Effect of fuel type on the microstructure and magnetic properties of solution combusted Fe3O4 powders

Porous magnetite (Fe₃O₄) powders were synthesized by solution combustion method using the glycine and urea at different fuel to oxidant ratios (ϕ). The combustion behavior depended on the fuel type as characterized by thermal analysis. The structure and phase evolution investigated by X-ray diffraction method showed nearly single phase Fe₃O₄ powders which were achieved only by using the glycine fuel at ϕ=1. The specific surface area and porous structures of the as-combusted Fe₃O₄ powders were characterized by N₂ adsorption-desorption isotherms and scanning electron microscopy, respectively. The surface area using the glycine fuel (62.6 m²/g) was higher than that of urea fuel (42.5 m²/g), due to different combustion reactions. Magnetic properties of the as-combusted powders were studied by vibration sample magnetometry which exhibited the highest saturation magnetization of 74 emu/g using the glycine fuel at ϕ=1 on account of its high purity and large crystallite size.     

Synthesis of CoFe2O4 powders with high surface area by solution combustion method: Effect of fuel content and cobalt precursor

High surface area cobalt ferrite (CoFe₂O₄) powders were synthesized by solution combustion method. The dependence of the adiabatic temperature and the released gases during combustion reaction on the fuel content and cobalt precursor type, cobalt nitrate and cobalt acetate, was thermodynamically calculated. Thermal analysis, infrared spectroscopy, X-ray diffractometry, nitrogen adsorption–desorption, electron microscopy and vibrating sample magnetometer were used for investigation of the phase evolution, surface areas, morphology and magnetic properties of the synthesized CoFe₂O₄ powders. The specific surface area decreased from 285.4 to 35.7 m²/g with increasing of fuel to oxidant molar ratio, ϕ, from 0.5 to 1.25 for the cobalt nitrate precursor, while the maximum surface area of 182.1 m²/g was attained at ϕ=1 for the cobalt acetate precursor. The synthesized CoFe₂O₄ powders from the cobalt nitrate precursor exhibited the higher saturation magnetization and coercivity on account of the higher purity and crystallinity.     

Microwave-assisted solution combustion synthesis of Fe3O4 powders

Magnetite (Fe₃O₄) powders were synthesized by solution combustion method at different fuel to oxidant ratios (ϕ = 0.5, 0.75, 1 and 1.5) using conventional and microwave ignition. The ignition method and fuel content affected the phase evolution, microstructure and magnetic properties of Fe₃O₄ powders as characterized by X-ray diffractometry, infrared spectroscopy, N₂ adsorption–desorption, electron microscopy and vibrating sample magnetometry techniques. Single phase Fe₃O₄ powders were only obtained using conventional ignition at ϕ value of 1, while the impurity phases such as α-Fe₂O₃ and FeO together with Fe₃O₄ phase were formed by microwave ignition. The bulky microstructure of conventionally combusted powders with specific surface area of 71.5 m²/g was transformed to disintegrated structure (76.5 m²/g) by microwave heating. The microwave combusted powders showed the highest saturation magnetization of 86.5 emu/g at ϕ value of 0.5 and the lower coercivity than that of conventionally combusted powders at all ϕ values, due to their larger particles.     

Nanocrystalline Cr2O3 and amorphous CrO3 produced by solution combustion synthesis

The synthesis of chromium oxides by solution combustion synthesis was investigated. Ammonium dichromate, glycine, urea and ammonium nitrate dissolved in aqueous solution were used as the precursors of the oxides. The effect of different reaction parameters, such as fuel richness, stoichiometry and fuel leanness was evaluated; such parameters were modified by changing the reagents and the fuel/oxidant ratio. Amorphous CrO₃ and crystalline Cr₂O₃ were synthesized. The results suggest that glycine is a better complexing/combustible agent for ammonium dichromate than urea. Addition of extra ammonium nitrate to stoichiometric compositions improved the specific surface area and reduced the crystallite size. The smallest crystallite size (≈20 nm) of Cr₂O₃ was obtained with glycine as fuel/complexant agent in fuel-lean mixtures. The highest specific surface area (63 m²/g) was observed with urea in fuel-rich mixtures, forming amorphous CrO₃.     

