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%).     

In situ synthesis of vanadium carbide–copper nanocomposite by a modified mechanochemical combustion method

Synthesis of vanadium carbide–copper nanocomposite was achieved via mechanochemical combustion method from reactant mixture of V₂O₅, CuO, C and Mg powders. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS). X-ray diffraction investigations indicated that the combustion products were V₄C₃, V₂C and Cu phases. Microstructural studies showed that a nanostructured powder with a mean particle size of about 100 nm was procured in the samples milled for 90 min.     

Structural,morphological and magnetic parameters investigation of multiferroic (1-x)Bi2Fe4O9- xCoFe2O4 nanocomposite ceramics

(1-x)Bi₂Fe₄O₉- xCoFe₂O₄ (0.0≤ x ≤1.0) multiferroic nanocomposites were prepared by wet chemical procedures combining reverse chemical co-precipitation and Pechini-type sol–gel techniques followed by mechanical blending process. The XRD and SAED results showed that the diffraction patterns are perfectly indexed to the constituent phases present in composite samples. The crystallite sizes of the constituent phases were 35.4 and 39.4 nm for cobalt and bismuth ferrites, respectively. The characteristic peaks in FT-IR spectra confirmed formation and purity of all specimens. FESEM micrographs revealed the uniform phase distribution with the mean grain size of approximately 40 and 230 nm for CoFe₂O₄ and Bi₂Fe₄O₉, respectively. TEM micrograph indicated suitable distribution in the as-prepared composite sample. The VSM results revealed that saturation and remnant magnetization increase by increasing CFO content in composites. Based on the results obtained from M-H curves, magnetic properties of composites did not originate only from linear combination of parent phases. The recorded coercivity values of all nanocomposites, for example 1443 Oe for x = 0.4 were higher than those of each parent phase i.e. 708 Oe for CoFe₂O₄ and 149 Oe for Bi₂Fe₄O_9, showing a noticeable improvement in magnetic properties.     

Synthesis and structural characterization of ultrafine terbium oxide powders

Glycine-nitrate self-propagating high-temperature synthesis was used to synthesize terbium oxide nanopowders whose phase transformations were investigated by methods of high-temperature differential scanning calorimetry, dilatometry, and X-ray diffraction analysis. The as-prepared powders consisting of Tb₇O₁₂ and Tb₁₁O₂₀ phases were converted to Tb₂O₃ after calcination at 600–800 °C in reducing atmosphere. The sintering behavior of Tb₂O₃ was studied under microwave heating up to 1780 °C. The microstructure of the powders and ceramics was investigated by scanning electron microscopy. Near full-density material was obtained at about 1620 °C. Further temperature increases causes a deterioration of the ceramics microstructure due to monoclinic Tb₂O₃ phase formation.     

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.     

Effects of Al particle size and nitrogen pressure on AlN combustion synthesis

This study investigates the combustion synthesis of AlN fibers using an NH₄Cl additive and reports the effects of Al particle size (3, 30, and 180 µm) and N₂ pressure (0.10, 0.25, and 0.50 MPa) on the purity and morphology of AlN fibers. The combustion temperature was directly measured during the synthesis to elucidate the formation mechanism of the AlN fibers. The phase purity and morphology of the products were studied using X-ray diffraction and scanning electron microscopy, respectively. When the particle size of Al was reduced from 180 to 3 µm, the purity of the AlN product increased significantly owing to the large reaction area, which increased the combustion temperature. Furthermore, lower N₂ pressures enhanced the formation of AlN nanofibers due to the accelerated gasification of Al. The optimum values of the particle size of Al and the N₂ pressure for the formation of high-purity AlN nanofibers were found to be 3 µm and 0.10 MPa, respectively.     

Synthesis,crystal structure,characterization and magnetic property of a new organophosphonate-based polyoxovanadate

A novel organophosphonate-based polyoxovanadate, Cs_1·5Na_3.5[H{V₃(H₂O)O₃}{O₃PC- (OH)(CH₃)PO₃}₃]·15H₂O (1) has been synthesized and further investigated by single-crystal X-ray diffraction analysis, IR spectrum, UV–vis spectroscopy, X-ray powder diffraction, thermogravimetric analysis and X-ray photoelectron spectroscopy. Single-crystal X-ray analysis reveals that compound 1 crystallizes in the triclinic space group P-1 with a = 9.506(3) Å, b = 15.150(5) Å, c = 17.915(6) Å, V = 2437.9(14) ų and Z = 2. Compound 1 exhibits a ring-shaped cluster with three branches of the 1-hydroxyethane 1, 1-diphosphonic acid [HEDP = H₂O₃P(OH)C(CH₃)PO₃H₂] ligands. Furthermore, the magnetic property of compound 1 has also been studied.     

