A novel method for fast and continuous preparation of superfine titanium dioxide nanoparticles in microfluidic system

Previously we had developed a microfluidic system that can be easily fabricated by bending a stainless-steel tube into large circular loops. In this study, a fast and continuous preparation method for superfine TiO₂ nanoparticles (TiO₂-NPs) was developed for the aforementioned microfluidic system. The proposed method can yield anatase TiO₂ in 3.5 min, in contrast to the traditional hydrothermal reaction method, which requires hours or even days. Different reaction conditions, such as reaction temperature (120–200 °C), urea concentration (20–100 g/L), and tube length (5–20 m) were investigated. X-ray diffraction and Brunauer–Emmett–Teller analysis indicate that the as-prepared TiO₂-NPs have crystalline sizes of 4.1–5.8 nm and specific surface areas of 250.7–330.7 m²/g. Transmission electron microscopy images show that these TiO₂-NPs have an even diameter of approximately 5 nm. Moreover, because of their small crystalline sizes and large specific surface areas, most of these as-prepared TiO₂-NPs exhibit considerably better absorption and photocatalytic performance with methylene blue than commercial P5 TiO₂ does.     

Green synthesis and enhanced photocatalytic activity of Ce-doped TiO2 nanoparticles supported on porous glass

A facile and green method to prepare Ce-doped TiO₂ nanoparticles supported on porous glass beads is reported. An ion exchange process and subsequent calcination yielded Ce-doped TiO₂ nanoparticles with a mean size of 4.8 ± 0.3 nm. The nanoparticles were dispersed on the surface of porous glass beads. The addition of Ce enhanced the visible light absorption of the TiO₂ nanoparticles in the 400–500 nm spectral window. The band gap of the as-prepared catalyst was 2.80 eV. The Ce-doped TiO₂ nanoparticles immobilized on porous glass beads exhibited excellent photocatalytic activity for the visible-light-degradation of methyl orange (MO) and rhodamine B (RhB); with rate constants of 0.095 and 0.230 min⁻¹; respectively. The effects of Ce dosage; reaction duration; and initial solution pH on the conversion of MO and RhB dyes were investigated. The green synthesis and favorable photocatalytic activity makes the Ce-doped TiO₂ nanoparticles immobilized on porous glass an attractive alternative for the efficient degradation of organic pollutants.     

2D reduced graphene oxide–titania nanocomposites synthesized under different hydrothermal conditions for treatment of hazardous organic pollutants

Two-dimensional reduced graphene oxide–titania (RGO–TiO₂) composites were prepared using a single-step hydrothermal method under various hydrothermal reaction conditions. The morphological and surface characteristics of the RGO–TiO₂ composites and reference materials were determined. The RGO–TiO₂ composites showed photocatalytic activity for the decomposition of two target pollutants that was superior to both pure TiO₂ and RGO under fluorescent daylight lamp illumination. The photocatalytic activity of the RGO–TiO₂ composite increased as the hydrothermal treatment time increased from 1 to 24 h, but then it decreased as the time increased to 36 h, which indicated the presence of an optimal treatment time. RGO–TiO₂ composites activated by violet light-emitting diodes (LEDs) displayed lower decomposition efficiency than those activated by a daylight lamp, likely because of the lower light intensity of violet LEDs (0.2 mW/cm²) when compared with that of the daylight lamp (1.4 mW/cm²). However, the photocatalytic decomposition of the target pollutants using the RGO–TiO₂ composite was more energy-efficient using the violet LEDs. The photocatalytic reaction rates increased as the residence time decreased, whereas the reverse was true for the decomposition efficiency.     

Capture of phosphates in surface water by TiO2 nanoparticles under UV irradiation

The capture of orthophosphates and total phosphorus from the Pudong Canal river in the Pudong District of Shanghai by TiO₂ nanoparticles is studied using a rotating photoreactor and the nano-TiO₂ photocatalyst Degussa P25. The effects of UV irradiation intensity in a range of 20–74 mW/cm², the loading of the TiO₂ nanoparticles in a range of 0.05–0.1 g/L, irradiation time up to 4 h, and pH values in a range of 2–10.5 on the capture efficiency are investigated. The results show that the capture of orthophosphates and total P are significantly enhanced by UV irradiation; at a loading of 0.1 g/L and an irradiation intensity above 36 mW/cm², orthophosphates and total phosphorus are rapidly captured by TiO₂ nanoparticles, causing an observed reduction from 0.4 mg/L down to 0.02 mg/L. pH values in a range of 2–10.5 have little effect on the capture efficiency of orthophosphates and total phosphorus.     

