Solution combustion synthesis of FeCr2O4 powders for pigment applications: Effect of fuel type

Solution combustion synthesis of iron chromite was reported using iron(III) nitrate nonahydrate and chromium(III) nitrate nonahydrate as starting materials, as well as glycine, urea, citric acid, and ethylene glycol as fuels. The influence of fuel type on the structure, molecular, microstructure as well as chromatic properties of samples was investigated. The X-ray diffraction (XRD) patterns showed that unlike themodynamical prediction, glycine fuel led to strongest combustion and consequent highest XRD peak intensities and lower lattice parameters. Moreover, the change of fuel type and mixing of fuels affected XRD data. Fourier transform infrared analysis showed that the band position of Cr–O and Fe–O bonds were shifted to higher frequencies by using of fuels with weaker combustion reactions. In addition, scanning electron micrographs showed that different morphologies of FeCr₂O₄ particles were obtained depending on the fuel type and ratios. Energy-dispersive X-ray spectroscopy analysis of the samples showed that oxygen concentration of samples was less than that of stoichiometric ratio of FeCr₂O₄ due to local reducing atmosphere. Furthermore, chromatic properties of the powders showed that the pigment synthesized with glycine fuel has a better and lighter grayish brown color than the other ones and can be used as a suitable industrial candidate to create a brown color in the ceramic glaze.     

Effects of the fuel type and fuel content on the specific surface area and magnetic properties of solution combusted CoFe2O4 nanoparticles

In this work, the different fuels (citric acid, glycine and urea) at the various fuel to oxidant ratios (ϕ=0.5, 0.75, 1 and 1.25) were used for solution combustion synthesis of CoFe₂O₄ nanoparticles. The phase evolution, microstructure, specific surface area and magnetic properties of the solution combusted CoFe₂O₄ nanoparticles were investigated by X-ray diffraction, thermal analysis, electron microscopy, adsorption-desorption isotherms and vibrating sample magnetometry techniques. The specific surface area of the combusted products decreased with the increase of fuel to oxidant ratio (ϕ), irrespective of the fuel type. However, the specific surface area for the glycine fuel was higher than the others, due to the higher combustion rate for releasing gaseous products. Furthermore, the solution combusted CoFe₂O₄ powders by the glycine fuel exhibited the higher saturation magnetization (63.6 emu/g) on account of their higher crystallinity and particle size.     

Turquoise blue nanocrystalline pigment based on Li1.33Ti1.66O4: Synthesis and characterization

Turquoise blue Li_1.33Ti_1.66O₄ is an environmentally friendly inorganic pigment, it was synthesized using the sol-gel method. The particle size was determined by X-ray diffraction (XRD) pattern and through high-resolution transmission electron microscopy (HRTEM), obtaining an average diameter of 27.5 ± 3 nm. The pigment shows a brilliant turquoise blue color, due to Ti³⁺-Ti⁴⁺ intervalence charge transfer transitions and presents thermal stability up to 1000 °C. The Li_1.33Ti_1.66O₄ nanoparticles were characterized by using X-ray diffraction, Raman scattering and UV-vis absorption spectroscopy. The color properties and the thermal stability of this pigment suggest that it has potential to be applied as a satisfactory pigment for cosmetics, plastics, glasses and inks.     

A novel approach for solution combustion synthesis of tungsten oxide nanoparticles for photocatalytic and electrochromic applications

Tungsten oxide (WO₃) and tungsten oxide hydrate (WO₃.H₂O) nanoparticles were synthesized via a novel solution combustion synthesis (SCS) method. Various organic fuels (i.e. oxalic acid, glycine, and citric acid) and heat sources were used to obtain different morphologies of nanoparticles. Combustion thermodynamic relations were explained based on propellant chemistry. Adiabatic temperature (T_ad) and specific impulse (I_sp) were also obtained. The synthesized nanoparticles were investigated by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and UV–Visible spectrophotometer. XRD patterns indicated that the structures were transformed from orthorhombic and amorphous structures to monoclinic and tetragonal ones, respectively, upon combustion on the hot plate. Fourier-transform infrared (FTIR) spectra provided evidence of WO₆ octahedral. SEM images showed different microstructures from sponge or rock-like to fine spherical particles with up to 100 nm size. The obtained band gap of all samples was higher than 2.6 eV which is the band gap of bulk tungsten oxide. The synthesized WO₃ nanoparticles showed over 50% photocatalytic efficiency for the degradation of azo dye. The results exhibited that the nanoparticles can be used to make the electroactive layer for electrochromic applications.     