Soft chemistry routes for the preparation of Ag-CoFe2O4 nanocomposites

Silver-cobalt ferrite nanocomposites (Ag-CoFe₂O₄) were synthesized through wet ferritization process and self-propagating combustion method. The structure, morphology, surface chemistry and magnetic properties of the nanocomposites were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer (VSM). X-ray diffraction patterns confirmed the formation of CoFe₂O₄ and Ag nanoparticles with cubic symmetry. The average crystallite size of CoFe₂O₄ by wet ferritization ranged between 60 Å and 87 Å; for those obtained by self-propagating combustion was in the range 232–290 Å. SEM micrographs revealed different morphological features of nanocomposites. Ag-CoFe₂O₄ obtained by wet ferritization exhibited typical superparamagnetic behaviour. The antimicrobial and anti-biofilm properties of all silver-cobalt ferrites were evaluated. The results revealed that the Ag-CoFe₂O₄ nanocomposites exhibited good microbicidal and anti-biofilm features.     

Sonochemical synthesis of CoFe2O4 nanoparticles and their application in magnetic polystyrene nanocomposites

CoFe₂O₄ (CoFe) nanoparticles were synthesized via a facile surfactant-free sonochemical reaction. For preparation of magnetic polymeric films, CoFe₂O₄ nanoparticles were added to polystyrene (PS). Nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Magnetic properties of the samples were investigated using an alternating gradient force magnetometer (AGFM). CoFe₂O₄ nanoparticles exhibit a ferromagnetic behaviour with a saturation magnetization of 62 emu/g and a coercivity of 640 Oe at room temperature. By preparing magnetic films the coercivity is increased. The coercivity of PS/CoFe₂O₄ (10%) nanocomposites is higher than that obtained for PS/CoFe₂O₄ (30%).     

Enhancement of the interfacial polarization resistance of La0.6Sr0.4Co0.2Fe0.8O3-δ cathode by microwave-assisted combustion method

Thermogravimetry, phase formation, microstructural evolution, specific surface area, and electrical properties of La_0.6Sr_0.4Co_0.2Fe_0.8O_3−δ (LSCF) cathode were studied as functions of its preparation technique. The pure perovskite LSCF cathode powder was synthesized through glycine–nitrate process (GNP) using microwave heating technique. Compared with conventional heating technique, microwave heating allows the rapid combustion to occur simultaneously between the nitrates and glycine in a controllable manner. The resulting powder is a single-phase nanocrystallite with a mean particle size of 113 nm and a high specific surface area of 12.2 m²/g, after calcination at 800 °C. Impedance analysis indicates that microwave heating has significantly reduced the polarization resistance of LSCF cathode. The area specific resistance (ASR) value of 0.059 and 0.097 Ω cm² at 800 °C and 750 °C, respectively, were observed. These values were twofold lower than the corresponding ASR of the cathode (0.133 and 0.259 Ω cm² at 800 °C and 750 °C, respectively) prepared through conventional heating. Results suggest that the microwave heating GNP strongly contributes to the enhancement of the LSCF cathode performance for intermediate temperature solid oxide fuel cells.     

Coupling CoFe2O4 and SnS2 nanoparticles with reduced graphene oxide as a high-performance electromagnetic wave absorber

The reduced graphene oxide (RGO)/CoFe₂O₄/SnS₂ composites have been successfully synthesized by two-step hydrothermal processes. TEM results show that CoFe₂O₄ and SnS₂ nanoparticles with both diameters about 5–10 nm are well dispersed on the surface of graphene. Compared with RGO/CoFe₂O₄ composites, the as-prepared RGO/CoFe₂O₄/SnS₂ composites exhibit excellent electromagnetic (EM) wave absorption properties in terms of both the maximum reflection loss and the absorption bandwidth. The maximum reflection loss of RGO/CoFe₂O₄/SnS₂ composites is −54.4 dB at 16.5 GHz with thickness of only 1.6 mm and the absorption bandwidth with the reflection loss below −10 dB is up to 12.0 GHz (from 6.0 to 18.0 GHz) with a thickness in the range of 1.5–4.0 mm. And especially, they cover the whole X band (8.0–12.0 GHz), which could be used for military radar and direct broadcast satellite (DBS).     

