Surface effect of natural zeolite (clinoptilolite) on the photocatalytic activity of TiO2

The surface interaction between TiO₂ and natural zeolite, clinoptilolite, has been investigated by means of transmission electron microscope (TEM), atom force microscope (AFM), X-ray diffractometer (XRD), diffuse reflectance infrared Fourier transform (DRIFT) and far Fourier transform infrared ray (FTIR) spectroscopy. And the photocatalytic degradation (PCD) rate of methyl orange (MO), a model of recalcitrant azo dye, in aqueous system has been measured to compare the photocatalytic activities of different photocatalysts. A model has been carried out to explain the incorporation between TiO₂ particles and natural zeolite. The results show that the TiO₂ particles loaded on zeolite are 50 nm or so, smaller than the pure one, and combine with zeolite via chemical force. Since the reserved adsorption ability and the existence of electron trapper, the TiO₂-zeolite performed more efficient at low initial concentration and in the later period of PCD process, as compared with pure TiO₂ nanopowders.     

Preparation and characterization of hexadecyl functionalized magnetic silica nanoparticles and its application in Rhodamine 6G removal

In this paper, a new adsorbent, hexadecyl functionalized magnetic silica nanoparticles (C₁₆/SiO₂-Fe₃O₄ NPs), was prepared by a facile method. The final product was characterized by X-ray diffractometer, transmission electron microscope, Fourier transform infrared spectrometer and vibration sample magnetometer. The preparation and adsorption conditions of the adsorbent were optimized. The adsorbent prepared maintaining volume ratio of tetraethylorthosilicate to hexadecyltrimethoxysilane at 1:0.5 and their total volume at 1100 μL exhibited high adsorption capacity. The optimum pH value for the adsorption experiments was 11.00. The adsorption behavior of Rhodamine 6G onto C₁₆/SiO₂-Fe₃O₄ NPs obeyed pseudo-second-order kinetic model and Langmuir isotherm. Thermodynamic data indicated that the adsorption process was spontaneous and exothermic. The adsorption capacity of the adsorbent could reach to 35.6 mg g⁻¹, owing to the hydrophobic attraction and the enhanced electrostatic attraction. The saturation magnetization of the magnetic adsorbent was 35 emu g⁻¹, which ensured the magnetic separation after adsorption.     

Synthesis of magnetic γ-Fe2O3-based nanomaterial for ultrasonic assisted dyes adsorption: Modeling and optimization

γ-Fe₂O₃ nanoparticles were synthesized and loaded on activated carbon. The prepared nanomaterial was characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transforms infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The γ-Fe₂O₃ nanoparticle-loaded activated carbon (γ-Fe₂O₃-NPs-AC) was used as novel adsorbent for the ultrasonic-assisted removal of methylene blue (MB) and malachite green (MG). Response surface methodology and artificial neural network were applied to model and optimize the adsorption of the MB and MG in their individual and binary solutions followed by the investigation on adsorption isotherm and kinetics. The individual effects of parameters such as pH, mass of adsorbent, ultrasonication time as well as MB and MG concentrations in addition to the effects of their possible interactions on the adsorption process were investigated. The numerical optimization revealed that the optimum adsorption (>99.5% for each dye) is obtained at 0.02 g, 15 mg L⁻¹, 4 min and 7.0 corresponding to the adsorbent mass, each dye concentration, sonication time and pH, respectively. The Freundlich, Langmuir, Temkin and Dubinin–Radushkevich isotherms were studied. The Langmuir was found to be most applicable isotherm which predicted maximum monolayer adsorption capacities of 195.55 and 207.04 mg g⁻¹ for the adsorption of MB and MG, respectively. The pseudo-second order model was found to be applicable for the adsorption kinetics. Blank experiments (without any adsorbent) were run to investigate the possible degradation of the dyes studied in presence of ultrasonication. No dyes degradation was observed.     