Synthesis and characterization of PANI nanostructures for supercapacitors and photoluminescence

Polyaniline structures were synthesized through a chemical method using citric acid and oxalic acid as carriers and 5???m size ??-alumina particles as a template. The obtained nano-size pristine products were characterized using X-ray diffraction, infrared spectroscopy, scanning electron microscopy, optical absorption spectroscopy, photoluminescence spectroscopy and cyclic voltammetry (CV). Nanofibrous PANI was obtained with oxalic acid, nanoparticles with oxalic acid and ??-alumina, net-like nanostructures with citric acid and spherical nanoparticles with citric acid and ??-alumina. The high intensity photoluminescence of PANI prepared with oxalic acid as a carrier is possibly due to greater chances of exciton formation resulting from increased ??-electron mobility. Electrochemical studies of PANI electrodes in 2.0?M H₂SO₄ were carried out at various scan rates. The CVs showed rectangular shape with added pronounced oxidation and reduction peaks.     

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.     

Preparation of nanocrystalline Sr3Al2O6 powders via citric acid precursor

Sr₃Al₂O₆ was synthesized via citric acid precursor. The effects of the molar ratio of citric acid to total metal cations concentration (CA/M) on the formation of Sr₃Al₂O₆ were investigated. Increasing the CA/M promoted the formation of Sr₃Al₂O₆. Single-phase and well-crystallized Sr₃Al₂O₆ was obtained from the CA/M = 1, CA/M = 2 and CA/M = 4 precursor at temperature 1200 °C, 1100 °C and 900 °C, respectively. Differential thermal analysis and thermogravimetric (DTA/TG), X-ray diffractometry (XRD) and field emission scanning electron microscopy (FESEM) were used to characterize the precursors and the derived oxide powders. Sr₃Al₂O₆ nanoparticles with a diameter of about 50-70 nm were obtained.     

A comparative study on citrate sol-gel and combustion synthesis methods of CoAl2O4 spinel

CoAl₂O₄ spinel was successfully synthesized by combustion synthesis method using glycine and urea by 1:1 molar ratio as fuels and sol-gel process using citric acid as a chelating agent. The as-synthesized powders were calcined at desired temperatures to obtain CoAl₂O₄ spinel as a single phase. X-ray diffraction, thermogravimetric, and differential thermal analysis results revealed that the formation of CoAl₂O₄ spinel in combustion method needs 300°C higher temperatures than those of sol-gel. Scanning electron microscopy and transmission electron microscopy analysis results revealed that “sol-gel spinel” had nanometric particle size which was smaller than those of “combustion spinel.” Temperature programed reduction with hydrogen and Fourier transform infrared spectroscopy results declared that there was a little residual cobalt oxide in combustion spinel while there is no oxide resided in “sol-gel spinel.” Consequently, the sol-gel method has more benefit in synthesizing spinel with sulfate precursors than combustion.     

Comparison of the microwave-induced combustion and solid-state reaction for the synthesis of LiMn2O4 powder and their electrochemical properties

In the current research, we proposed a new method called microwave-induced combustion synthesis to produce LiMn₂O₄ powders. The microwave-induced combustion synthesis entails the dissolution of metal nitrates, and urea in water, and then heating the resulting solution in a microwave oven. Spinel LiMn₂O₄ powders were successfully synthesized by microwave-induced combustion. The microwave-heated LiMn₂O₄ powders annealed at various temperatures in the range of 600–800 °C were determined. The resultant powders were characterized by X-ray diffractometer (XRD), and scanning electron microscopy (SEM). The annealed samples were used as cathode materials for lithium-ion battery, for which their discharge capacity and electrochemical characteristic properties in terms of cycle performance were also investigated. The LiMn₂O₄ cell provides a high initial capacity of 133 mAh/g and excellent reversibility. The excellent capacity and reversibility were attributed to LiMn₂O₄ powders with small and uniform particle size produced by microwave-induced combustion synthesis.     