In situ synthesis of CNTs/Fe–Ni/TiO2 nanocomposite by fluidized bed chemical vapor deposition and the synergistic effect in photocatalysis

Carbon nanotube (CNTs)/Fe–Ni/TiO₂ nanocomposite photocatalysts have been synthesized by an in situ fluidized bed chemical vapor deposition (FBCVD) method. The composite photocatalysts were characterized by XRD, Raman spectroscopy, BET, FESEM, TEM, UV–vis spectroscopy, and XPS. The results showed that the CNTs were grown in situ on the surface of TiO₂. Fe(III) in TiO₂ showed no chemical changes in the growth of CNTs. Ni(II) was partly reduced to metal Ni in the FBCVD process, and the metal Ni acted as a catalyst for the growth of CNTs. The photocatalytic activities of CNTs/Fe–Ni/TiO₂ decreased with the rise of the FBCVD reaction temperature. For the sample synthesized at low FBCVD temperature (500 °C), more than 90% and nearly 50% of methylene blue were removed under UV irradiation in 180 min and under visible light irradiation in 300 min, respectively. The probable mechanism of synergistic enhancement of photocatalysis on the CNTs/Fe–Ni/TiO₂ nanocomposite is proposed.     

Visible light-driven photocatalysis of W,N co-doped TiO2

W, N co-doped TiO2 nanoparticles were synthesized by a sol-gel method. The prepared samples were characterized by X-ray diffraction （XRD）, field emission scanning electron microscopy （FE-SEM）, trans- mission electron microscopy （TEM）, Fourier transform infrared spectroscopy （FT-1R）, X-ray photoelectron spectroscopy （XPS） and diffuse reflectance spectrophotometry （DRS）. The results showed that the co- doped photocatalysts were essentially uniform spherical particles with the smallest particle size of 22.5 nm. Compared to un-doped TiO2, N-TiO2 and P-25, the absorption edge of the W, N co-doped TiO2 shifted to longer wavelength and its photocatalytic activity for degradation of methyl orange （MO） under Xe-lamp （350W） was higher.     

Functionalized TiO2@ZrO2@Y2O3 ：Eu3＋ core-multishell microspheres and their photoluminescence properties

TiO2@ZrO2@Y2O3 ：Eu3＋ composite particles with a core-multishell structure were synthesized through the combination of a layer-by-layer （LBL） self-assembly method and a sol-gel process. The obtained sam- ples were characterized with scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, X-ray photoelectron spectroscopy （XPS）, X-ray diffraction （XRD）, and fluorescence spectropho- tometry. The results showed that the composite particles had a core-multishell structure, spherical morphology, and a narrow size distribution. The presence of a ZrO2 layer on the TiO2 core can effec- tively prevent the reaction between the TiO2 core and a Y203 shell; the temperature for the reaction between the TiO2 core and the Y203 shell in the TiO2@ZrO2@Y2O3 ：Eu core-multishell phosphor can be elevated by 300 ℃ compared to that for TiO2@ZrO2：Eu. Upon excitation of the core-multishell particles in the ultraviolet （254 nm）, the Eu3＋ ion in the Y2O3 ：Eu3＋ shell shows its characteristic red emission （611 nm, 5D0→7F2）, and the photoluminescence （PL） intensity of the phosphor with the core-multishell structure was obviously greater than that of the core-shell TiO2@Y2O3 ：Eu phosphor.     

Size and shape effects on magnetic properties of Ni nanoparticles

Pure Ni nanoparticles ranging in size from 24 to 200 nm are prepared via thermal decomposition of nickel acetylacetonate in oleylamine. The as-prepared Ni particles change from spherical to dendritic or starlike with increasing precursor concentration. The particles are stable because the organic coating occurs in situ. Magnetic measurement reveals that all the Ni nanoparticles are ferromagnetic and show ferromagnetic–paramagnetic transitions at their Curie points. The saturation magnetization M_s is size-dependent, with a maximum value of 52.01 and 82.31 emu/g at room temperature and 5 K, respectively. The coercivity decreases at first and then increases with increasing particle size, which is attributed to the competition between size effect and shape anisotropy. The Curie temperature T_c is 593, 612, 622, 626 and 627 K for the 24, 50, 96, 165 and 200 nm Ni nanoparticles, respectively. A theoretical model is proposed to explain the size-dependence of Ni nanoparticle Curie temperature.     

