Solvent-deficient synthesis of cerium oxide: Characterization and kinetics

The reaction mechanism and kinetics of CeO₂ synthesis using a solvent-deficient method are investigated by simultaneous thermogravimetric analysis (TGA)/differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The decomposition process of the cerium(III) nitrate hexahydrate and ammonium bicarbonate precursor mixture with four observed stages is monitored using TGA/DSC measurements in a nonisothermal regime with heating rates of 5, 10, 15 and 20?°C min^?1. The proposed mechanism indicates a complex synthesis with several parallel reactions, some of which occur at room temperature. A detailed kinetic analysis is performed using isoconversional (expanded Friedman, modified Coats-Redfern and Kissinger) and model fitting (N^th order and nucleation and growth models) methods. The first three stages are best described by the N^th order model with activation energy values of 21, 53 and 90?kJ?mol^?1. The last stage, during which ammonium nitrate decomposition occurs, is best fit by the nucleation and growth model and has an activation energy of 129?kJ?mol^?1. The proposed mechanism, supported by the kinetic analysis in our study, indicates that CeO₂ has already formed before the reaction reaches 200?°C. The average crystallite size of CeO₂ synthesized at 300?°C, which was calculated from the XRD measurements and observed in the SEM and TEM data, is between 10 and 20?nm.     

Plasma-electrochemical synthesis of europium doped cerium oxide nanoparticles

In the present study,a plasma-electrochemical method was demonstrated for the synthesis of europium doped ceria nanoparticles.Ce(NO3)3· 6H2O and Eu(NO3)3·5H2O were used as the starting materials and being dissolved in the distilled water as the electrolyte solution.The plasma-liquid interaction process was in-situ investigated by an optical emission spectroscopy,and the obtained products were characterized by complementary analytical methods.Results showed that crystalline cubic CeO2:Eu3+ nanoparticles were successfully obtained,with a particle size in the range from 30 to 60 nm.The crystal structure didn't change during the calcination at a temperature from 400℃ to 1000℃,with the average erystallite size being estimated to be 52 nm at 1000℃.Eu3+ ions were shown to be effectively and uniformly doped into the CeO2 lattices.As a result,the obtained nanophosphors emit apparent red color under the UV irradiation,which can be easily observed by naked eye.The photoluminescence spectrum further proves the downshift behavior of the obtained products,where characteristic 5Do → 7F1,2,3 transitions of Eu3+ ions had been detected.Due to the simple,flexible and environmental friendly process,this plasma-electrochemical method should have great potential for the synthesis of a series of nanophosphors,especially for bio-application purpose.     

Synthesis and encapsulation of magnetite nanoparticles in PLGA: effect of amount of PLGA on characteristics of encapsulated nanoparticles

Oleic acid-coated superparamagnetic iron oxide nanoparticles (Fe₃O₄) encapsulated within poly(d,l-lactide-co-glycolide) (PLGA) particles were prepared by the w/o/w emulsion technique using poly(vinyl alcohol) as a dispersant. The concentration of PLGA in the oil phase was varied (5, 15, 30, 45, and 60?mg/ml) at constant magnetite concentration in the oil phase (5?mg/ml) to study the properties of composite Fe₃O₄–PLGA nanoparticles. Even though PLGA concentration varied widely in the oil phase, the weight percent of 7–16?nm diameter magnetite in the particles varied only from 56 to 62?% (23–28?vol.%). The obtained composite nanoparticles were essentially spherical with magnetite spatially uniformly dispersed in individual PLGA particles, as measured by transmission electron microscopy (TEM). Also, the magnetite concentration in each particle did not vary widely as determined qualitatively via microscopy. Hydrodynamic diameters of the composite nanoparticles as measured by dynamic light scattering increased by approximately 10?% with added magnetite, with a smaller relative increase in diameter measured by TEM. The zeta potential of the particles was about ?26?mV, independent of Fe₃O₄ loading. Relatively high saturation magnetizations (36–45?emu/g) were measured for these highly loaded particles, with the latter value only 7?emu/g lower than the value measured for the oleic acid-coated particles alone.     

