In situ preparation of hydrophobic CaCO3 nanoparticles in a gas–liquid microdispersion process

This study presents a novel process of in situ surface modification of CaCO₃ nanoparticles using a multiple-orifice dispersion microreactor. CO₂/Ca(OH)₂ precipitation reaction was employed to prepare CaCO₃ nanoparticles with sodium stearate surfactant. Synthesized CaCO₃ products were characterized by thermogravimetric analysis (TGA), infra-red (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and Brunauer–Emmet–Teller analysis (BET). The effect of various operation parameters on nanoparticles and the dosage of sodium stearate were determined. The results showed that the preparation process could be precisely controlled with efficient mass transfer process. The particles were highly hydrophobic with a contact angle of 117° and monodisperse with an average size of 30 nm. The adsorptions of sodium stearate and calcium ion on solid particles during the in situ surface modification process were investigated.     

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.     

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.     

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.     

Programmed nanoparticle-loaded microparticles for effective antigen/adjuvant delivery

A microscale vaccine containing SiO2 nanoparticles loaded in CaCO3 microparticles was constructed using the co-precipitation method.The antigen ovalbumin(OVA)wa...     

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.     

Novel synthesis with an atomized microemulsion technique and characterization of nano-calcium carbonate （CaCO3）/poly（methyl methacrylate） core-shell nanoparticles

The synthesis of hard-core/soft-shell calcium carbonate （CaCO3）/poly（methyl methacrylate） （PMMA） hybrid structured nanoparticles （〈100nm） by an atomized microemulsion polymerization process is reported. The polymer chains were anchored onto the surface of nano-CaCO3 through use of a cou- pling agent, triethoxyvinyl silane （TEVS）. Ammonium persulfate （APS）, sodium dodecyl sulfate （SDS） and n-pentanol were used as the initiator, surfactant and cosurfactant, respectively. The polymeriza- tion mechanism of the core-shell latex particles is discussed. The encapsulation of nano-CaCO3 by PMMA was confirmed using a transmission electron microscope （TEM）. The grafting percentage of the core-shell particles was investigated by thermogravimetric analysis （TGA）. The nano-CaCO3/PMMA core-shell par- ticles were characterized by Fourier transform infrared （FTIR） spectroscopy and differential scanning calorimetry （DSC）. The FTIR results revealed the existence of a strong interaction at the interface of the nano-CaCO3 particle and the PMMA, which implies that the polymer chains were successfully grafted onto the surface of the nano-CaCO3 particles through the link of the coupling agent, In addition, the TGA and DSC results indicated an enhancement of the thermal stability of the core-shell materials compared with that of the pure nano-PMMA, The nano-CaCO3/PMMA particles were blended into a polypropylene （PP） matrix by melt processing. It can also be observed using scanning electron microscopy （SEM） that the PMMA chains grafted onto the CaCO3 nanoparticles interfere with the aggregation of CaCO3 in the polymer matrix （PP matrix） and thus improve the compatibility of the CaCO3 nanoparticles with the PP matrix.     

Electrosynthesis and catalytic properties of silver nano/microparticles with different morphologies

Electrosynthesis of powdery silver particles can be effectively carried out with an H₂O–oleic acid or an H₂O–glycerol mix solvent (volume ratio 1:1) as the electrolytic medium and AgNO₃ as the supporting electrolyte. Experimental results indicate that the presence or absence of the surfactant sodium dodecyl sulfate (SDS) and the choice of electrolytic medium have a significant impact on the shape and size of the prepared Ag particles. With H₂O–glycerol as the electrolytic medium, spherical Ag nanoparticles can be obtained in the presence of SDS (0.6 g/L), while an Ag sample electrodeposited without SDS has a dendritic microcrystalline structure. For the reduction of methyl orange (MO) and methylene blue (MB) with NaBH₄ as the reducing agent, the spherical Ag nanoparticles exhibit much better catalytic activity than the dendritic Ag microparticles. Further investigations show that surface modification by an oleic acid medium could greatly improve the catalytic activity of the electrodeposited Ag particles for the reduction of MO and MB.     

Wear and performance analysis of a 4-stroke diesel engine employing nanolubricants

In the present study, the performance of a 4-stroke diesel engine was experimentally evaluated upon adding Al₂O₃ or SiO₂ nanoparticles to the engine oil (SAE15W40). The viscosity and density of the resulting nanolubricants were determined while varying both the nanoparticle volume fraction and the temperature. Field emission scanning electron microscopy (FE–SEM) showed that the nanoparticles had a spherical morphology and dynamic light scattering analysis determined some aggregation of the nanoparticles in the engine oil. A pin-on-disc test apparatus was used for friction and wear analysis in the presence of the nanolubricants. Examination of wear scars by FE–SEM and energy dispersive spectroscopy found evidence of ball bearing and surface polishing effects, which were responsible for improvements in the tribological properties of the oil. The performance of these nanolubricants in a 4-stroke diesel engine test rig was assessed, and the greatest improvements in the tribological behavior and engine performance were observed when employing 0.3 vol% Al₂O₃.     

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.     

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.     