Structure and magnetic properties of CoFe2O4/SiO2 nanocomposites obtained by sol-gel and post annealing pathways

The influence of the CoFe₂O₄ nanoparticles concentration in silica matrix on the structural and magnetic properties of xCoFe₂O₄/(100−x)SiO₂ nanocomposites with x=10, 30, 50, 70 and 90 was studied. Magnetic CoFe₂O₄ nanoparticles dispersed in silica matrix was obtained by sol-gel method, followed by annealing at 1100 °C. The X-ray diffraction pattern and FT-IR spectra revealed the single spinel ferrite structure for all samples. The FT-IR spectra also suggested the formation of the amorphous silica matrix. The results showed that the increase of cobalt ferrite concentration (x) in the silica matrix leads to high crystallinity, specific surface area and particle size. The magnetic CoFe₂O₄ nanoparticles have spherical shapes and size in the 6–35 nm range. The Mössbauer measurements were fitted with two Zeeman sextets, indicating that all the samples were completely magnetically ordered. The vibrating sample magnetometer studies showed that the saturation magnetization (Ms) and coercivity (Hc) of the CoFe₂O₄ nanocrystals embedded in silica matrix possessed a linear relationship with the mean crystallite size. Also, the saturation magnetization of the studied nanocomposites increases with the increase of cobalt ferrite concentration (x) in the silica matrix.     

Solution combustion synthesis of nanostructured iron oxides with controllable morphology,composition and electrochemical performance

Nanostructured iron oxides have emerged as promising materials for electrochemical energy storage and conversion devices due to their high theoretical capacity, eco-friendliness and earth abundance. Particularly, the morphology- and composition-controllable synthesis of nanostructured iron oxides is extremely important to optimize their electrochemical performance. However, the development of facile and effective synthetic method is still a great challenge. In this paper, we demonstrated a one-pot solution combustion synthesis (SCS) approach for the time- and energy-effective preparation of nanostructured iron oxides with controllable morphology and composition just by tuning the molar ratio (φ) of fuel (glycine) to oxidizer (ferric nitrate). Innovatively, the effects of φ value on the control of combustion reaction mechanism, morphology and composition of SCS products, and the electrochemical properties in relation to the morphology and composition have been systematically investigated. The results revealed that with the increase of φ value, the reaction mechanism varied from pyrolysis to combustion and the combustion phenomenon changed from volumetric mode to self-propagating mode. Correspondingly, the morphology of products evolved from uniform nanoneedles to porous nanosheets, and finally into aggregated nanoparticles. Meanwhile, the phase composition of these products changed from amorphous α-Fe₂O₃ to crystalline α-Fe₂O₃, and eventually into α-Fe₂O₃/Fe₃O₄ composites. When evaluated as lithium ion battery anode, the as-prepared α-Fe₂O₃/Fe₃O₄ porous nanosheets (φ = 1.0 product) exhibited the best electrochemical properties (a high reversible capacity of ~ 1200 mA h g^?1 and an excellent rate capability) among all the SCS products, which may be attributed to its mesoporous structure (supply favorable accessibility for electrons), nanosheet morphology (shorten the transport length of Li⁺) and appropriate proportion of Fe₃O₄ phase (enhance the electronic conductivity). Consequently, the facile SCS method demonstrated here might provide a new methodology for the morphology and composition-controllable synthesis of nanomaterials, for which a number of prospective applications in electrochemical fields can be envisioned.     