Preparation of mesoporous poly (acrylic acid)/SiO2 composite nanofiber membranes having adsorption capacity for indigo carmine dye

Mesoporous poly (acrylic acid)/SiO₂ (PAA/SiO₂) composite nanofiber membranes functionalized with mercapto groups were fabricated by a sol-gel electrospinning method, and their adsorption capacity for indigo carmine was investigated. The membranes were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, x-ray powder diffraction (XRD), and nitrogen adsorption–desorption measurement. SEM and TEM observation results showed that the PAA/SiO₂ fibers had diameters between 400–800 nm and mesopores with an average pore size of 3.88 nm. The specific surface area of the mesoporous nanofiber membranes was 514.89 m²/g. The characteristic peaks for mercapto group vibration in FTIR and Raman spectra demonstrated that the mercapto groups have been incorporated into the silica skeleton. The adsorption isotherm data of indigo carmine on the membranes fit well with Redlich–Peterson model, and the maximum adsorption capacity calculated was 523.11 mg/g. It was found that the removal rate of indigo carmine by the membranes reached a maximum of 98% in 90 min and the adsorption kinetics followed a pseudo-second-order model. The high adsorption capacity of PAA/SiO₂ nanofiber membrane makes it a promising adsorbent for indigo carmine removal from the wastewater.     

Synthesis and characterization of Co3O4 nanorods by thermal decomposition of cobalt oxalate

Cobalt oxalate was used as a precursor to prepare Co₃O₄ nanorods by thermal decomposition. The combinations of triphenylphosphine and oleylamine were added as surfactants to control the morphology of the particles. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The diameters of Co₃O₄ nanorods are 20 nm and the average lengths are around 500 nm. The hysteresis loops of the obtained samples reveal the ferromagnetic behaviors, the enhanced coercivity (H_c) and decreased saturation magnetization (M_s) in contrast to their respective bulk materials. The study provides a simple and efficient route to synthesize Co₃O₄ nanorods at low temperature.     

Adsorption and interaction of organosilanes on TiO2 nanoparticles

Organosilanes with different organic functional groups are precursors of corresponding organosilanol which can be attached to the surface of oxide nanoparticles by silyation. In this work, surface of commercial TiO₂ nanoparticles was modified by 3-aminopropyltrimethoxysilane (APS) and phenyltrimethoxysilane (PTMS) through an aqueous process. The amount of adsorbed organosilane was evaluated by energy dispersive X-ray spectroscopy and was found to be 3 times higher on PTMS treated sample than on APS treated sample. The orientation and bonding of the molecules on particle surface was analyzed using Fourier transform infrared spectroscopy and time-of-flight secondary ion mass spectrometry. The obtained data confirmed that bonding of organosilanols on particle surface was realized through Si-O-Ti bonds and organic functional groups were extended away from particle surface on both APS and PTMS modified particles. It was found that phenylsilanol molecules are cross-linked to each other through Si-O-Si bonds, while such bonds are very little to none between aminosilanol molecules. A model of adsorption is proposed to explain these observations.     

Adsorption of biodegradable chelating compounds on inorganic oxides

The Fourier transform infrared photoacoustic spectroscopy (FT-IR/PAS) method to characterize the interactions between selected aminopolycarboxylic acids and inorganic oxides surfaces is reviewed. In this work, the adsorption of four aminopolycarboxylates (biodegradable and with augmented biodegradability; all in the form of sodium salts), viz. ethylenediaminedisuccinic (EDDS), diethylenetriaminepentaacetic (DTPA), N-(hydroxyethyl)ethylenediaminetriacetic (HEDTA) and methylglycinediacetic (MGDA) acids on: zirconia, titania and alumina was carried out. The obtained results differ depending on the kind of aminopolycarboxylic acid used and the type of oxide support adsorbent characterized by its pH_PZC value.     

Synthesis of thiol-functionalized MCM-41 mesoporous silicas and its application in Cu(II), Pb(II), Ag(I), and Cr(III) removal

Thiol-functionalized MCM-41 mesoporous silicas were synthesized via evaporation-induced self-assembly. The mesoporous silicas obtained were characterized by X-ray diffraction (XRD), nitrogen adsorption–desorption analysis, Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The products were used as adsorbents to remove heavy metal ions from water. The mesoporous silicas (adsorbent A) with high pore diameter (centered at 5.27 nm) exhibited the largest adsorption capacity, with a BET surface area of 421.9 m² g^?1 and pore volume of 0.556 cm³ g^?1. Different anions influenced the adsorption of Cu(II) in the order NO₃ ^? < OAc^? < SO₄ ^2? < CO₃ ^2? < Cit^? < Cl^?. Analysis of adsorption isotherms showed that Cu²⁺, Pb²⁺, Ag⁺, and Cr³⁺ adsorption fit the Redlich–Peterson nonlinear model. The mesoporous silicas synthesized in the work can be used as adsorbents to remove heavy metal ions from water effectively. The removal rate was high, and the adsorbent could be regenerated by acid treatment without changing its properties.     

