Characterization of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles synthesized by various methods

Microwave-induced combustion with glycine, CTAB-assisted hydrothermal process with NaOH and NH3, EDTA assisted-hydrothermal methods have been applied to prepare NiFe₂O₄ nanoparticles for the first time. Structural and magnetic properties of the products were investigated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmison electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and electron spin resonance spectrometry (EPR). TEM measurements showed that morphology of the product depends on the synthesis method employed. The average cystallite size of NiFe₂O₄ nanoparticles was in the range of 14–59 nm as measured by XRD. The uncoated sample (Method A) had an EPR linewidth of 1973 Oe, the coated samples reached lower values. The magnetic dipolar interactions existing among the Ni ferrite nanoparticles are reduced by the coatings, which could cause the decrease in the linewidth of the EPR signals. Additionally, the linewidth increases with an increase in the size and the size distribution of nanoparticles.     

Synthesis and characterization of chitosan coating of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles for biomedical applications

Nickel ferrite nanoparticle is a soft magnetic material whose appealing properties as well as various technical applications have rendered it as one of the most attractive class of materials; its technical applications range from its utility as a sensor and catalyst to its utility in biomedical processes. The present paper focuses first on the synthesis of NiFe₂O₄ nanoparticles through co-precipitation method resulting in calcined nanoparticles that were achieved at different times and at a constant temperature (773 k). Afterward, they were dispersed in water that was mixed by chitosan. Chitosan was bonded on the surface of nanoparticles by controlling the pH of media. In order to assess the structural and magnetic properties of nanoparticles, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and vibrating sample magnetometer (VSM) analyses were conducted at room temperature. As per the results of XRD analysis, the pure NiFe₂O₄ was synthesized. Additionally, nanoparticles grew in size by extending the calcination process duration. TEM micrographs were used to determine the size and shape of particle; the obtained results indicate that the particle size was in a range of 17–30 nm and of a circular shape. The proper chitosan covering was also indicated by FTIR results. The VSM analysis also revealed that the saturated magnetization of NiFe₂O₄ nanoparticles stood in a range of 29 emu/g and 45 Q_e. A stable maximum temperature ranging from 30 to 42 was successfully achieved within 10 min. Also, a specific absorption rate of up to 8.4 W/g was achieved. The study results revealed that the SAR parameter of the coated nickel ferrite nanoparticle is more than that of pure nickel ferrite or cobalt ferrite nanoparticles.     

Non-isothermal decomposition kinetics of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles synthesized using egg white solution route

The thermal decomposition kinetics of nickel ferrite (NiFe₂O₄) precursor prepared using egg white solution route in dynamical air atmosphere was studied by means of TG with different heating rates. The activation energy (E _α) values of one reaction process were estimated using the methods of Flynn–Wall–Ozawa (FWO) and Kissinger–Akahira–Sunose (KAS), which were found to be consistent. The dependent activation energies on extent of conversions of the decomposition reaction indicate “multi-step” processes. XRD, SEM and FTIR showed that the synthesized NiFe₂O₄ precursor after calcination at 773 K has a pure spinel phase, having particle sizes of ~54 ± 29 nm.     

Kinetics of microwave-enhanced solid-phase reaction of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> formation

Microwave-enhanced solid-phase reaction between iron(III) oxide and nickel(II) oxide has been studied at 850–900°C. The formal-kinetic approach to data processing showed that microwave treatment considerably increases the rate of the solid-phase reactions and changes its rate-controlling stage.     

Effect of Copper Substitution on Magnetic Properties of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> Ferrite

The many-body Green’s function theory has been used to study the magnetic properties of Cu_xNi_1?xFe₂O₄ spinels. We present a new method to calculate the expectation values in terms of the eigenvalues and eigenvectors of the equations of motion matrix for the set of Green’s functions. Magnetization and magnetic susceptibility are given when external magnetic field is applied in (x–z) plane. The mean field theory has been used to calculate nearest-neighbor exchange and next-nearest-neighbor superexchange interactions. The intraplanar and the interplanar interactions are deduced. The magnetic phase diagram is deduced using high-temperature series expansions. The ferrimagnetic and paramagnetic phases are determined. The critical exponents associated with the magnetic susceptibility \(\left( \gamma \right)\) and the correlation lengths \(\left( \nu \right)\) have been deduced. These results are comparable with those obtained by magnetic measurements and are comparable with those of 3D Heisenberg model.     

