Microwave-hydrothermal synthesis of γ-Fe2O3 nanoparticles and their magnetic properties

Nanosized γ-Fe₂O₃ is synthesized by the microwave-hydrothermal method. Powder X-ray diffraction and transmission electron microscopic studies showed that the average particle size is 10 nm. Magnetic studies reveal that the γ-Fe₂O₃ nanoparticles are superparamagnetic at room temperature, with a superparamagnetic blocking temperature of 200 K. The magnetic characteristics of the nanoparticles indicate their strongly interacting nature.     

Boronic acid functionalized superparamagnetic iron oxide nanoparticle as a novel tool for adsorption of sugar

Synthesis of boronic acid functionalized superparamagnetic iron oxide nanoparticles has been reported. Magnetite nanoparticles were prepared by simple co-precipitation from Fe²⁺ and Fe³⁺ solution. m-Aminophenyl boronic acid was attached to iron oxide particles through 3,4-dihydroxy benzaldehyde through CN bond. X-ray diffraction and selected area electron diffraction have shown the formation of inverse spinel phase magnetite of both as prepared and functionalized magnetite particles. FTIR shows attachment of boronic acid-imine onto iron oxide surface through enediol group. Transmission electron microscopy shows well dispersion of boronic acid functionalized particles of size 8 ± 2 nm. Vibration sample magnetometry shows both the particles are superparamagnetic at room temperature having saturation magnetization (Ms) 52 emu/g. In this work the affinity of these boronic acid functionalized particles towards sugar binding was studied taking dextrose sugar as a model. The influence of pH and sugar concentration has been extensively investigated. The results show that such boronic acid modified superparamagnetic particles are efficient support for sugar separation having maximum sugar loading capacity (60 µg/50 µl) at pH 8.     

Ultrasonic-assisted synthesis and magnetic studies of iron oxide/MCM-41 nanocomposite

Iron oxide nanoparticles were stabilized within the pores of mesoporous silica MCM-41 amino-functionalized by a sonochemical method. Formation of iron oxide nanoparticles inside the mesoporous channels of amino-functionalized MCM-41 was realized by wet impregnation using iron nitrate, followed by calcinations at 550 °C in air. The effect of functionalization level on structural and magnetic properties of obtained nanocomposites was studied. The resulting materials were characterized by powder X-ray diffraction (XRD), high-resolution transmission electron microscopy and selected area electron diffraction (HRTEM and SAED), vibrating sample and superconducting quantum interface magnetometers (VSM and SQUID) and nitrogen adsorption–desorption isotherms measurements. The HRTEM images reveal that the most of the iron oxide nanoparticles were dispersed inside the mesopores of silica matrix and the pore diameter of the amino-functionalized MCM-41 matrix dictates the particle size of iron oxide nanoparticles. The obtained material possesses mesoporous structure and interesting magnetic properties. Saturation magnetization value of magnetic iron oxide nanopatricles stabilized in MCM-41 amino-functionalized by in situ sonochemical synthesis was 1.84 emu g⁻¹. An important finding is that obtained magnetic nanocomposite materials exhibit enhanced magnetic properties than those of iron oxide/MCM-41 nanocomposite obtained by conventional method. The described method is providing a rather short preparation time and a narrow size distribution of iron oxide nanoparticles.     

Hydrothermal synthesis of magnetite crystals: From sheet to pseudo-octahedron

In this paper, we developed a hydrothermal method to fabricate sheet-like and pseudo-octahedral magnetite crystals. X-ray diffraction (XRD) confirmed the products were pure spinel-structured magnetite. Scanning electron microscopy (SEM) was used to investigate the morphology of the obtained crystals. By carefully regulating the initial NaOH concentrations, the morphology of the products could be changed from sheet-like crystals to pseudo-octahedral crystals. Transmission electron microscopy (TEM) analysis indicated the sheet-like crystals were the oriented aggregation of nanoparticles. Pseudo-octahedral magnetite crystals were single crystalline, and were obtained by dissolution-recrystallization of the sheet-like crystals. Vibrating sample magnetometer (VSM)) suggested the magnetic properties of the products were strongly related to the morphology. The coercivity of the sheet-like magnetite crystals was 100 Oe, larger than 30 Oe of the pseudo-octahedral crystals, but the saturation magnetization of the sheet-like magnetite crystals was 40 emu/g, smaller than 85 emu/g of the pseudo-octahedral crystals.     