Oxidative desulfurization of dibenzothiophene over Fe promoted Co–Mo/Al_2O_3 and Ni–Mo/Al_2O_3 catalysts using hydrogen peroxide and formic acid as oxidants

This work reports the enhancing effect of a highly cost effective and efficient metal, Fe, incorporation to Co or Ni based Mo/Al_2O_3 catalysts in the oxidative desulfurization(ODS) of dibenzothiophene(DBT) using H_2O_2 and formic acid as oxidants. The influence of operating parameters i.e. reaction time, catalyst dose, reaction temperature and oxidant amount on oxidation process was investigated. Results revealed that 99% DBT conversion was achieved at 60 °C and 150 min reaction time over Fe–Ni–Mo/Al_2O_3. Fe tremendously enhanced the ODS activity of Co or Ni based Mo/Al_2O_3 catalysts following the activity order: Fe–Ni–Mo/Al_2O_3 NFe–Co–Mo/Al_2O_3 NNi–Mo/Al_2O_3 NCo–Mo/Al_2O_3, while H_2O_2 exhibited higher oxidation activity than formic acid over all catalyst systems. Insight about the surface morphology and textural properties of fresh and spent catalysts were achieved using scanning electron microscopy(SEM), X-ray diffraction(XRD), energy dispersive X-ray(EDX)analysis, Atomic Absorption Spectroscopy(AAS) and BET surface area analysis, which helped in the interpretation of experimental data. The present study can be deemed as an effective approach on industrial level for ODS of fuel oils crediting to its high efficiency, low process/catalyst cost, safety and mild operating condition.     

Fabrication of microwave absorbing CoFe2O4 coatings with robust superhydrophobicity on natural wood surfaces

A superhydrophobic wood surface with microwave absorption property was prepared based on the formation of CoFe₂O₄ nanoparticles and subsequent hydrophobization using fluorinated alkylsilane (FAS). Meanwhile, sticky epoxy resin was worked as a caking agent by adhering abundant of CoFe₂O₄ nanoparticles to wood surface. The as-prepared superhydrophobic coatings on wood maintain stable superhydrophobicity after suffering a significant abrasion. Moreover, the complex permeability and permittivity of the coated wood composites were measured in the frequency range of 2–18 GHz by vector network analysis. The microwave absorption properties were elucidated by the traditional coaxial line method. The results show that the as-prepared wood composites have excellent microwave absorption properties at the frequency of 16 GHz, and the minimum reflection loss can reach −12.3 dB. The approach presented may provide further routes for designing outdoor wood wave absorbers with a specified absorption frequency.     

Solid-state combustion synthesis of spinel LiMn2O4 using glucose as a fuel

Spinel LiMn₂O₄ cathode material was rapidly synthesized in 1 h by solid-state combustion synthesis using metal carbonates as metal ion sources and glucose as a fuel. The effect of different amounts of glucose on the structure and electrochemical performance of as-prepared LiMn₂O₄ was investigated by X-ray diffraction (XRD), scanning electron micrographs (SEM), galvanostatic charge–discharge test, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). LiMn₂O₄ spinel was identified as the main crystalline phase with the presence of minor Mn₃O₄. The amount of glucose greatly affected the formation of Mn₃O₄. The optimal content of glucose was found to be 10 wt%. Under this condition, the Mn₃O₄ peaks almost disappeared, and high-purity spinel LiMn₂O₄ was obtained. Its initial discharge specific capacity of was 125.9 mAh/g, and discharge specific capacity retained at 105.2 mAh/g after 40 cycles. The detail influence of glucose on the electrochemical activity, reversibility and cycling performance of LiMn₂O₄ was discussed.     