Physical and electrochemical properties of LiFe<Subscript>0.5</Subscript>Mn<Subscript>1.5</Subscript>O<Subscript>4</Subscript> spinel synthesized by different methods

The study deals with the synthesis and comparison of physicochemical properties of LiFe_0.5Mn_1.5O₄ based cathode materials synthesized by the standard ceramic and the auto-ignition method.     

Coordination mechanism,characterization, and photoluminescence properties of spinel ZnAl<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles prepared by a modified polyacrylamide gel route

Single-phase ZnAl₂O₄ nanoparticles with the spinel structure were successfully synthesized using a modified polyacrylamide gel method according to the atomic ratio of Zn to Al = 1: 1.8. The as-prepared samples were characterized by means of X-ray powder diffraction (XRD), thermogravimetric analysis (TG), differential scanning calorimetry analysis (DSC), field-emission scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and photoluminescence (PL) spectra. XRD patterns show that the pure phase of ZnAl₂O₄ is obtained after heating the xerogel at 900°C for 5 h in air. The SEM images reveal that the ZnAl₂O₄ nanoparticles have a narrow particle size distribution and the average particle size is around 45 nm. Photoluminescence (PL) spectra demonstrate the single phase ZnAl₂O₄ nanoparticles have an emission peak located at 469 nm when excited by 350 nm light. The phase structure, coordination mechanism, and luminescence properties have been discussed on the basis of the experimental results.     

Electrochemical properties of spinel Li<Subscript>4</Subscript>Ti<Subscript>5</Subscript>O<Subscript>12</Subscript> nanoparticles prepared via a low-temperature solid route

Spinel phase Li₄Ti₅O₁₂ (s-LTO) with an average primary particle size of 150 nm was synthesised via a solid state route by calcining a precursor mixture at 600 °C. The precursor was prepared from a stoichiometric mixture of TiO₂ nanoparticles and an ethanolic solution of Li acetate and activated by ball-milling. Effects of the calcination temperature and atmosphere are examined in relation to the coexistence of impurity phases by X-ray diffraction and ⁶Li MAS NMR. The charge capacity of s-LTO, determined from cyclic voltammogram at a scan rate of 0.1 mV/s, was 142 mAh/g. The capacity of our optimised material is superior to that of commercially available spinel (a-LTO), despite the considerably smaller BET-specific surface area of the former. The superior properties of our material were also demonstrated by galvanostatic charging/discharging. From these observations, we conclude that the presented low-temperature solid state synthesis route provides LTO with improved electrochemical performance.     

Nano-Architecture of Facetted NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/(Ni,Fe)O Particles Produced by Induction Plasma

Facetted nickel ferrite (NiFe₂O₄) and bunsenite [(Ni,Fe)O] nanocrystals were grown from the decomposition of iron and nickel nitrate precursors using an inductively coupled plasma reactor. The full range of the two-phase region of the Fe₂O₃–NiO pseudo-equilibrium phase diagram was investigated by producing nanopowders with bulk Ni/(Ni + Fe) ratios of 0.33, 0.4, 0.5, 0.75 and 1.0. A Ni-poor [Ni/(Ni + Fe) ≤ 0.5] precursor solution produced truncated octahedron nanocrystals, whereas nanocubes were obtained at higher ratios [Ni/(Ni + Fe) ≈ 1]. In both cases, it is shown that the nanocrystals adopt a morphology close to the Wulff shape of the crystalline system (spinel and NaCl, respectively). As the bulk Ni/(Ni + Fe) ratio increases from 0.33 (the stoechiometric composition of nickel ferrite), bunsenite is epitaxially segregated on the {110} and {111} facets of nickel ferrite, while leaving the NiFe₂O₄ {100} facets exposed. A precursor solution at a Ni/(Ni + Fe) ratio of 0.75 gave an (Ni,Fe)O-rich nanopowder with a random and irregular interconnected morphology. The structure of these nanocrystals can be understood in terms of their thermal history in the plasma reactor. These results highlights the possibility of producing organized multi-phased nanomaterials of binary systems having two phases stable at high temperatures, using a method known to be easily scalable.     