Novel environmentally friendly synthesis of superparamagnetic magnetite nanoparticles using mechanochemical effect

A novel method for synthesizing superparamagnetic magnetite nanoparticles in water system via coprecipitation under an environmentally friendly condition has been developed. In this method, an almost neutral suspension containing ferrous hydroxide and goethite is used as the starting suspension and subjected to a ball-milling treatment. The product was characterized by transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, dynamic light scattering, superconducting quantum interference device magnetometry, and Mössbauer spectroscopy. The mechanochemical effect generated by the ball-milling treatment promoted the reaction between ferrous hydroxide and goethite even at room temperature, resulting in the formation of homogeneous magnetite nanoparticles. Simultaneously, it also contributed to crystallize the formed magnetite nanoparticles while inhibiting the particle growth. This resulted in the formation of ultrafine magnetite nanoparticles of about 10 nm having a single crystal structure. This method could provide ferromagnetic magnetite nanoparticles with superparamagnetism under the moderate condition without neither heating nor any additives such as surfactant and organic solvent.     

A facile route to sonochemical synthesis of magnetic iron oxide (Fe3O4) nanoparticles

A facile sonochemical approach was applied for the large scale synthesis of iron oxide magnetic nanoparticles (NPs) using inexpensive and non-toxic metal salts as reactants. The as-prepared magnetic iron oxide NPs has been characterized by XRD, TEM, EDS, and VSM. X-ray diffraction (XRD) and EDS analysis revealed that Fe₃O₄ NPs have been successfully synthesized in a single reaction by this simple method. Transmission electron microscopy (TEM) data demonstrated that the particles were narrow range in size distribution with 11 nm average particle size. Moreover, TEM measurements also show that the synthesized nanoparticles are almost spherical in shape. The magnetization curve from vibrating sample magnetometer (VSM) measurement shows that as-synthesized NPs were nearly superparamagnetic in magnetic properties with very low coercivity, and magnetization values were 80 emu/g, which is very near to the bulk value of iron oxide. The estimated value of mass susceptibility of as-synthesized nanoparticles is Xg = 5.71 × 10^− 4 m³/kg.     

Structural and magnetic properties of Mn nanoparticles prepared by arc-discharge

Mn nanoparticles are prepared by arc discharge technique. MnO, α-Mn, β-Mn, and γ-Mn are detected by X-ray diffraction, while the presence of Mn₃O₄ and MnO₂ is revealed by X-ray photoelectron spectroscopy. Transmission electron microscopy observations show that most of the Mn nanoparticles have irregular shapes, rough surfaces and a shell/core structure, with sizes ranging from several nanometers to 80 nm. The magnetic properties of the Mn nanoparticles are investigated between 2 and 350 K at magnetic fields up to 5 T. A magnetic transition occurring near 43 K is attributed to the formation of the ferrimagnetic Mn₃O₄. The coercivity of the Mn nanoparticles, arising mainly from Mn₃O₄, decreases linearly with increasing temperature below 40 K. Below the blocking temperature T_B ≈ 34 K, the hysteresis loops exhibit large coercivity (up to 500 kA/m), owing to finite size effects, and irreversibility in the loops is found up to 4 T, and magnetization is not saturated up to 5 T. The relationship between structure and the magnetic properties are discussed.     

Synthesis and characterizations of Ni-Fe@spinel oxide core-shell nanoparticles

Core-shell Ni-Fe@ferrite nanoparticles with an average diameter of 14 nm and shell thickness of 3 nm were synthesized through a redox-transmetalation process. The alloy core and spinel oxide shell were verified by X-ray photoelectron spectroscopy, X-ray diffraction, and transmission electron microscopy. The hydrophobic oleylamine molecules on the surface were replaced by hydrophilic meso-2,3-Dimercaptosuccinic acid to make the nanoparticles to be water-soluble. X-ray diffraction study of the as-prepared core-shell nanoparticles indicates that they remained face centered cubic alloy core and spinel shell form in air. Magnetic measurements indicate that the core-shell nanoparticles exhibit superparamagnetic and exchange bias characteristics at 300 K and 5 K, respectively.     

Facile preparation of carbon coated magnetic Fe3O4 particles by a combined reduction/CVD process

In this work, we report a simple method for the preparation of magnetic carbon coated Fe₃O₄ particles by a single step combined reduction of Fe₂O₃ together with a Chemical Vapor Deposition process using methane. The temperature programmed reaction monitored by Mössbauer, X-ray Diffraction and Raman analyses showed that Fe₂O₃ is directly reduced by methane at temperatures between 600 and 900 °C to produce mainly Fe₃O₄ particles coated with up to 4 wt% of amorphous carbon. These magnetic materials can be separated into two fractions by simple dispersion in water, i.e., a settled material composed of large magnetic particles and a suspended material composed of nanoparticles with an average size of 100-200 nm as revealed by Scanning Electron Microscopy and High-resolution Transmission Electron Microscopy. Different uses for these materials, e.g., adsorbents, catalyst supports, rapid coagulation systems, are proposed.     