Synthesis of (Fe,Cr)2O3 solid solution pigment powders for ink application

Iron chromite pigment was synthesized via solution combustion using iron(III) nitrate nonahydrate and chromium(III) nitrate nonahydrate as starting materials, and glycine, urea, citric acid, and ethylene glycol as fuels. The effect of postheating temperature on the structure, microstructure, and chromatic properties of the synthesized powders was also studied. X-ray diffraction patterns showed that the as-synthesized powders were amorphous to crystalline FeCr₂O₄ phases, depending on fuel type. Moreover, regardless of the fuel type, postheating led to the d-space shift and oxidation and formation of (Fe,Cr)₂O₃ solid solution. Phase transformation of FeCr₂O₄ to (Fe,Cr)₂O₃ solid solution was observed at 500/750°C depending on the dominant phase present in the as-synthesized particles. Fourier transform infrared analysis illustrated a shift in the band position of octahedral M–O and tetrahedral M–O bonds due to the movement of Fe cations and the lattice shrinkage by increasing the postheating temperature. Moreover, scanning electron micrographs showed that Fe_0.7Cr_1.3O₃ semispherical fine particles consisted mainly of porous and spongy FeCr₂O₄ particles due to the oxidation and phase transformation during postheating. According to chromatic measurements, the ink prepared by using the powders synthesized in the presence of glycine and post-heated at 500°C showed reddish-brown color which could be considered a promising candidate for tile decoration application. Furthermore, rheology studies revealed that the prepared ink showed non-Newtonian shear thinning behavior.     

Magnetic phase transition and magneto-dielectric analysis of spinel chromites: MCr2O4 (M = Fe,Co and Ni)

In this work, we present magnetic phase transition temperatures and magneto-dielectric coupling in MCr₂O₄ (M = Fe, Co and Ni) ceramics, synthesized using sol–gel auto-combustion route. In order to develop their respective crystalline textures, all these chromites were calcined at 650?°C for 2?h. X-ray diffraction patterns confirmed that FeCr₂O₄ had a rhombohedral structure while NiCr₂O₄ and CoCr₂O₄ exhibited a spinel-type cubic structure. The presence of relevant elements in the specific stoichiometric ratios was confirmed using energy dispersive X-ray spectroscopy. The shapes and sizes of the grains for all the samples were determined using the images obtained from a field emission scanning electron microscope. Temperature dependent magnetic analysis have shown that FeCr₂O₄, CoCr₂O₄ and NiCr₂O₄ are ferromagnetic at 5?K and their magnetic phase transition temperatures were measured as 80, 83 and 90?K, respectively. Spin-orbit interference was also studied through magneto-dielectric coupling for these chromites using a modified impedance analyzer set-up.     

Synthesis and structural characterization of layered Li[Ni1/3Co1/3Mn1/3]O2 cathode materials by ultrasonic spray pyrolysis method

The layered Li[Ni_1/3Co_1/3Mn_1/3]O₂ materials were synthesized by a spray pyrolysis method using citric acid as a polymeric agent. The Li[Ni_1/3Co_1/3Mn_1/3]O₂ powders were characterized by means of X-ray diffraction (XRD), charge/discharge cycling, cyclic voltammetry, and high-resolution transmission electron microscopy (TEM). The discharge capacity increases linearly with the increase of the upper cut-off voltage limit. TEM analysis showed that particles in the as-prepared powder possessed a polycrystalline structure. During cycling, the particle structure is mostly preserved although some surface grains on the polycrystalline particle became separated and transformed to the spinel phase.     

Synthesis of multi-walled carbon nanotube bundles on the Fe-Co-Mo/Al2O3 catalyst

The Fe-Co-Mo/Al₂O₃ catalyst was synthesized by ??wet combustion?? with the use of metal nitrates and citric acid. Multi-walled carbon nanotubes obtained by the catalytic pyrolysis of propylene were shown to grow on this catalyst in the form of bundles. The influence of process parameters on the properties of the nanotubes was studied.     

Effects of carbon source and carbon content on electrochemical performances of Li4Ti5O12/C prepared by one-step solid-state reaction