Preparation of MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles by microemulsion method and their characterization

This work presents the preparation and characterization of magnesium ferrite which is one of the important magnetic oxides with spinel structure. Magnesium ferrite was prepared via microemulsion method mediated hydrolytic decomposition of mixed alkoxide solutions. This microemulsion was using for preparation magnesium ferrit for the first time. The starting solution, composed from magnesium methoxide and iron ethoxide in dry ethanol, was introduced in to the prepared microemulsion and sequentially hydrolyzed by distilled water addition (Pithan et al. in J Cryst Growth 280:191–200, 2005; Shiratori et al. in J Eur Ceram Soc 25:2075–2079, 2005; Herrig and Hempelmann in Mater Lett 27:287–292, 1996). After raw powder precipitation, the samples were decantanted by ethanol and then calcined at temperatures 800, 900, 1,000 or 1,100 °C for 1 h. The resulting samples were characterized using powder X-ray diffraction, high resolution transmission electron microscopy, Mössbauer spectroscopy and magnetic measurements. X-ray diffraction and Mössbauer spectroscopy confirmed the presence of the spinel phase. The particles size was calculated from the XRD line broadening using Scherrer equation and their size was found about 31–38 nm, with only slight dependence on the heat treatment temperature. TEM revealed the particles size of about 39 nm. Magnetic measurements showed a ferrimagnetic behavior for all samples.     

Comparative study of the synthesis of CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> and NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> in silica through the polymerized complex route of the sol–gel method

In this work the synthesis of CoFe₂O₄-SiO₂ and NiFe₂O₄-SiO₂ nanocomposites was studied via the sol–gel method, using the polymerized complex route. The polymerized precursors obtained by the reaction of citric acid, ethylene glycol, tetraethylorthosilicate, ferric nitrate, and cobalt nitrate or nickel chloride were characterized by nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy. NMR and IR spectra of the precursors, without and with metallic ions, show the formation of polymeric chains with ester and ether groups and complexes of metal-polymeric precursor. The nanocomposites were obtained by the thermal decomposition of the organic fraction and characterized by X-ray diffraction (XRD) and vibrating sample magnetometry (VSM). XRD patterns show the formation of CoFe₂O₄ and NiFe₂O₄ in an amorphous silica matrix above 400 °C in both cases. When the calcination temperature was 800 °C the particle size of the crystalline phases, calculated using the Scherrer equation, reached ∼35 nm for the two oxides. VSM plots show the ferrimagnetic behavior that is expected for this type of magnetic material; the magnetization at 12.5 KOe of the CoFe₂O₄-SiO₂ and NiFe₂O₄-SiO₂ compounds was 29.5 and 17.4 emu/g, respectively, for samples treated at 800 °C.     

Effect of the modifier ion on the properties of MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript> and ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> pigments

Magnesium and zinc ferrites have been prepared by the polymeric precursor method. The organic material decomposition was studied by thermogravimetry (TG) and differential thermal analysis (DTA). The variation of crystalline phases and particle morphology with calcination temperature were investigated using X-ray diffraction (XRD) and scanning electronic microscopy (SEM), respectively. The colors of the ferrites were evaluated using colorimetry. Magnesium ferrite crystallizes above 800°C, presenting a yellow- orange color with a reflectance peak at the 600–650 nm range, while zinc ferrite crystallizes at 600°C, with a reflectance peak between 650–700 nm, corresponding to the red-brick color.     