Solution combustion synthesis of cerium oxide nanoparticles as corrosion inhibitor

In this study, combustion synthesis of cerium oxide nanoparticles was reported using cerium nitrate hexahydrate as starting material as well as urea, glycine, glucose, and citric acid as fuels. The influence of fuel type on structure, microstructure, band gap, and corrosion inhibition was investigated. X-ray diffraction (XRD) patterns and scanning electron microscopy micrographs showed that CeO₂ nanoparticles with different morphologies were obtained depending on the fuel type. Microstructural changes from unreacted gel to sponge-like morphologies were resulted by varying the fuel type from urea, glycine, and glucose to citric acid. In addition to Ce–O bonds, Fourier transform infrared analysis showed carbon bonds of carbonaceous compositions from incomplete combustion which were declined during combustion reaction. Furthermore, corrosion analyses showed that samples synthesized using urea fuel released the most Ce⁺⁴ ions and could have better protection than other samples.     

Pharmacological potential of cerium oxide nanoparticles

Nanotechnology promises a revolution in pharmacology to improve or create ex novo therapies. Cerium oxide nanoparticles (nanoceria), well-known as catalysts, possess an astonishing pharmacological potential due to their antioxidant properties, deriving from a fraction of Ce(3+) ions present in CeO(2). These defects, compensated by oxygen vacancies, are enriched at the surface and therefore in nanosized particles. Reactions involving redox cycles between the Ce(3+) and Ce(4+) oxidation states allow nanoceria to react catalytically with superoxide and hydrogen peroxide, mimicking the behavior of two key antioxidant enzymes, superoxide dismutase and catalase, potentially abating all noxious intracellular reactive oxygen species (ROS) via a self-regenerating mechanism. Hence nanoceria, apparently well tolerated by the organism, might fight chronic inflammation and the pathologies associated with oxidative stress, which include cancer and neurodegeneration. Here we review the biological effects of nanoceria as they emerge from in vitro and in vivo studies, considering biocompatibility and the peculiar antioxidant mechanisms.     

Cytotoxic activity of greener synthesis of cerium oxide nanoparticles using carrageenan towards a WEHI 164 cancer cell line

Carrageenan hydrogel as a “greener” and a vegetable-based stabilizing agent has the potential for many biosyntheses of different nanoparticles by sol-gel method. Herein, we describe for the first time an economic and eco-friendly preparation of cerium oxide nanoparticles (CeO₂-NPs) using carrageenan. When carrageenan hydrogel comes in contact with a cerium nitrate solution, cerium ions anchor themselves to the –SO₃^- groups into the carrageenan and after the gelation process, have fewer opportunities escaping from the polymeric network. The CeO₂-NPs were well-prepared and successfully characterized by PXRD, FTIR, FESEM, UV–Vis, and TGA-DTA. The calcined CeO₂-NPs showed strong UV absorption (λ_max = 328?nm) with the calculated band gap of 2.69?eV. The results obtained from FESEM images indicate that CeO₂-NPs obtained at 600?°C ranges from 18 to 60?nm and have a mean diameter of ~34?nm. The in vitro cytotoxicity study on WEHI 164 cell line has mentioned low toxic and non-toxic CeO₂-NPs in a range of concentrations (0.97–250?μg/ml), thus, we reckon that the greener synthesized CeO₂-NPs will have persistent utilization in various fields of medical applications.     

Morphology-controlled therapeutic activity of cerium oxide nanoparticles for mild traumatic brain injury

The design and optimization of nanostructures with unique morphologies and properties are at the forefront of biomedical nanotechnology. Cerium oxides are widely used to investigate the effect of morphology on performance. However, elucidating the morphology–activity relationship of cerium oxide nanocrystals in biomedical applications remains challenging. Herein, the therapeutic effects of cerium oxide nanoparticles with different morphologies: cerium oxide nanorods with two different aspect ratios (CeO_x NRs_A and CeO_x NRs_B), cerium oxide nanopolyhedra (CeO_x NPs), and cerium oxide nanocubes (CeO_x NCs) are investigated in in vivo and in vitro mild traumatic brain injury (TBI) models. Cerium oxide nanoparticles inhibit oxidative stress and inflammation after mild TBI, alleviating cognitive impairment; furthermore, the therapeutic effect is significantly affected by their morphology. Owing to the higher Ce³⁺/Ce⁴⁺ ratio, exposure of more active crystal surfaces, and greater number of exposed oxygen vacancies, CeO_x NRs show better activity than CeO_x NPs and CeO_x NCs for mild TBI. Among the two investigated types of cerium oxide nanorods, CeO_x NRs_A, with a higher Ce³⁺/Ce⁴⁺ ratio on the surface, appear to spread better than CeO_x NRs_B in the injured lesions. The factors causing morphology-controlled biomedical performance, such as Ce³⁺/Ce⁴⁺ molar ratio, surface area, and aspect ratio, are discussed.     