Spherical Zn2SiO4:Eu@SiO2 phosphor particles in core-shell structure: Synthesis and characterization

Spherical SiO₂ particles have been coated with Zn₂SiO₄:Eu³⁺ phosphor layers by a Pechini sol-gel process. The microstructure and luminescent properties of the obtained Zn₂SiO₄:Eu³⁺@SiO₂ particles were well characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra, and lifetime. The results demonstrate that the Zn₂SiO₄:Eu³⁺@SiO₂ particles, which have regular and uniform spherical morphology, emitted an intensive red light emission at 613 nm under excitation at 395 nm. Besides, the effects of the Eu³⁺ concentration, annealing temperature and charge compensators of Li⁺ ions on the PL emission intensities were investigated in detail.     

Synthesis of Fe3O4/CNTs magnetic nanocomposites at the liquid-liquid interface using oleate as surfactant and reactant

Carbon nanotubes (CNTs)-based magnetic nanocomposites have attracted significant research interest owing to their great potentialities in various technological fields. In this investigation, a kind of novel Fe₃O₄/CNTs magnetic nanocomposites were prepared by in situ chemical precipitation using oleate as reactant and surfactant at the liquid-liquid interface of cyclohexane/ethanol/water mixture solvent. The as-prepared samples were characterized via transmission electron microscopy (TEM), X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) and vibration sample magnetometry (VSM). Results indicated that the Fe₃O₄/CNTs magnetic nanocomposites dispersed well in organic medium were prepared organic medium, were prepared. The magnetic nanocomposites were proved to be superparamagnetic with coercive force of 3.69 Oe. A mechanism scheme was proposed to illustrate the formation process of the magnetic nanocomposites.     

Synthesis, infrared and microwave absorbing properties of (BaFe12O19+BaTiO3)/polyaniline composite

The (BaFe₁₂O₁₉+BaTiO₃)/polyaniline composite was synthesized by in situ polymerization and introduced into epoxy resin and polyethylene to be a microwave and infrared absorber. The spectroscopic characterizations of the formation processes of (BaFe₁₂O₁₉+BaTiO₃)/polyaniline composite were examined using Fourier transform infrared, ultraviolet-visible spectrophotometer, X-ray diffraction, scanning electron microscopy, transmission electron microscopy and electron spin resonance. Microwave absorbing properties were investigated by measuring reflection loss in 2-18 and 18-40 GHz microwave frequency range using the free space method. Thermal extinction measurements in the 3-5 and 8-12 μm were done to evaluate the shielding effectivity of infrared. The results showed that a significant absorption frequency range shifting and thermal extinction could be obtained by adding polyaniline to the BaFe₁₂O₁₉+BaTiO₃ blend.     

Dendrimer-conjugated magnetic nanoparticles for removal of zinc (II) from aqueous solutions

Dendrimers are novel nanostructure materials that possess a unique three-dimensional molecular configuration. They have high adsorption capacities of heavy metals. Dendrimer-conjugated magnetic nanoparticles (Gn-MNPs) combining the superior adsorbent of dendrimers with magnetic nanoparticles (MNPs) have been developed for effective removal and recovery of Zn(II). In this study, the Gn-MNPs were synthesized, characterized, and examined as reusable adsorbents of Zn(II). Characterization conducted by transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and elemental analysis revealed that dendrimers were successfully coated onto the surface of MNPs made of magnetite (Fe₃O₄). The pH effect studies indicate the Zn(II) adsorption with Gn-MNPs is a function of pH. The adsorption efficiency increases with increasing pH. At pH less than 3, Zn(II) is readily desorbed. Hence, the Gn-MNPs can be regenerated using the diluted HCl aqueous solution (0.1 M) where Zn(II) can be recovered in a concentrated form. It was found that the Gn-MNPs underwent 10 consecutive adsorption–desorption processes still retained the original removal capacity of Zn(II). The adsorption data were fitted well with both Langmuir and Freundlich isotherms. The maximum adsorption capacity determined by the Langmuir model is 24.3 mg/g at pH 7 and 25°C. A synergistic effect between the complexation reaction and the electrostatic interaction may account for the overall performance of Gn-MNPs.     