Li₄Ti₅O₁₂/C composites were synthesized by one-step solid-state reaction method using four commonly used organic compounds or organic polymers as carbon source, i.e., polyacrylate acid (PAA), citric acid (CA), maleic acid (MA) and polyvinyl alcohol (PVA). The physical characteristics of Li₄Ti₅O₁₂/C composites were investigated by X-ray diffraction, electron microscopy, Raman spectroscopy, particle size distribution and thermogravimetry-derivative thermogravimetry techniques. Their electrochemical properties were characterized by cyclic voltammograms, electrochemical impedance spectra, constant current charge–discharge and rate charge–discharge. These analyses indicated that the carbon source and carbon content have a great effect on the physical and electrochemical performances of Li₄Ti₅O₁₂/C composites. An ideal carbon source and appropriate carbon content effectively improved the electrical contact between the Li₄Ti₅O₁₂ particles, which enhanced the discharge capacity and rate capability of Li₄Ti₅O₁₂/C composites. PAA was the best carbon source for the synthesis of Li₄Ti₅O₁₂/C composites. When the carbon content was 3.49 wt.% (LiOH·H₂O/PAA molar ratio of 1), as-prepared Li₄Ti₅O₁₂/C showed the maximum discharge capacity. At 0.2 C, initial capacity of the optimized sample was 168.6 mAh g⁻¹ with capacity loss of 2.8% after 50 cycles. At 8 and 10 C, it showed discharge capacities of 143.5 and 132.7 mAh g⁻¹, with capacity loss of 8.7 and 9.9% after 50 cycles, respectively.     

Synthesis and electrochemical properties of Li[Li0.07Ni0.1Co0.6Mn0.23]O2 as a possible cathode material for lithium-ion batteries

The layered Li[Li_0.07Ni_0.1Co_0.6Mn_0.23]O₂ materials were synthesized by sol-gel method with glycine or citric acid as chelating agent. The prepared materials were characterized by means of XRD, SEM and Raman spectroscopy. Li/Li[Li_0.07Ni_0.1Co_0.6Mn_0.23]O₂ cells were assembled and subjected to charge-discharge studies at different C rates, viz 0.2, 1, 2 and 4 C. Although the samples showed less discharge capacity at 4 C rate the fade in capacity per cycle is lesser than that of capacity fade at 0.2 C rate. The citric acid assisted sample is found to be superior in terms of discharge capacity, capacity retention rate and also in thermal stability to that of sample prepared with glycine as chelating agent.     

Surface modification of Cr2O3 nanoparticles with 3-amino propyl trimethoxy silane (APTMS). Part 1: Studying the mechanical properties of polyurethane/Cr2O3 nanocomposites

The surface of Cr₂O₃ nanoparticles was modified with various amounts of 3-amino propyl trimethoxy silane (APTMS). Thermal gravimetric analysis (TGA), turbidimeter and Fourier transform infrared (FTIR) spectroscopy were utilized in order to investigate APTMS grafting on the nanoparticles. Then, polyurethane nanocomposites were prepared using various loadings of silane modified Cr₂O₃ nanoparticles. The nanoparticles dispersion in the coating matrix was studied by a field emission scanning electron microscopy (FESEM). Dynamic mechanical thermal analysis (DMTA) and tensile test were utilized in order to investigate the mechanical properties of the nanocomposites. Results obtained from FTIR, TGA and turbidimeter measurements revealed that the organic functional groups of the silane were successfully grafted on the surface of the nanoparticles. The mechanical properties of the polyurethane were significantly enhanced using 2 wt% Cr₂O₃ nanoparticles modified with 0.43 g silane/5 g pigment compared with other samples.     

Size-controlled high magnetization CoFe2O4 nanospheres and nanocubes using rapid one-pot sonochemical technique

Highly crystalline single phase spherical and monodisperse cobalt ferrite (CoFe₂O₄) nanoparticles (NPs) with uniform shape and size distribution have been synthesized by one pot-rapid sonochemical method. The effect of different solvents, such as aqueous, alcoholic, and a mix of water/ethanol in 1:1 volume ratio on the shape, size, and crystalline structure of CoFe₂O₄ NPs were studied using X-ray diffraction, transmission electron microscopy, energy dispersive spectroscopy and Fourier transform infrared spectroscopy. The size of CoFe₂O₄ nanoparticle was controlled in the range from 20 to 110 nm based on the solvent medium used in the synthesis process. Furthermore, the evolution from spherical to cubic morphology of cobalt ferrite NPs is achieved by simply changing the solvent medium from aqueous to alcoholic medium. The magnetic properties of all the synthesized CoFe₂O₄ NPs were studied by vibrating sample magnetometer (VSM) at room temperature. The magnetization value was found to be particle size dependent, and high magnetization (Ms) of 92.5 emu/g was obtained for the CoFe₂O₄ NPs sample synthesized in a mixed solution of water and ethanol. A possible reaction mechanism for the formation of cobalt ferrite NPs by the sonochemical technique was discussed. The facile method adopted in our study appears to be a promising route for synthesis of highly crystalline nanoparticles within short times and without the need for using any calcination process.     