Stability and thermal conductivity of nanofluids of tin dioxide synthesized via microwave-induced combustion route

SnO₂ nanofluids were prepared by dispersing tin dioxide nanoparticles in deionized (DI) water as a base fluid. 4–5 nm tin dioxide crystals were synthesized via chloride solution combustion synthesis (CSCS) using SnCl₄ and sorbitol as a novel precursor and the fuel, respectively. Ammonium nitrate was also used as the combustion aid. The molar ratio of sorbitol plus ammonium nitrate to SnCl₄ was set at unity; whereas, the molar ratio of sorbitol-to-ammonium nitrate divided by that of stoichiometric value (Φ) was varied in the range of 0.5–1.4 in order to find the optimum values of specific surface area for the CSCS technique. Transition electron microscopy (TEM), scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and Brunauer–Emmet–Teller (BET) techniques were employed for the characterization of the nanoparticles. Since SnO₂ nanoparticles form clusters within fluids, the fluids were ultrasonicated to improve the dispersion and stability of the nanoparticles. The colloidal stability of the SnO₂ nanofluids was quantitatively characterized by UV–vis spectrophotometric measurements. The results of the UV–vis experiments indicate higher dispersion together with enhanced stability for the nanofluid prepared by SnO₂ nanoparticles synthesized at Φ = 1.0. After 500 h sedimentation time, the relative concentration of the nanofluid with the highest stability is remained at around 77% of the initial concentration of the fluid.A transient hot-wire apparatus was used to measure the thermal conductivities of the nanofluids. In addition, the effects of pH and temperature on the thermal conductivity were also investigated. At 353 K, for the nanofluid prepared by SnO₂ nanoparticles synthesized at Φ = 1.0 at a weight fraction of 0.024%, thermal conductivity is enhanced up to about 8.7%, with an optimal pH = 8.     

Anode-supported SOFCs based on Sm0.2Ce0.8O2−δ electrolyte thin-films fabricated by co-pressing using microwave combustion synthesized powders

Decreasing the electrolyte thickness is an effective approach to improve solid oxide fuel cells (SOFCs) performance for intermediate-temperature applications. Sm_0.2Ce_0.8O_2−δ (SDC) powders with low apparent density of 32±0.3 mg cm⁻³ are synthesized by microwave combustion method, and SDC electrolyte films as thin as ~10 μm are fabricated by co-pressing the powders onto a porous NiO–SDC anode substrate. Dense SDC electrolyte thin films with grain size of 300–800 nm are achieved at a low co-firing temperature of 1200 °C. Single cells based on SDC thin films show peak power densities of 0.86 W cm⁻² at 650 °C using 3 vol% humidified H₂ as fuel and ambient air as oxidant. Both the thin thickness of electrolyte films and ultra-fine grained anode structure make contributions to the improved cell performance.     

Synthesis of the metastable α-Al1.8Fe0.2O3 solid solution from precursors prepared by combustion

The aim of the paper is to synthesise α-Al_1.8Fe_0.2O₃ solid solutions from precursors prepared by the nitrate/fuel combustion synthesis route, using either citric acid or urea, or a mixture of both as the fuel, and different fuel/nitrates ratios. In a first part, global reactions are proposed for each synthesis, which are useful to explain the differences in powder volume, morphology, crystallisation state and specific surface area reported in the second part of the study. In a third part, the powders were further calcined at 1100 °C in order to obtain the corundum form. A combination of Mössbauer spectroscopy, XRD and specific surface area measurements revealed that only the powders prepared with Φ_e = 2 are the desired monophased α-Al_1.8Fe_0.2O₃ solid solutions.     

A novel CoFe2O4/polyacrylate nanocomposite prepared via an in situ polymerization in emulsion system

A CoFe₂O₄/polyacrylate nanocomposite was synthesized by in situ emulsion polymerization of an acrylic acid monomer in the presence of CoFe₂O₄ magnetic fluid. X-ray diffraction and FT-IR spectra confirmed the formation of the CoFe₂O₄/polyacrylate nanocomposite. Transmission electron microscopy images showed that CoFe₂O₄ nanoparticles with the particle sizes of about 12 nm were well dispersed in the polymer matrix. The nanocomposite exhibited superparamagnetic behavior at room temperature under an applied magnetic field. The formation mechanism of the nanocomposite was investigated as well.     