Nanofibers and nanoplatelets of MoO3 via an electrospinning technique

Polyvinyl alcohol (PVA)/ammonium molybdate composite fibers were prepared by using sol-gel processing and electrospinning technique. After calcinations of the above precursor fibers at 500 °C, MoO₃ nanofibers with a diameter of 100-150 nm were successfully obtained. MoO₃ nanoplatelets and submicron platelets were prepared by further calcinations of the MoO₃ nanofibers at 600 and 700 °C. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). A possible growth mechanism for the MoO₃ nanofibers and nanoplatelets was suggested.     

Microwave-assisted synthesis and optical property of CdMoO4 nanoparticles

Microwave-assisted synthesis is a novel method used to synthesize CdMoO₄ nanoparticles in propylene glycol. The effects of reaction time and microwave power on phase, morphologies, and optical properties of CdMoO₄ nanoparticles were studied, using X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and UV-visible spectroscopy. The present analyses proved that these crystalline powders were scheelite-type tetragonal structured CdMoO₄, with the crystallite size of 14-20 nm, and 4.51-4.73 eV band gaps, controlled by the synthetic conditions.     

In vitro evaluation of bioactivity of CaO-SiO2-P2O5-Na2O-Fe2O3 glasses

Glasses with compositions 41CaO(52 − x)SiO₂4P₂O₅·xFe₂O₃3Na₂O (2 ≤ x ≤ 10 mol.%) were prepared by melt quenching method. Bioactivity of the different glass compositions was studied in vitro by treating them with simulated body fluid (SBF). The glasses treated for various time periods in SBF were evaluated by examining apatite formation on their surface using grazing incidence X-ray diffraction, Fourier transform infrared reflection spectroscopy, scanning electron microscopy and energy dispersive spectroscopy techniques. Increase in bioactivity with increasing iron oxide content was observed. The results have been used to understand the evolution of the apatite surface layer as a function of immersion time in SBF and glass composition.     

Effect of calcination temperature on the structure and hydroxylation activity of Ni0.5Cu0.5Fe2O4 nanoparticles

Nanocrystalline Ni_0.5Cu_0.5Fe₂O₄ was synthesized by sol-gel method with varying calcination temperature over the range of 500-1000. The powders obtained were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). In addition, thermal analysis (TG-DTG-DTA) of the precursor was carried out. The study reveals the simultaneous decomposition and ferritization process at rather low temperature (280-350). For the crystalline structure investigated, single cubic spinel is gained when the precursor was decomposed at 800-1000, whereas separated crystal CuO formed when calcination temperature is below 800. The increase of calcination temperature favors the appearance of Fe_B³⁺, Cu_A²⁺ and O on the spinel surface. The hydroxylation activity is relative to the amount of Cu_B²⁺ species on the spinel surface. The lattice oxygen species on the spinel surface are favorable for the deep oxidation of phenol.     

Investigate the ultrasound energy assisted adsorption mechanism of nickel(II) ions onto modified magnetic cobalt ferrite nanoparticles: Multivariate optimization

In present study, magnetic cobalt ferrite nanoparticles modified with (E)-N-(2-nitrobenzylidene)-2-(2-(2-nitrophenyl)imidazolidine-1-yl) ethaneamine (CoFe₂O₄-NPs-NBNPIEA) was synthesized and applied as novel adsorbent for ultrasound energy assisted adsorption of nickel(II) ions (Ni²⁺) from aqueous solution. The prepared adsorbent characterized by Fourier transforms infrared spectroscopy (FT-IR), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and X-ray diffraction (XRD). The dependency of adsorption percentage to variables such as pH, initial Ni²⁺ ions concentration, adsorbent mass and ultrasound time were studied with response surface methodology (RSM) by considering the desirable functions. The quadratic model between the dependent and independent variables was built. The proposed method showed good agreement between the experimental data and predictive value, and it has been successfully employed to adsorption of Ni²⁺ ions from aqueous solution. Subsequently, the experimental equilibrium data at different concentration of Ni²⁺ ions and 10 mg amount of adsorbent mass was fitted to conventional isotherm models like Langmuir, Freundlich, Tempkin, Dubinin-Radushkevich and it was revealed that the Langmuir is best model for explanation of behavior of experimental data. In addition, conventional kinetic models such as pseudo-first and second-order, Elovich and intraparticle diffusion were applied and it was seen that pseudo-second-order equation is suitable to fit the experimental data.     