Polyethylene glycol assisted facile sol-gel synthesis of lanthanum oxide nanoparticles: Structural characterizations and photoluminescence studies

In this study, lanthanum oxide nanoparticles (La₂O₃ NPs) synthesised via the facile sol-gel method, using a solution of micro-sized lanthanum oxide powders containing 20% nitric acid and high molecular weight polyethylene glycol (PEG). The as synthesised La₂O₃ NPs were then characterized using X-ray diffraction (XRD), environmental scanning electron microscopy (ESEM), energy-dispersive X-ray (EDS) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and photoluminescence (PL) spectroscopy. Our findings indicated that the concentration of PEG strongly influences the particle size and the lattice strain of the La₂O₃ NPs. A single phase hexagonal crystal structure was confirmed via XRD studies with lattice constants, a =?b =?0.3973?nm and c =?0.6129?nm. The average crystallite size and lattice strains estimated were in the range of approximately 25–28?nm and 0.0050–0.0055 respectively. The incremental nature of the crystallinity and lattice strains of the NPs was observed with the subsequent enhancement of PEG-contents, while the average particle size was reduced. The average particle size of La₂O₃ NPs estimated from ESEM imaging was consistent with that obtained from the XRD data. The photoluminescence spectra revealed a strong emission band located at a wavelength of 365?nm (typical green band) for all La₂O₃NPsamples. This is ascribed to the recombination of delocalized electrons around the conduction band with a single charged state of a surface oxygen vacancy.     

Enhanced anti-biofilm activity of facile synthesized silver oxide nanoparticles against K. pneumoniae

Journal of Inorganic and Organometallic Polymers and Materials - The silver oxide nanoparticle was successfully synthesized using floral waste by simple one pot, cost effective method. The complete...     

One step green synthesis of hexagonal silver nanoparticles and their biological activity

Hexagonal and spherical silver nanoparticles were prepared by in situ and green synthesis using sun light as reducing agent with assistance newly prepared cationic surfactant which act also as capping agents. The silver nanoparticles formation was investigated using UV–vis spectrophotometer, transmission electron microscope (TEM), dynamic light scattering (DLS), energy dispersive X-ray (EDX) and FTIR. The results showed formation uniform, well arrangement hexagonal and spherical shapes. Increasing hydrophobic chain length increase the stability and amount of AgNPS. Both prepared surfactants and surfactants capping silver nanoparticles showed high antimicrobial activity against Gram-positive and Gram-negative bacteria.     

Production of high porosity nanoparticles of cerium oxide in clay

Cerium oxide nanoparticles modified montmorillonite was obtained by interaction of a clay with (NH₄)₂Ce(NO₃)₆. The mean size of cerium oxide nanoparticles in clay was at 3.5 nm. The product was an amorphous solid and showed high permanent porosity and stability at high temperatures. The amorphous structure of the sample was proven by X-ray diffraction and electronic diffraction. The porous structure was studied by means of chemisorption and it was shown that samples calcined at 550 °C had S_BET = 239 m²/g; micropore volume = 0.1839 cm³/g; average pore diameter = 3.07 nm.     

Electric field-assisted synthesis/sintering cerium oxide: 5 wt.% gadolinium oxide

Gadolinium oxide ceramic powders were mixed to cerium oxide ceramic powders, pressed to pellets, and sintered either at 1450 °C or applying 200 V cm⁻¹ electric field at 800 °C, 900 °C and 1000 °C. The structural phases and the microstructure of the sintered pellets were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The formation of substitutional solid solution was followed by monitoring the increase of the electrical conductivity by impedance spectroscopy and X-ray diffraction. The main results show that Joule heating due to the flow through the pellets of the electric current, which was produced by the application of the electric field, allows for promoting partial solid solution as well as partial sintering the ceria-gadolinia pellets. Moreover, grain growth that occurred in the high temperature sintered pellets was inhibited in the electric field-assisted synthesized/sintered pellets, being an alternative technique for producing cerium oxide-gadolinium oxide solid solutions.     

Microwave assisted hydrothermal synthesis of engineered cerium oxide nanopowders

Cerium oxide nanopowders have been prepared via microwave assisted hydrothermal technique in the presence of different amounts of poly vinyl pyrrolidone (PVP). The prepared nanopowders were characterized using XRD, TEM and SAED. The results showed that the particle size of the ceria nanopowders was decreased with the increase of PVP amount. The prepared ceria has nanocrystalline cubic fluorite structure with high purity. The influence of PVP content on the densification behavior of CeO₂ was investigated by means of dilatometer and scanning electron microscopy (SEM). It was found that the increase of PVP amount reduced sintering temperature. The cold-pressed powders can be sintered to full density at temperatures starting from 1070 °C in just 10 min.     