Immobilization of Ti02 nanoparticles on activated carbon fiber and its photodegradation performance for organic pollutants

The immobilization of titanium dioxide （TiO2） on activated carbon fiber （ACF）, （TiO2/ACF）, was accomplished by sol-gel-adsorption method followed by calcination at temperatures varying from 300 to 600℃ in an argon atmosphere. The material properties were determined by scanning electron microscope （SEM）, X-ray diffraction （XRD） and nitrogen adsorption. The photodegradation behavior of TiO2 /ACF was investigated in aqueous solutions using phenol and methyl orange （MO） as target pollutants. The effects of calcination temperature, photocatalyst dosage, initial solution pH and radiation time on the degradation of organic pollutants were studied. It was found that organic pollutants could be removed rapidly from water by the TiO2/ACF photocatalyst and the sample calcined at 500℃ exhibited the highest removal efficiency. Kinetics analysis showed that the photocatalytic degradation reaction can be described by a first-order rate equation. In addition, the possibility of cyclic usage of the photocatalyst was also confirmed. Moreover, TiO2 is tightly bound to ACF and can be easily handled and recovered from water. It can therefore be potentially applied for the treatment of water contaminated by organic pollutants.     

Effect of calcining temperature and time on the characteristics of Sb-doped SnO2 nanoparticles synthesized by the sol–gel method

Spherical Sb-doped SnO₂ (ATO) nanoparticles were synthesized by the sol–gel route, employing SnCl₄·5H₂O and SbCl₃ as precursors in an ethanol solution. The influences of the calcining temperature and calcining time on the crystallite size, crystallinity, lattice parameters, lattice distortion ratio and the resistivity of the ATO nanoparticles were synthetically investigated. The results suggested that the ATO nanoparticles were crystallized in a tetragonal cassiterite structure of SnO₂ with a highly (1 1 0)-plane-preferred orientation. The calcining temperature had a dominating effect on the crystallite size, crystallinity, lattice distortion ratios and resistivity of the ATO. As the calcining temperature increased, the average crystallite size increased, the crystallinity was promoted accompanied by a decrease in the lattice distortion ratio and a corresponding decrease in the resistivity of the ATO. X-ray diffraction (XRD) and Fourier transform infrared spectrophotometer (FTIR) analysis revealed that Sb ions could not entirely supplant the Sn ions in the SnO₂ lattice for a calcining time of less than 0.5 h, even at a calcining temperature of 1000 °C. The ATO nanoparticles calcined at 1000 °C for 3.0 h possessed the lowest resistivity of 10.18 Ω cm.     

Experimental studies on heat transfer and friction factor characteristics of Al2O3/water nanofluid in a circular pipe under laminar flow with wire coil inserts

In this paper, fully developed laminar flow convective heat transfer and friction factor characteristics of Al₂O₃/water nanofluid flowing through a uniformly heated horizontal tube with and without wire coil inserts is presented. For this purpose, Al₂O₃ nanoparticles of 43 nm size were synthesized, characterized and dispersed in distilled water to form stable suspension containing 0.1% volume concentration of nanoparticles. The Nusselt number in the fully developed region were measured and found to increase by 12.24% at Re = 2275 for plain tube with nanofluid compared to distilled water. Two wire coil inserts made of stainless steel with pitch ratios 2 and 3 were used which increased the Nusselt numbers by 15.91% and 21.53% respectively at Re = 2275 with nanofluid compared to distilled water. The better heat transfer performance of nanofluid with wire coil insert is attributed to the effects of dispersion or back-mixing which flattens the temperature distribution and make the temperature gradient between the fluid and wall steeper. The measured pressure loss with the use of nanofluids is almost equal to that of the distilled water. The empirical correlations developed for Nusselt number and friction factor in terms of Reynolds/Peclet number, pitch ratio and volume concentration fits with the experimental data within ±15%.     