The use of petroleum coke as fuel in chemical-looping combustion

Chemical-looping combustion is a novel technique used for CO₂ separation that previously has been demonstrated for gaseous fuel. This work demonstrates the feasibility of using solid fuel (petroleum coke) in chemical-looping combustion (CLC). Here, the reaction between the oxygen carrier and solid fuel occurs via the gasification intermediates, primarily CO and H₂. A laboratory fluidized-bed reactor system for solid fuel, simulating a CLC-system by exposing oxygen-carrying particles to alternating reducing and oxidizing conditions, has been developed. In each reducing period, 0.2 g of petroleum coke was added to 20 g of oxygen carrier composed of 60% active material of Fe₂O₃ and 40% inert MgAl₂O₄. The effect of steam and SO₂ concentration in the fluidizing gas was investigated as well as effect of temperature. The rate of reaction was found to be highly dependent on the steam and SO₂ concentration as well as the temperature. Also shown was that the presence of a metal oxide enhances the gasification of petroleum coke. A preliminary estimation of the oxygen carrier inventory needed in a real CLC system showed that it would be below 2000 kg/MW_th.     

Properties of NiFe2O4 ceramics from powders obtained by auto-combustion synthesis with different fuels

Nickel ferrite (NiFe₂O₄) powders derived by auto-combustion synthesis using three different fuels (citric acid, glycine and dl-alanine) have been characterized. The sintering behavior of ceramics using these powders has been compared. Oxygen balance (OB) setting for the chemical reaction is found to regulate the combustion reaction rate. A rapid reaction rate and a high flame temperature are achieved with dl alanine fuel yielding single phase NiFe₂O₄ powder in the as-burnt stage, whereas powders derived with citric acid and glycine fuels show poor crystallinity and necessitate post-annealing. The powder particles are largely agglomerated with a non-uniform distribution in shape and size, and the average particle size is estimated in the range ~ 54–71 nm. Powders derived from dl-alanine fuel show better phase purity, smaller crystallite size, larger surface area and superior sintering behavior. Additional Raman modes discerned for dl-alanine derived powder support a 1:1 ordering of Ni²⁺ and Fe³⁺ at the octahedral sites relating to microscopic tetragonal P4₁22 symmetry expected theoretically for the formation of NiFe₂O₄ with inverse spinel structure. Microstructure of sintered ceramics depends on the precursor powders that are used and sintering at 1200 °C is found to be optimum. Citric acid and glycine derived powders yield high saturation magnetization (M_s~47–49 emu/g), but poor dielectric properties, whereas dl-alanine derived powders yield ceramics with high resistivity (~3.4×10⁸ Ω cm), low dielectric loss (tan δ~0.003 at 1 MHz) and high magnetization (46 emu/g). Dielectric dispersion and impedance analysis show good correlation with the changes in the ceramic microstructure.     

Polyaniline (PANI)–Co0.5Mn0.5Fe2O4 nanocomposite: Synthesis,characterization and magnetic properties evaluation

Polyaniline (PANI)/Cobalt-manganese ferrite, (PANI)/Co_0.5Mn_0.5Fe₂O₄, nanocomposite was synthesized by oxidative chemical polymerization of aniline in the presence of ammonium peroxydisulfate (APS). Microwave assisted synthesis method was used for the fabrication of core CoFe₂O₄ nanoparticles. The structural, morphological, thermal and magnetic properties of the nanocomposite were investigated in detail by X-ray diffraction (XRD), fourier-transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The average crystallite size of (PANI)/Co_0.5Mn_0.5Fe₂O₄ nanocomposite by the line profile method was 20±9 nm. The magnetization measurements revealed that (PANI)/Co_0.5Mn_0.5Fe₂O₄ nanocomposite has superparamagnetic behavior with blocking temperature higher than 300 K. The saturation magnetization of the composite is considerably low compared to that of CoFe₂O₄ nanoparticles due to the partial replacement of Co²⁺ ions and surface spin disorder. As temperature decreases, both coercivity and strength of antiferromagnetic interactions increase which results in unsaturated magnetization of the nanocomposite.