Mesoporous composite of LiFePO4 and carbon microspheres as positive-electrode materials for lithium-ion batteries

Mesoporous LiFePO₄/C microspheres consisting of LiFePO₄ nanoparticles are successfully fabricated by an eco-friendly hydrothermal approach combined with high-temperature calcinations using cost-effective LiOH and Fe³⁺ salts as raw materials. In this strategy, pure mesoporous LiFePO₄ microspheres, which are composed of LiFePO₄ nanoparticles, were uniformly coated with carbon (∼1.5 nm). Benefiting from this unique architecture, these mesoporous LiFePO₄/C microspheres can be closely packed, having high tap density. The initial discharge capacity of LiFePO₄/C microspheres as positive-electrode materials for lithium-ion batteries could reach 165.3 mAh/g at 0.1 C rate, which is notably close to the theoretical capacity of LiFePO₄ due to the large BET surface area, which provides for a large electrochemically available surface for the active material and electrolyte. The material also exhibits high rate capability (∼100 mAh/g at 8 C) and good cycling stability (capacity retention of 92.2% after 400 cycles at 8 C rate).     

Highly dispersed Mn2O3 microspheres: Facile solvothermal synthesis and their application as Li-ion battery anodes

Nanostructured transition metal oxides are promising alternative anodes for lithium ion batteries. Li-ion storage performance is expected to improve if high packing density energy particles are available. Herein, Mn₂O₃ microspheres with a ca. 18 μm diameter and a tapped density of 1.33 g/cm³ were synthesized by a facile solvothermal–thermal coversion route. Spherical MnCO₃ precursors were obtained through solvothermal treatment and they decomposed and converted into Mn₂O₃ microspheres at an annealing temperature of 700 °C. The Mn₂O₃ microspheres consisted of Mn₂O₃ nanoparticles with an average 40 nm diameter. These porous Mn₂O₃ microspheres allow good electrolyte penetration and provide an ion buffer reservoir to ensure a constant electrolyte supply. The Mn₂O₃ microspheres have reversible capacities of 590 and 320 mAh/g at 50 and 400 mA/g, respectively. We thus report an efficient route for the fabrication of energy particles for advanced energy storage.     

SiO2-coated pure anatase TiO2 catalysts for enhanced photo-oxidation of naphthalene and anthracene

Our current efforts reveal the preparation of SiO₂@TiO₂ nanocomposites having different thicknesses of silica shell and the relationship to photocatalytic activity (PCA) for the photo-oxidation of naphthalene and anthracene. The presence of SiO₂ coating over TiO₂ surface was demonstrated by FT-IR analysis, with peaks corresponding to SiOSi (1081 cm⁻¹) and SiOTi (950 cm⁻¹) bonds observed. High-resolution transmission electron microscopy analysis confirmed the presence of SiO₂ in the as-prepared nanocomposites and the amount of Si, Ti, and O was determined by energy dispersive X-ray spectroscopy analysis. Increasing the SiO₂ shell thickness increases the surface area of the nanocomposites (69–235 m²/g), which enhances naphthalene/anthracene adsorption. However, the observed PCA trend presents an inverse correlation to the adsorption studies, where the as-prepared samples possessing the highest surface areas exhibited the least PCA, while catalysts having lower surface areas (among silica coated samples) displayed the highest PCA in the degradation of naphthalene and anthracene to CO₂. Despite complete degradation of naphthalene and anthracene, incomplete mineralization occurred, ascribed to the formation of various intermediates, identified by GC–MS analysis.     

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%.     

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.     

Preparation of nano-sized Al2O3–2SiO2 powder by sol–gel plus azeotropic distillation method

Nano-sized amorphous Al₂O₃–2SiO₂ powder was prepared by a sol–gel method coupled with azeotropic distillation. The structure of the powder was investigated by DTS, BET, TEM, FT-IR, TG-DTA and XRD, showing that n-butanol azeotropic distillation could effectively remove water from the aluminosilicate gels and prevent the formation of hard agglomerates in the drying process. The average particle diameter of the powder was about 70 nm. The largest BET specific surface area of the powder was 669 m²/g. To examine the alkali-activation reactivity of the powder, alkali-activation tests were performed with the powder reacting with sodium silicate solution. The synthetic powder was found to be highly reactive.     

Preparation of nanosized hollow silica spheres from Na2SiO3 using Fe3O4 nanoparticles as templates

Nanosized hollow silica spheres with average diameters from 43 to 70 nm were prepared by removal of Fe₃O₄ templates with hydrochloric acid from silica-coated Fe₃O₄ core–shell composites. The shells of the hollow silica spheres had nanopores with average diameters of 0.92–1.25 nm. When the silica-coated Fe₃O₄ core–shell composites were prepared at a high pH value or with a low mole ratio of Na₂SiO₃ to Fe₃O₄, the resulting hollow silica spheres consisted of highly porous shells. When the silica-coated Fe₃O₄ core–shell composites were prepared with a high mole ratio of Na₂SiO₃ to Fe₃O₄, the resulting hollow silica spheres had large diameters and thick shells. The release rate of herbicide, ammonium glyphosate, could be tuned by using hollow silica spheres with different shell thicknesses.     

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.