Synthesis,characterization, thermal study,and crystal structure of a new layered alkaline earth metal sulfonate: Sr[C2H4(SO3)2]

A rare two-dimensional layered inorganic–organic hybrid material, strontium sulfonate Sr[C₂H₄(SO₃)₂] was synthesized by hydrothermal reaction of strontium chloride hexahydrate and ethane disulfonic acid at 160 °C. Single-crystal X-ray diffraction was utilized for structural determination. Data showed that the compound, crystallized in the monoclinic system and space group of C2/c. With cell parameters a = 8.3183(7) Å, b = 5.4416(5) Å and c = 14.9784(13) Å. The new material was extensively studied by DRIFT-infrared spectroscopy, thermogravimetric analysis, SEM and powder X-ray diffraction. Results show that the compound is thermally stable.     

Influence of cobalt ferrite content on the structure and magnetic properties of (CoFe2O4)X (SiO2-PVA)100-X nanocomposites

(CoFe₂O₄)_X(SiO₂-PVA)_100-X (X = 5, 25, 50, 75 and 95%) nanocomposites were prepared via sol-gel route and annealed at 700 and 1100 °C. The influence of CoFe₂O₄ content on the structure, morphology and magnetic properties of nanocomposites was studied. X-ray diffraction patterns, Mössbauer and Fourier transform infrared spectra revealed the formation of CoFe₂O₄ as unique magnetic phase. The crystallinity degree increases with the CoFe₂O₄ content and the annealing temperature. Transmission electron microscopy images revealed the spherical shape of the obtained nanocomposites. Mössbauer spectra exhibit typical magnetic sextets, allowing the calculation of the cations distribution among tetrahedral and octahedral sites and the stoichiometry of CoFe₂O₄. A strong correlation between the particle morphology and the magnetic properties of nanocomposites was found. The highest saturation magnetization was identified for (CoFe₂O₄)₉₅(SiO₂-PVA)₅ nanocomposite.     

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.     

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.     

Investigation on mechanochemical combustion behavior of Mg–V2O5–Co3O4-C reactive system to synthesize VC–Co nanocomposite powder

VC–Co nanocomposite powders were obtained by mechanochemical combustion synthesis from a mixture of V₂O₅, Co₃O₄, C and Mg powders. The synthesized powders were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). VC–Co nanocomposite was directly produced after 10 min milling through a mechanically induced self-sustaining reaction without further heat treatment. TEM analysis showed that a nanostructured powder with a mean particle size of 100 nm was procured in the sample milled for 10 min.     

Synthesis,structure and characterization of a new nonlinear optical calcium borate [Ca2B5O9]·[H(OH)2]

A new nonlinear optical crystal [Ca₂B₅O₉]·[H(OH)₂] (1) has been synthesized under hydrothermal condition. Compound 1 crystallizes in the monoclinic space group C2 with lattice constants a = 10.111(2) Å, b = 7.754(11) Å, c = 6.198(14) Å, β = 127.04(3)° and Z = 2. The fundamental building block (FBB) of 1 is a [B₅O₁₂] unit with two BO₃ triangles and three BO₄ tetrahedra. 1 was characterized by single-crystal X-ray diffraction, IR and UV–Vis spectroscopy, thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD) respectively. Also, powder second harmonic generation (SHG) measurements indicate that 1 is phase matchable and displays a SHG response of about 3.5 times that of KDP (KH₂PO₄).     

Mechanochemical-molten salt synthesis of α-Al2O3 platelets

The polyaluminium chloride (PACl) precursor was used for a simple and scaled-up mechanochemical-molten salt synthesis of α-Al₂O₃ platelets. PACl, as a low temperature α-Al₂O₃ precursor, was firstly mechanically activated by high-energy ball milling for 5 min, followed by a next 5 min ball milling in the presence of a NaCl–KCl salt mixture. The starting formation temperature of the α-Al₂O₃ phase was 600 °C. In the subsequent annealing in the temperature range of 660–1000 °C, the α-Al₂O₃ phase with a well developed plate-like morphology was obtained. The products were characterized by X-ray powder diffractometry, scanning electron microscopy (SEM), and thermal analysis (DTA, TG) and solution ²⁷Al NMR spectroscopy.     

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.     

Production of TiB2 by SHS and HCl leaching at different temperatures: Characterization and investigation of sintering behavior by SPS