The microstructure and magnetic properties of Ni<Subscript>0.4</Subscript>Zn<Subscript>0.6</Subscript>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript> films prepared by spin-coating method

Nickel zinc ferrite (Ni_0.4Zn_0.6Fe₂O₄) films on Si (100) substrate were synthesized using a spin-coating method. The crystallinity of the Ni_0.4Zn_0.6Fe₂O₄ films with the thickness of about 386 nm became better as the annealing temperature increased. The films have smooth surface, relatively good packing density and uniform thickness. The volatilization of Zn is serious at 900 °C. With the increase of annealing temperature, the saturation magnetization M _s increases in the temperature ranging from 400 to 700 °C, however, decreases above 700 °C, and the coercivity H _c increases in the temperature range 400–800 °C, decreases above 800 °C. After annealed at 700 °C for 2 h in air with the heating rate 2 °C/min, the film shows a maximum saturation magnetization M _s of 349 emu/cc and low coercivity H _c of 66 Oe. The M _s is higher than others which prepared by this method, however, the H _c is lower. The M _s of Ni_0.4Zn_0.6Fe₂O₄ films annealed at 700 °C increases with increasing annealing time and the H _c changes slightly.     

Ferroelectric properties of La and V co-substituted SrBi<Subscript>4</Subscript>Ti<Subscript>4</Subscript>O<Subscript>15</Subscript> films prepared by sol-gel method

SrBi₄Ti₄O₁₅ (SBTi), SrBi_3.89La_0.1Ti_3.97V_0.03O₁₅ (SBLTV) thin films have been fabricated on Pt/Ti/SiO₂/Si by the sol–gel method. Well-saturated hysteresis loops with remnant polarization around 46.7 μC/cm² are obtained on Pt/SBLTV/Pt capacitors. The capacitor shows excellent fatigue resistance with no polarization reduction up to 10⁹ switching cycles even at low test frequency of 50 kHz. The improvement of ferroelectric and fatigue-endurance properties are attributed to the La³⁺ and V⁵⁺ co-substitution, which brings about the concentration decrease and the mobility weakening of the defects.     

Effect of Cr doping on the ac electrical properties of MgAl<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles

Magnesium aluminate nanoparticles with different chromium concentration (0–12%) have been synthesized by a citrate–nitrate sol–gel route. X-ray diffraction studies confirmed the formation of single-phase cubic spinel structure excluding the presence of any secondary phase. Crystallite size of the synthesized nanoparticles was found to increase from 8.5 to 19.8 nm with the increase in Cr concentration. Fourier transformed infrared spectroscopic studies confirmed the presence of AlO₆ group which led to the formation of MgAl₂O₄ spinel structure. Surface morphology of the sintered pellets was investigated with the help of a field emission scanning electron microscope which revealed the existence of both grain and grain boundary along with their aggregates. The dielectric constant, dielectric loss and ac conductivity were studied as a function of frequency of the applied electric field for different composition and their nature of variation with frequency has been elucidated on the basis of Maxwell–Wagner interfacial model. Impedance spectroscopy technique has been used to study the effect of grain and grain boundary on the electrical properties of this spinel oxide. All the electrical parameters showed strong dependence on the nanostructural properties and were found to vary consistently with the increase of doping concentration.     

Preconcentration of Pb(II) by using Mg(II)-doped NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles as a magnetic solid phase extraction agent

Magnesium(II)-doped nickel ferrite (Mg–NiFe₂O₄) nanoparticles are introduced as a new adsorbent for magnetic solid phase extraction of lead(II) ions from aqueous solutions. The structure and morphology of the adsorbent was characterized by FTIR, X-ray diffraction and scanning electron microscopy. The effects of pH value, amount of adsorbent, type, concentration and volume of the eluent and adsorption/desorption time on the extraction efficiency were studied. Following elution with hydrochloric acid, Pb(II) ions were quantified by flame atomic absorption spectrometry. Under optimized conditions, the calibration graph is linear in the 0.5–125 ng mL^?1 Pb(II) ion concentration range. Other figures of merit include (a) a 0.2 ng mL^?1 limit of detection, (b) an enrichment factor of 200, (c) an intra-day relative standard deviation (for n =?6 at 50 ng mL^?1) of 1.6%, and (d) an inter-day precision of 3.8%. The method was validated by the analysis of the certified reference material, NIST SRM 1566b. It was successfully applied to the determination of Pb(II) ion in spiked water samples, industrial wastewater and acidic lead battery waters.