Preparation of SiO2/TiO2 Janus particles by electrostatic assembly,hydrolysis and calcination

This paper describes a novel chemical method for preparing SiO₂/TiO₂ Janus particles. First, polystyrene (PSt)/SiO₂ particles with a raspberry-like structure are prepared by electrostatic assembly. The influences of the reaction time of sulfonation and the treatment times of polyelectrolyte solutions (PDADMAC, PSS) on PSt and SiO₂ are investigated with respect to the surface charge density of the particles. SiO₂/TiO₂ Janus particles are then obtained by hydrolysis of butyl titanate on the surface of PSt/SiO₂ particles followed by a calcination process. Particle size analyzer, Zeta potential instrument, FTIR, TEM and SEM are used to characterize the particle size, the amount of charge on the surface of PSt and SiO₂ particles and the compositions and morphologies of PSt/SiO₂, SiO₂/TiO₂ and PSt/SiO₂/TiO₂. The diameters of the PSt, SiO₂, PSt/SiO₂ and SiO₂/TiO₂ particles are 2.0 μm, 303 nm, 2.7 μm and 330 nm, respectively.     

Magnetic and electrochemical behavior of rhombohedral α-Fe2O3 nanoparticles with (1 0 4) dominant facets

Uniform rhombohedral α-Fe₂O₃ nanoparticles, ～60 nm in size, were synthesized via a triphenylphosphine-assisted hydrothermal method. Scanning electron micrograph (SEM) and transmission electron micrograph (TEM) analyses showed that the as-synthesized rhombohedral nanoparticles were enclosed by six (1 0 4) planes. The concentration of triphenylphosphine played an important role in morphological evolution of the α-Fe₂O₃ nanoparticles. The as-prepared rhombohedral nanoparticles possessed remanent magnetization M_r of 2.6 × 10^?3 emu/g and coercivity H_C of 2.05 Oe, both lower than those of other α-Fe₂O₃ particles with similar size, indicating their potential applications as superparamagnetic precursor materials. Furthermore, these rhombohedral α-Fe₂O₃ nanoparticles exhibited good sensor capability toward H₂O₂ with a linear response in the concentration range of 2–20 mM.     

Synthesis and phase evolution of LiNb0.6Ti0.5O3 powder via a sol–gel method

A simple sol–gel route was demonstrated for the synthesis of LiNb_0.6Ti_0.5O₃ (M-phase) powder, using cheap and manageable starting materials at a relatively low temperature. The phase transitions in both chemical and solid-state processes were studied by X-ray diffraction (XRD) in detail. The results showed that in the sol–gel process the anatase TiO₂ phase first appeared at 400 °C and then LiNbO₃ solid solution (LiNbO₃ ss) emerged at 500 °C. When calcined to 600 °C, the M-phase started to appear along with the decrease of TiO₂ and LiNbO₃ ss. Single M-phase could be formed at 700 °C, which is 300 °C lower than that by the traditional solid-state method. A plausible evolution mechanism of the as-synthesized powder in calcination was proposed. The produced powder has potential applications in microelectronics systems.     

Hydrothermal synthesis of Mn-Zn ferrites from spent alkaline Zn-Mn batteries

Nanocrystalline Mn-Zn ferrites （Mno.GZno.4Fe204） with particle size of 12 nm were synthesized hydrotherreally using spent alkaline Zn-Mn batteries, and accompanied by a study of the influencing factors. The nanocrystals were examined by powder X-ray diffraction （XRD） for crystalline phase identification, and scanning electron microscopy （SEM） for grain morphology. The relationship between concentration of Fe（II）, Mn（II）, and Zn（II） and pH value was obtained through thermodynamic analysis of the Fe（II）-Mn（II）-Zn（II）-NaOH-H2O system. The results showed that all ions were precipitated completely at a pH value of 10-11. The optimal preparation conditions are： co-precipitation pH of 10.5, temperature of 200 ℃ and time of 9 h.     

Preparation and gas sensing performances of palladium surface-modified flower-like SnO2 nanopowders

Flower-like SnO2 nanopowders prepared by a hydrothermal method were surface modified with palla- dium via impregnation. The crystal structure, morphology, and surface chemistry states of the samples were characterized by means of X-ray diffraction （XRD）, scanning electron microscopy （SEM）, and X-ray photoelectron spectroscopy （XPS）, respectively. The gas sensing performances were also investigated. For a hydrothermal temperature of 220 ℃, flower-like SnO2 nanoparticles consist of nanorods with diameters of 40 nm and lengths of 100 nm. The XPS and XRD results reveal that palladium exists in the Pd0 chemical state but the crystal is too small to be detected. The 0.3 wt% Pd modified SnO2 sensor shows better sensi- tivity, up to 21, for 70 μL/L ethanol gas at an optimal working temperature of 250 ℃. The quick response time （3 s） and fast recovery time （-20 s） are the main characteristics of this sensor.     