Preparation and magnetic behavior of carbon-encapsulated iron nanoparticles by detonation method

Carbon-encapsulated iron (Fe@C) nanoparticles with core/shell structure have been successfully synthesized by detonation method, using a homemade composite explosive precursor. The detonation reaction was ignited by a non-electric detonator in nitrogen gas in an explosion vessel. The as-prepared detonation products were characterized by X-ray Diffraction, Transmission electron Microscopy, Raman spectroscopy and X-ray fluorescence. The magnetic behavior of the Fe@C materials was measured by vibrating sample magnetometer. The results showed that the detonation products were made up of the body centered cubic iron core and the graphitic carbon shell, of which the core diameter was in the range of 15–50 nm. Raman spectroscopy indicated that both graphitic and amorphous carbon occured in the outside shell structures. The hysteresis loops showed the as-made Fe@C nanoparticles were of superparamagnetic at 300 K temperature. A detonation reaction mechanism was proposed to explain the growth process of Fe@C nanoparticles based on these results.     

Characterization and magnetic properties of Sm- and Gd-substituted CoFe2O4 nanoparticles prepared by forced hydrolysis in polyol

Pure nanoparticles of the CoFe_2−xRE_xO₄ (RE = Gd, Sm; x = 0.0, 0.1) system have been prepared by forced hydrolysis in polyol. The insertion of Sm³⁺ and Gd³⁺ cations into the cobalt ferrite structure has been investigated. X-ray micro-analysis (EDX) shows that the RE contents are close to the nominal ones. X-ray diffraction (XRD) evidences a cell size increase with slight distortions in the spinel-like lattice indicating the entrance of RE³⁺ ions. Micro-Raman spectroscopy confirms the cubic inverse-spinel structure and rules out the existence of impurities like hematite. Magnetic measurements (SQUID) show important differences in the magnetic properties of the unsubstituted and substituted particles. All the particles are superparamagnetic at room temperature and ferrimagnetic at low temperature. However, their main magnetic characteristics appear to be directly dependent on the RE content.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Synthesis and characterization of ultrafine poly(vinylalcohol phosphate) coated magnetite nanoparticles

Nanosized magnetite (Fe3O4) particles showing superparamagnetism at room temperature have been prepared by controlled coprecipitation of Fe2+ and Fe3+ in presence of highly hydrophilic poly(vinylalcohol phosphate)(PVAP). The impact of polymer concentration on particle size, size distribution, colloidal stability, and magnetic property has been extensively studied. The aqueous suspension of magnetite, prepared using 1% PVAP solution is stable for four weeks at pH 5-8. X-ray diffractograms show the formation of nanocrystalline inverse spinel phase magnetite. Transmission Electron Microscopy confirmed well dispersed cubic magnetite particles of size of about 5.8 nm. Dynamic Light Scattering measurement shows narrow distribution of hydrodynamic size of particle aggregates. Infrared spectra of samples show strong Fe--O--P bond on the oxide surface. UV-visible studies show aqueous dispersion of magnetite formed by using 1% PVAP solution is stable at least for four weeks without any detoriation of particle size. Magnetization measurements at room temperature show superparamagnetic nature of polymer coated magnetite nanoparticles.     

Solid-phase reaction synthesis of mesostructured tungsten disulfide material with a high specific surface area

A mesostructured tungsten disulfide (WS₂) material was prepared through a solid-phase reaction utilizing ammonium tetrathiotungstate as the precursor and n-octadecylamine as the template. The as-synthesized WS₂ material was characterized by X-ray powder Diffraction (XRD), Low-temperature N₂ Adsorption (BET method), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). The characterization results indicate that the WS₂ material has the typical mesopore structure (3.7 nm) with a high specific surface area (145.9 m²/g), and large pore volume (0.18 cm³/g). This approach is novel, green and convenient. The plausible mechanism for the formation of the mesostructured WS₂ material is discussed herein.     

Electrical, optical and vibrational characteristics of nano structured yttrium barium stannous oxide synthesized through a modified combustion method

A single step combustion process for the preparation of nanoparticles of yttrium barium stannous oxide is reported in this paper. The structure, phase purity and particulate properties of the as prepared nano YBa₂SnO_5.5 powder were examined by X-ray diffraction and transmission electron microscopy. The as prepared powder obtained itself is phase pure and possess cubic structure with lattice constant 8.240 Å. The particle size of the as prepared sample from Transmission Electron Microscopy analysis is in the range of ∼15 nm. Vibrational studies carried out on the as prepared powder also confirm the cubic structure of the as prepared sample. The thermal stability of the nano particle is analyzed by thermo gravimetric and differential thermal analysis. The material is a semiconductor with excellent luminescent properties. Chemical compatibility of the sample with YBCO is analyzed. The YBCO-YBa₂SnO_5.5 composite showed T_c(0) at 92 K.     