Vegetable oil aided hydrothermal synthesis of cerium oxide nanocrystals

Hydrothermal synthesis of cerium oxide nanocrystals was performed with in-situ surface modification using soybean oil and palm oil as capping agents. The synthesized nanocrystals were examined by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric analysis (TGA). TEM results showed single crystalline nature with stable dispersion. FT-IR spectra and TGA plots further confirmed the adsorption of fatty acid molecules onto cerium oxide surface. Our findings have the advantages of reduced materials costs compared to using single component surfactants and the production of valuable by-product glycerol.     

A facile synthesis of Te nanoparticles with binary size distribution by green chemistry

Our work reports a facile route to colloidal Te nanocrystals with binary uniform size distributions at room temperature. The binary-sized Te nanocrystals were well separated into two size regimes and assembled into films by electrophoretic deposition. The research provides a new platform for nanomaterials to be efficiently synthesized and manipulated.     

Mechanically reinforced biodegradable nanocomposites. A facile synthesis based on PEGylated silica nanoparticles

Biodegradable nanocomposites consisting of poly(?-caprolactone) (PCL) reinforced by PEGylated silica (polyethylene-glycol/SiO₂) nanoparticles were prepared by a melt-extrusion process. The PEGylated silica nanoparticles were prepared in a facile, one-pot synthesis process. Transmission electron microscopy (TEM) observations of the PEGylated silica nanoparticles inside the PCL matrix indicated that a homogeneous dispersion had been achieved. As a result, the storage modulus (E′) in the rubbery plateau increased significantly with the filler contents at all temperatures studied, at values approximately 45% higher than the neat PCL, at a loading level of only 4 wt.%. In comparison, in the absence of polyethylene-glycol (PEG) the silica nanoparticles formed aggregates inside the PCL matrix, and the reinforcement was negligible. The results from X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (FTIR) analyses identified the location of the PEG at the PCL/silica interface.     

A facile synthesis of ergostanol

Ergosteryl acetate is hydrogenated in one step to ergostanyl acetate over 10% Pd/C in ethyl acetate-acetic acid at 150 C.     

Impact of physicochemical properties of cerium oxide nanoparticles on their toxicity effects

The advancing production and application of cerium oxide nanoparticles (CeO₂-NPs) in recent years have raised scientists concern about their toxicity. Numerous investigations have been performed to study the toxicity of CeO₂-NPs although their results are sometimes contradictory. In this review, we display the most important factors that are effective in CeO₂-NPs toxicity. The studies are classified based on the target that is selected for toxicity assessment (cytotoxicity, respiratory toxicity, hepatotoxicity, neurotoxicity, dermal toxicity, phytotoxicity, and environmental toxicity). Various representative examples are presented in each class. It seems to be difficult to achieve a comprehensive view and a deterministic conclusion since several parameters are involved in interpreting the results. In order to reach repeatable and comparable results, it is necessary to design a standard protocol to study the toxicity of CeO₂-NPs. Physicochemical properties of nanoparticles, experiment set up, and toxicity assessment methods are some parameters that should be considered in this standardization.     

Green facile synthesis of low-toxic superparamagnetic iron oxide nanoparticles (SPIONs) and their cytotoxicity effects toward Neuro2A and HUVEC cell lines

Superparamagnetic iron oxide (Fe₃O₄) nanoparticles (SPIONs) were synthesized by co-precipitation using polyvinyl alcohol (PVA) as a capping agent under alkaline condition. The produced X-ray diffraction (XRD) pattern evidenced the presence of peaks corresponding to the inverse spinel structure of the prepared SPIONs. Debye-Scherrer and field emission scanning microscopy (FESEM) showed the prepared SPIONs to be well-defined with about <?50?nm size. Likewise, the superparamagnetic properties of the SPIONs measured by Vibrating Sample Magnetometer (VSM) showed high saturation magnetization (~ 65.36?emu/g). The in vitro cytotoxicity studies on Neuro2A and HUVEC cells have mentioned low toxic and non-toxic SPIONs, respectively in a range of concentrations (1.17–150?μg/ml), thus, we reckon that the synthesized SPIONs will have persistent utilization in different fields of medical applications.