TiO2-loaded activated carbon fiber: Hydrothermal synthesis,adsorption properties and photo catalytic activity under visible light irradiation

TiO₂-loaded activated carbon fibers (ACF) were prepared by a hydrothermal method. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrometry and UV–vis diffuse reflectance spectra (DRS). SEM images showed that the TiO₂ nanoparticles were deposited on the surface of ACF, and the particle size and loading amount of TiO₂ were varied by changing the initial concentration of tetrabutyl titanate (TBOT). The results of an ash experiment showed that the loading amounts of TiO₂ were 18.4%, 43.3%, 52.5%, 75.1%, and 91.1% for initial concentrations of TBOT of 0.07, 014, 0.21, 0.28, and 0.35 mol/L, respectively. Physical interactions played an important role in the formation of TiO₂/ACF composite fibers that absorb UV and visible light. Compared with those of ACF, improved adsorption and photocatalytic activity toward Rhodamine B (RhB) were observed for TiO₂/ACF composite fiber. The Rhodamine B could be removed efficiently by TiO₂/ACF composite fibers, and the TiO₂ loading amount had a significant effect on the photocatalytic activity of TiO₂/ACF composite fibers.     

Comparison of the effects of measured and computed thermophysical properties of nanofluids on heat transfer performance

This article reports a comparison of the differences between using measured and computed thermophysical properties to describe the heat transfer performance of TiO₂–water nanofluids. In this study, TiO₂ nanoparticles with average diameters of 21 nm and a particle volume fraction of 0.2–1 vol.% are used. The thermal conductivity and viscosity of nanofluids were measured by using transient hot-wire apparatus and a Bohlin rotational rheometer, respectively. The well-known correlations for calculating the thermal conductivity and viscosity of nanofluids were used for describing the Nusselt number of nanofluids and compared with the results from the measured data. The results show that use of the models of thermophysical properties for calculating the Nusselt number of nanofluids gave similar results to use of the measured data. Where there is a lack of measured data on thermophysical properties, the most appropriate models for computing the thermal conductivity and viscosity of the nanofluids are the models of Yu and Choi and Wang et al., respectively.     

Synthesis and characterization of BaMgAl10O17：Eu2＋ phosphor prepared by homogeneous precipitation

A homogeneous precipitation process based on urea hydrolysis reaction was exploited to synthesize BaMgAl10O17：Eu2＋ phosphor. The process parameters, such as the dosage of urea, the calcination tem- peratures and the concentration of Eu2＋, were refined in light of the characterization of the products. The experimental results revealed that pure and well-crystallized BaMgAl10O17：Eu2＋ phosphor could be obtained at 1250℃, a much lower temperature than that for traditional solid-state reaction. The as-prepared phosphor particles were small in grain size, regular in morphology, and uniform in size distribution. Because of the high homogeneity of the process, the as-prepared phosphor exhibited stronger emission intensity and higher thermal stability than the sample prepared by solid-state reaction at 1600℃.     

Interaction between Weibull parameters and mechanical strength reliability of industrial-scale water gas shift catalysts

A fundamental step in the production of an industrial catalyst is its crushing strength assessment. Limited literature exists in which the strength reliability of supported catalysts is investigated from production to their application in a reactor. In this work, cylindrical supports were prepared by pelletizing high porosity γ-alumina powder, and Cu–Zn/γ-Al₂O₃ catalysts were prepared by impregnation of the pelletized γ-alumina supports with an aqueous solution of copper and zinc nitrates. The support-forming variables, such as binder concentration, compaction pressure, calcination temperature, and drying procedure were investigated. The Weibull method was used to analyze the crushing strength data of the supports, and the fresh and used catalysts before and after the low-temperature water gas shift reaction. Support formation at a 50 wt% binder concentration, 1148 MPa compaction pressure, 500 °C calcination temperature, and rapid drying (100 °C, 8 h) led to the maximum support mechanical reliability. The most reliable catalyst with respect to simultaneous appropriate catalytic performance and mechanical strength was prepared from a support with the lowest mean crushing strength (26.25 MPa). This work illustrates the importance of the Weibull modulus as a useful mechanical reliability index in manufacturing a supported solid catalyst.