Fabrication of nanocomposite particles with superparamagnetic and luminescent functionalities

A new kind of superparamagnetic luminescent nanocomposite particles has been synthesized using a modified Stöber method combined with an electrostatic assembly process. Fe₃O₄ superparamagnetic nanoparticles were coated with uniform silica shell, and then 3-aminopropyltrimethoxysilane was used to terminate the silica surface with amino groups. Finally, negatively charged CdSe quantum dots (QDs) were assembled onto the surface of the amino-terminated SiO₂/Fe₃O₄ nanoparticles through electrostatic interactions. X-ray diffraction (XRD), transmission electron microscopy (TEM), microelectrophoresis, UV-vis absorption and emission spectroscopy and magnetometry were applied to characterize the nanocomposite particles. Dense CdSe QDs were immobilized on the silica surface. The thickness of silica shell was about 35 nm and the particle size of the final products was about 100 nm. The particles exhibited favorable superparamagnetic and photoluminescent properties.     

One-pot synthesis of iron oxide-carbon core-shell particles in supercritical water

The quantitatively limited use of hydrogen peroxide in supercritical water allows for the in situ formation of iron oxides and graphitic carbon from ferrocene in one step. The structure of the particles prepared at 400-500 °C is comprised of nano- to micro-meter size of magnetite and maghemite cores covered with graphitic carbon shells. The morphology and size of the core-shell particles and the phase composition of iron-oxide cores are different dependent on the preparation conditions. The particles prepared at 400 °C contain, as dominant iron-oxide phase, the magnetite core particles ranging from nano- to micro-meter scales with no morphological regularity, while those prepared at 500 °C are comprised of hexagram shape and micro-meter size of maghemite cores. The observed morphology, the dimension of the core particles, and the dominant phase composition suggested that the iron-oxide cores would be formed through the oxidation of iron(II) to iron(III) and two different hydrolysis paths. Furthermore, the higher preparation temperature of 500 °C has shown a tendency to form smaller crystallite sizes of polycrystalline iron-oxide cores. The decrease of subcrystal sizes in the vicinity of superparamagnetic thresholds effects the reduction of coercivity in the ferromagnetic hysteresis.     

The enhanced coercivity for the magnetite/silica nanocomposite at room temperature

Magnetite/silica nanocomposite was synthesized by a facile solvothermal processing at 150 °C for about 10 h. X-ray diffraction (XRD) analysis revealed the effect of annealing on the crystallinity of silica. Transmission electron microscopy (TEM) images showed the good dispersion of magnetite in the silica matrix. Magnetic properties of the nanocomposite were characterized by vibration sample magnetometer (VSM), and the enhanced coercivity was explained by the intrinsic anisotropy of the particles enhanced by the interparticle dipolar fields.     

Microstructure control on thermoelectric properties of Ca0.96Sm0.04MnO3 synthesised by co-precipitation technique

Nanopowder of Ca_0.96Sm_0.04MnO₃ (CSM) perovskite was prepared by chemical co-precipitation technique. It was characterized and studied by X-ray diffraction and Transmission Electron Microscopy. Nano-crystalline CSM phase having grain size of 60-70 nm can be prepared by calcination at 1073 K for 6 h in air. The obtained nanopowder was pressed, sintered at 1373 K for 24 h to obtain a dense sample. In comparison, CSM samples prepared from normal powder need sintering temperature of 1623 K to reach a similar microstructure, showing the efficiency of nanopowder to decrease the sintering temperature. The thermoelectric properties of samples prepared with two different processes were studied. The Seebeck coefficient and the thermal conductivity slightly decrease by using the nanopowder while the value of the electrical resistivity does not change. This results in the same figures of merit for the two materials.     

Synthesis of magnetic nanoparticles in bicontinuous microemulsions. Effect of surfactant concentration

Precipitation was accomplished at 80 °C for magnetic nanoparticles in bicontinuous microemulsions that were stabilized with different concentrations of a surfactants mixture of dodecyltrimethylammonium bromide/didodecyldimethylammonium bromide (3/2, w/w). These nanoparticles were characterized by X-ray Diffraction, Scanning Transmission Electronic Microscopy (STEM), and Vibrating Sample Magnetometry (VSM), which demonstrated that they were composed of magnetite or a mixture of magnetite-maghemite. The particles were found to have average diameters between 6.9 and 7.9 nm with relatively narrow particle size distribution and showed possible superparamagnetic behavior. In addition, we observed an inverse dependence of particle size on surfactant concentration. Yields obtained in these precipitation reactions were found to be up to three times higher than those typically reported in specialized literature about precipitation of magnetic nanoparticles in reverse microemulsions.