Sub-micron sized TiB₂ ceramic powders were prepared via self-propagating high-temperature synthesis (SHS) followed by HCl leaching at different temperatures. Purified powders obtained using optimum process parameters were consolidated by field assisted sintering technology/spark plasma sintering (FAST/SPS) technique. Phase and microstructural analyses of both the powder and sintered samples were carried out by X-ray diffractometer (XRD) and scanning electron microscope (SEM). The chemical analyses and particle size measurements of the specimen were conducted by inductively coupled plasma-mass spectrometry (ICP-MS) and dynamic light scattering (DLS) techniques. The final properties of the sintered sample were determined in terms of density and microhardness. The effects of different HCl leaching temperatures on the formation, microstructure, particle size, purity and sintering behavior of the SHS-produced TiB₂ powders were investigated. The SHS reaction of TiO₂-B₂O₃-Mg powders as a starting mixture yielded MgO, Mg₃(BO₃)₂ and Mg beside the desired phase TiB₂. All three magnesium containing by-products were completely removed by performing hot HCl leaching. TiB₂ powders after SHS reaction and leaching with 9.3 M HCl for 30 min at 80 °C revealed a minimum purity of 98.4% and a homogenous particle size distribution with an average particle size of 536 nm. In the ultimate SPS experiment which was conducted at 1500 °C for 5 min under a pressure of 50 MPa, a relative density of 94.9% and a micro-hardness value of 24.56 GPa were achieved.     

Enhanced performance of Fe2O3 doped yttria stabilized zirconia hollow fiber membranes for water treatment

Fe₂O₃ powders were introduced as sintering aid to fabricate yttria-stabilized zirconia (YSZ) hollow fiber membranes using a combined wet-spinning and post-sintering method. The obtained Fe₂O₃-YSZ hollow fiber membranes show enhanced performance for water treatment with fine crystal structure in terms of bending strength and pure water permeability. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), and thermogravimetric analysis (TGA) along with mechanical tests were employed to investigate the structural evolution in the sintering process and the effect of Fe₂O₃. It is suggested that the Fe₂O₃ dopants dissolve into YSZ at elevated temperatures, providing defect sites and vacancies for fast ion migration, favoring for densification and grain growth of the YSZ, which yields dense microstructures of fine crystallites at relatively low sintering temperature. The Fe₂O₃-YSZ hollow fiber membranes sintered at 1150 °C show a 3-fold increase of the permeate flux of pure water (F) (743 L m⁻² h⁻¹) along with comparable bending strength (152 MPa) compared to pure YSZ membranes. This modified method can reduce sintering costs and therefore fabrication costs which should pave the way for scale-up production for ceramic hollow fiber membranes.     

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).     

Development of novel magnetic-dielectric ceramics for enhancement of reflection loss in X band

The purpose of this research was to develop BaFe_9.5Al_1.5CrO₁₉-xCaCu₃Ti₄O₁₂ nanocomposites (x=10%, 20%, 30%, 40%, 50%) and investigate their structural and magnetic features. The substituted barium hexaferrite (BaFe_9.5Al_1.5CrO₁₉) nanoparticles and calcium copper titanate (CaCu₃Ti₄O₁₂) particles were synthesized by the auto-combustion sol-gel method. The structural, chemical composition and morphology of CaCu₃Ti₄O₁₂ (CCTO) and the nanocomposites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy, respectively. The magnetic and microwave properties of nanocomposites were also investigated by vibrating sample magnetometer and vector network analyzer, respectively. The results confirmed that 1100 °C is the optimum synthesis temperature for CCTO, the mean particles size of the CCTO particles changing from 220 nm (at 850 °C) to 2.18 µm (1250 °C). The SEM micrograph revealed that in all of the BaM-xCCTO nanocomposites (x=10%, 20%, 30%, 40%, 50%), the CCTO dielectric particles were attached to the substituted barium hexaferrite nanoparticles, indicating the effectiveness of the adopted synthesis method. Due to the presence of a dielectric phase in the nanocomposites the saturation magnetization decreases from 22 emu/g to 12 emu/g. The coercive field was a slightly larger than substituted barium hexaferrite and increased from 5.558 kOe for substituted barium hexaferrite to 5.813 kOe for BaM-50CCTO due to hindered motion of the domain walls by the dielectric phase and also to the collective behavior of agglomerated barium ferrite nanoparticles. The BaM-30CCTO nanocomposite shows the highest value of reflection loss compared to other nanocomposites. The reflection dip frequency of BaM-30CCTO nanocomposite was −48.85 dB at 10.93 GHz.     

Relaxor behavior and ferroelectric properties of a new Ba4SmFe0.5Nb9.5O30 tungsten bronze ceramic

Unfilled tungsten bronze ceramics with a composition of Ba₄SmFe_0.5Nb_9.5O₃₀ were prepared by the conventional solid-state sintering method. The phase, microstructure, dielectric and ferroelectric properties were studied. Room temperature XRD results indicated that the ceramic occurs in the tetragonal space group P4bm phase with cell parameters of a=b=12.4712(2) Å and c=3.9430(2) Å. The temperature-dependent dielectric properties, XRD data and Raman spectra data indicated that BSFN ceramics exhibit no phase changes from 35 °C to 450 °C. Fitting of a Vogel-Fulcher relationship with an activated energy E_a of 0.11 eV indicates an unambiguous dielectric relaxor state near room temperature. Furthermore, the BSFN ceramics exhibited residual polarization and coercive field of 3.45 µC/cm² and 24.65 kV/cm, respectively.