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Graphical abstract Schematic of the synthesis of Mg(II)-doped NiFeO₄ nanoparticles and their application as a magnetic sorbent for solid-phase extraction of a Pb(II) ions prior to determination by flame atomic absorption spectrometry (FAAS).

     

Investigation of catalytic activity of ZnAl<Subscript>2</Subscript>O<Subscript>4</Subscript> and ZnMn<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles in the thermal decomposition of ammonium perchlorate

A new powder metallurgy technique was developed in order to increase the reinforcement proportion of aluminum with two different fractions of Al₂O₃. Aluminum powders were mixed with 20 % vol of alumina particles as primarily reinforcement, and additional alumina was produced in situ as a result of reaction between Al and additional 7.5 % vol of Fe₂O₃ powder. The three grades of powders were milled and hot-pressed into small preforms, and differential scanning analysis (DSC) was performed to determine the kinetics of microstructural transformations produced on heating. DSC curves were mathematically processed to separate the superposing effects of thermal reactions. Transformation points on resulting theoretical curves evidenced two distinct exothermal reaction peaks close to the melting point of aluminum that were correlated with formation of Fe–Al compounds and oxidation of aluminum. Microstructural investigations by means of SEM-EDX and XRD suggested that these exothermal reactions produced complete decomposition of iron (III) oxide and formation of Fe–Al compounds during sintering at 700 °C, and therefore, heating at higher temperatures would not be necessary. These results, along with calculation of activation energies, based on Kissinger’s method, could be used to optimize the fabrication of Al-Al₂O₃ composites by means of reactive sintering at moderate temperatures.     

Effect of heat treatment on magnetic MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles

MgFe₂O₄ (Mg-ferrite) nanoparticles encapsulated in amorphous SiO₂ were prepared by the wet chemical method. The particle sizes were estimated, based on the X-ray diffraction peaks, to be between 3 and 8 nm, depending on the annealing temperature. The particle size increased as the annealing temperature increased. From the magnetization measurements, the blocking temperature, T _b, was found to be between 30 and 60 K. The magnetization values varied with the annealing or quenching conditions. To clarify the process of crystal growth, thermogravimetric and differential thermal analysis (TG-DTA) measurements were performed and the results were compared with the X-ray diffraction patterns.     

Amperometric CO<Subscript>2</Subscript> gas sensor based on interconnected web-like nanoparticles of La<Subscript>2</Subscript>O<Subscript>3</Subscript> synthesized by ultrasonic spray pyrolysis

Thin films of La₂O₃ were deposited onto glass substrates by ultrasonic spray pyrolysis. Their structural and morphological properties were characterized by X-ray diffraction, Fourier transform Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray photo-electron spectroscopy, Brunauer-Emmett-Teller and optical absorption techniques. The sensor displays superior CO₂ gas sensing performance at a low operating temperature of 498 K. The signal change on exposure to 300 ppm of CO₂ is about 75%, and the signal only drops to 91% after 30 days of operation.

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Graphical abstract Schematic diagram of the CO₂ gas sensing mechanism of an interconnected web-like La₂O₃ nanostructure in presence of 300 ppm of CO₂ gas and at an operating temperature of 498 K.

     

Colloidal properties of aqueous dispersions of ultradispersed Al<Subscript>2</Subscript>O<Subscript>3</Subscript> prepared by explosion synthesis

The electrosurface properties of aluminum oxide particles prepared by shock—wave loading of aluminum powder in an oxygen-containing atmosphere and the aggregation stability of its aqueous dispersions are studied by the macroelectrophoresis method, potentiometric titration, and photometry. The enhanced stability of the dispersions in acid media and in the vicinity of the isoelectric point compared to that in alkaline media is explained by the effect of the structural component of the disjoining pressure, which appears due to the predominant hydration of the cationic forms of aluminum that are present on the surface of dispersed phase particles.Translated from Kolloidnyi Zhurnal, Vol. 67, No. 1, 2005, pp. 128–131. Original Russian Text Copyright © 2005 by Chiganova, Nafikova.