interface trap in the ZnO film grain boundaries.     

Tuning the band gap of ZnO nanoparticles by ultrasonic irradiation

In this present paper, we report the tunability of ZnO nanoparticles by ultrasonic irradiation. Different sized ZnO nanoparticles viz. 2.58–2.97 nm have been synthesized with variation of ultrasonic irradiation time 75–270 min in presence of Histidine as capping agent. UV and visible spectroscopy study revealed that as ultrasonic irradiation time increases, there is increase in amount of formed ZnO nanoparticles and also there is red shift in absorption edge. This confirms the tunability of bandgap of histidine capped ZnO nanoparticles with ultrasonic irradiation. Growth mechanism for controlling the size of ZnO nanoparticles are also discussed.     

Visible light-activated cadmium-doped ZnO nanostructured photocatalyst for the treatment of methylene blue dye

An attempt was made to prepare Cd-doped ZnO photocatalyst for visible light assisted degradation of a textile dye (methylene blue, MB) in aqueous solutions by a traditional sol–gel process. The as-prepared nanoparticles were characterized by X-ray diffraction, UV–vis diffuse reflectance spectroscopy, and photoluminescence spectra techniques. The results showed that the Cd-doped ZnO possess the single-phase hexagonal wurtzite structure. The photocatalytic activity of the nanoparticles under visible light was investigated by measuring the photodegradation of MB in aqueous dispersion. The effects of key operation parameters such as initial dye concentration, catalyst loading as well as initial pH value on the decolorization extents were investigated. The results indicate that the decolorization of the organic molecule followed a pseudo-first-order kinetics according to the Langmuir–Hinshelwood model. Under the optimum operation conditions, approximately 85.0% dye removal was achieved within 3.5 h.     

Synthesis of nano-MoS<Subscript>2</Subscript>/TiO<Subscript>2</Subscript> composite and its catalytic degradation effect on methyl orange

A nano-MoS₂/TiO₂ composite was synthesized in H₂ atmosphere by calcining a MoS₃/TiO₂ precursor, which was obtained via a quick deposition of MoS₃ on anatase nano-TiO₂ under a strong acidic condition. The obtained nano-MoS₂/TiO₂ composite was characterized by X-ray diffraction spectroscopy, Brunauer–Emmett–Teller (BET) surface area, scanning electron microscopy, high-resolution transmission electron microscopy, energy-dispersive spectrometry, ultraviolet–visible spectroscopy, and Fourier transform infrared spectroscopy. The results show that the composite had a high BET surface area because of its small size and irregularly layered structure. MoS₂ in the composite was composed of typical layered structures with thicknesses of 2–8 nm and lengths of 10–40 nm. The composite contained a wide and intensive absorption at 400–700 nm, which is in the visible light region, and presented a positive catalytic effect on removing methyl orange from the aqueous solution. The catalytic activity of the composite was influenced by the initial concentration of methyl orange, the amount of the catalyst, the pH value, and the degradation temperature. In addition, the composite catalyst could be regenerated and repeatedly used via filtration three times. The deactivating catalyst could be reactivated after catalytic reaction by heating at 450 °C for 30 min in H₂.