Effect of Fe2O3 nanoparticles on combustion of coal surrogate (Anisole): Enhanced ignition and formation of persistent free radicals

This contribution explores the effect of nanoparticles of iron (III) oxide (Fe₂O₃) on the combustion of coal surrogate, i.e., anisole, identifying the changes in ignition features as well as the occurrence of persistent organic pollutants in the initiation channels. The method applies packed-bed reactor coupled with Fourier transform infrared (FTIR) spectroscopy to quantitate the ignition temperature under typical fuel-rich conditions, in-situ electron paramagnetic resonance (EPR) to elucidate the formation of environmentally-persistent free radicals (EPFR), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) to monitor the chemisorption of organic substrates on the nanoparticles, as well as X-ray diffraction for particles characterisation (PXRD). We employ cluster-based quantum mechanical calculation to map the reaction pathway within the scope of the density functional theory. The results of Fe₂O₃-mediated combustion of anisole depict an excessive reduction in ignition temperature from 500?°C around 220?°C at λ?=?0.8. As confirmed both from EPR and DRIFTS measurements, the chemisorption of anisole on α-Fe₂O₃ surfaces follows the direct dissociation of the O–CH₃ (and OCH₂–H), leading to the formation of surface-bound phenoxy radicals at temperatures as low as 25?°C and incurring an estimated energy barrier of E_a?=?18?kJ mol^?1 and a preexponential factor of A?=?2.7?×?10¹² M^?1 s^?1. This insight applies to free-radical chain reactions that induce spontaneous fires of coal, as coal comprises ferric oxide nanoparticles, and equally to coexistence of aromatic fuels with thermodynamically reactive Fe₂O₃ surface, e.g., in fly ash, at the cooled-down tail of combustion stacks.     

Removal of organic dye by air and macroporous ZnO/MoO3/SiO2 hybrid under room conditions

A new macroporous ZnO/MoO₃/SiO₂ hybrid was synthesized by a method involving sol-gel technology and biomimetic synthesis. It was characterized by Elemental analysis, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-ray photoelectron spectrum (XPS) and scanning electron microscopy (SEM). Chemical degradation of 0.3 g/L Safranin T (ST) by air oxidation over macroporous ZnO/MoO₃/SiO₂ hybrid was studied. It was found that the decolorization efficiency and the chemical oxygen demand (COD) removal of ST reached above 95.3% and 93.2%, respectively, within 25 min at room temperature and atmospheric pressure. And the organic pollutant was mineralized to simple inorganic species such as HCO₃⁻, Cl⁻ and NO₃⁻, while the total organic carbon (TOC) decreased 95.4%. The structure and morphology of the catalyst were still stable after six cycling runs and the leaching test showed negligible leaching effect.     

Preparation and characterization of silica-coated Fe3O4 nanoparticles used as precursor of ferrofluids

Fe₃O₄ magnetic nanoparticles (MNPs) were synthesized by the co-precipitation of Fe³⁺ and Fe²⁺ with ammonium hydroxide. The sodium citrate-modified Fe₃O₄ MNPs were prepared under Ar protection and were characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and vibrating sample magnetometer (VSM). To improve the oxidation resistance of Fe₃O₄ MNPs, a silica layer was coated onto the modified and unmodified MNPs by the hydrolysis of tetraethoxysilane (TEOS) at 50 °C and pH 9. Afterwards, the silica-coated Fe₃O₄ core/shell MNPs were modified by oleic acid (OA) and were tested by IR and VSM. IR results revealed that the OA was successfully grafted onto the silica shell. The Fe₃O₄/SiO₂ core/shell MNPs modified by OA were used to prepare water-based ferrofluids (FFs) using PEG as the second layer of surfactants. The properties of FFs were characterized using a UV-vis spectrophotometer, a Gouy magnetic balance, a laser particle size analyzer and a Brookfield LVDV-III+ rheometer.