Synthesis and magnetic properties of nano-sized Cu0.5Ni0.5Fe2O4 via citrate and aloe vera: A comparative study

In this report, Cu_0.5Ni_0.5Fe₂O₄ nanoparticles were synthesized by solgel using eco-friendly aloe vera extract and citric acid separately and their properties were discussed. Structural, Functional, morphological, magnetic properties of the samples were characterized using X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Transmission electron microscopy (TEM), Vibrating sample magnetometer (VSM). XRD exhibited the samples have single phase cubic spinel with average size of 46.4?nm and 35.45?nm. Two characteristics bands of ferrite were confirmed by FTIR. TEM indicated different morphology of the samples with some regularity. VSM data showed that higher coercivity for the sample prepared by aloe vera extract.     

Synthesis and magnetic properties of monodisperse CoFe2O4 nanoparticles coated by SiO2

The monodisperse CoFe₂O₄ nanoparticles were synthesized by a modified chemical coprecipitation method. Coating SiO₂ on the surface of the CoFe₂O₄ nanoparticles was carried out to keep single domain particles non-interacting with cubic magnetocrystalline anisotropy. The Curie temperatures (T_c) of the monodisperse CoFe₂O₄ nanoparticles can be accurately measured because the SiO₂ shells prevented the aggregation and growth of nanoparticles at high temperature. The magnetic properties of the CoFe₂O₄@SiO₂ nanoparticles with core-shell structure in a wide temperature range (300～950?K) were investigated. It is remarkable that the coercive field (H_c) of CoFe₂O₄ nanoparticles increased from about 760?Oe to 1806?Oe after being coated with SiO₂, which increased by 137.6% compared to the uncoated samples at 300?K. The saturation magnetization (M_s) of the CoFe₂O₄@SiO₂ nanoparticles is 34.59?emu/g, which is about 52% of the naked CoFe₂O₄ nanoparticles value (66.51?emu/g) at 300?K. The hysteresis loops of the CoFe₂O₄@SiO₂ nanoparticles showed an orderly magnetic behavior at high temperature, such as the M_s, remanence magnetization (M_r) and H_c decreased as temperature increasing, being equal to zero near T_c. This is a good indication that the CoFe₂O₄@SiO₂ nanoparticles are suitable for a wide variety of technological applications at high temperature.     

Structural and ferroelectric properties of hafnium substituted BiFeO3 multiferroics synthesized via auto combustion technique

A series of BiFe_1-xHf_(3/4)xO₃ ( 0%, 5%, 10%, 15% and 20%) nanoparticles were synthesized by simple auto combustion technique using citric acid as a fuel. Thermogravimetric (TGA), differential thermogravimetric (DTA), structural, magnetic, dielectric and ferroelectric analyses were investigated. Thermogravimetric analysis provides information of temperature at which phase develops (600?°C). DTA predicts ferroelectric to paraelectric transformation temperature which is found to be 822?°C. X-ray diffraction (XRD) results confirm formation of distorted rhombohedral structure for all compositions along with few traces of Bi₂₅FeO₄₀. The tolerance factor is increased from 0.845 to 0.853 due to larger ionic radius of Hf⁴⁺ substitution on Fe site. Crystallite size (D) is found in the range of 24.2–30.48?nm. Saturation magnetization (Ms) is increased to 16 times and remanent magnetization (Mr) is increased to 8 times than that of pure BiFeO₃. This increment in magnetic parameters is due to reduction of oxygen vacancies, small crystalline size (less than 62?nm), structural distortion and unbalancing condition for antiferromagnetic magnetic moments of Fe³⁺ ions. Dielectric parameters depict decrement behavior with increasing of applied field up to 3?GHz. For Fe_1-xHf_(3/4)xO₃, lower value of dielectric permittivity for all compositions is due to reduction of polarization and less growth of grains but more growth of grain boundaries because of mismatching of Hf and Fe³⁺ ions. P-E hysteresis loop changes from round shape to elliptical shape and it confirms less lossy nature of ferroelectric loops. Higher values of Ms as well as Mr but lower values of dielectric constant as well as remanent polarization for these nanoparticles make them useful for MeRAM (magnetoelectric random access memory) and high resonant applications.