Microwave-assisted synthesis of iron(III) oxyhydroxides/oxides characterized using transmission electron microscopy,X-ray diffraction,and X-ray absorption spectroscopy

Microwave-assisted synthesis of iron oxide/oxyhydroxide nanophases was conducted using iron(III) chloride titrated with sodium hydroxide at seven different temperatures from 100 to 250 °C with pulsed microwaves. From the X-ray diffraction (XRD) results, it was determined that there were two different phases synthesized during the reactions which were temperature dependent. At the lower temperatures, 100 and 125 °C, it was determined that an iron oxyhydroxide chloride was synthesized. Whereas, at higher temperatures, at 150 °C and above, iron(III) oxide was synthesized. From the XRD, we also determined the FWHM and the average size of the nanoparticles using the Scherrer equation. The average size of the nanoparticles synthesized using the experimental conditions were 17, 21, 12, 22, 26, 33, 28 nm, respectively, for the reactions from 100 to 250 °C. The particles also had low anisotropy indicating spherical nanoparticles, which was later confirmed using transmission electron microscopy (TEM). Finally, X-ray absorption spectroscopy (XAS) studies show that the iron present in the nanophase was present as iron(III) coordinated to six oxygen atoms in the first coordination shell. The higher coordination shells also conform very closely to the ideal or bulk crystal structures.     

Magnetic behavior of iron oxide nanoparticle–biomolecule assembly

Iron oxide nanoparticles of 8–20 nm in size were investigated as an assembly with biomolecules synthesized in an aqueous solution. The magnetic behavior of the biomolecule–nanoparticles assembly depends sensitively on the morphology and hence the distribution of the nanoparticles, where the dipole coupling between the nanoparticles governs the overall magnetic behavior. In assemblies of iron oxide nanoparticles with trypsin, we observe a formation of unusual self-alignment of nanoparticles within trypsin molecules. In such an assembly structure, the magnetic particles tend to exhibit a lower spin-glass transition temperature than as-synthesized bare iron oxide nanoparticles probably due to reduced interparticle couplings within the molecular matrix. The observed self-alignment of nanoparticles in biomolecules may be a useful approach for directed nanoparticles assembly.     

Preparation of superparamagnetic magnetite nanoparticles by reverse precipitation method: Contribution of sonochemically generated oxidants

Magnetic iron oxide nanoparticles were successfully prepared by a novel reverse precipitation method with the irradiation of ultrasound. TEM, XRD and SQUID analyses showed that the formed particles were magnetite (Fe₃O₄) with about 10 nm in their diameter. The magnetite nanoparticles exhibited superparamagnetism above 200 K, and the saturation magnetization was 32.8 emu/g at 300 K. The sizes and size distributions could be controlled by the feeding conditions of FeSO₄ · 7H₂O aqueous solution, and slower feeding rate and lower concentration lead to smaller and more uniform magnetite nanoparticles. The mechanisms of sonochemical oxidation were also discussed. The analyses of sonochemically produced oxidants in the presence of various gases suggested that besides sonochemically formed hydrogen peroxide, nitrite and nitrate ions contributed to Fe(II) ion oxidation.     

High coercivity and superparamagnetic behavior of nanocrystalline iron particles in alumina matrix

Single-domain nanoscale magnetic iron particles have been embedded uniformly in an amorphous matrix of alumina using a pulsed laser deposition technique. Structural characterization by transmission electron microscopy (TEM) reveals the presence of a crystalline iron and an amorphous alumina phase. Fine particle magnetism have been investigated by carrying out field and temperature dependence of magnetization measurements using superconducting quantum interference device magnetometer. The particle size of Fe in Al₂O₃ matrices prepared by changing the deposition time of Fe, have been found to be 9, 7 and 5 nm from TEM studies. At 10 K, the coercivities of these samples are found be 450, 350 and 150 Oe, respectively. At 300 K, the coercivity of Fe–Al₂O₃ sample decreases from 100 to 50 Oe as the particle size decreases from 9 to 7 nm and finally the sample turns superparamagnetic when the Fe particle size becomes around 5 nm. Based on the calculated value of blocking temperature, T_B, (481 K), magnetic anisotropy K (4.8×10⁵ erg/cm³) for Fe, and the Boltzmann constant k_B (1.38×10⁻¹⁶ erg/K) from T_B=KV/25k_B, the mean radius of Fe particles is found to be 9.3 nm. in one of the samples. This is in good agreement with the particle size measured using TEM studies.     

Surface characterisation of dextran-coated iron oxide nanoparticles prepared by laser pyrolysis and coprecipitation

The favoured mechanism of adsorption of dextran on the surface of maghemite nanoparticles (5 nm) prepared by laser pyrolysis seems to be the collective hydrogen bonding between dextran hydroxyl groups and iron oxide particle surface. After heating, the formation of a surface complex between the polysaccharide oxygen atoms and the surface iron atoms gave rise to a stronger bonding.     

Sonochemical synthesis,structural, magnetic and grain size dependent electrical properties of NdVO4 nanoparticles

NdVO₄ nanoparticles are successfully synthesized by efficient sonochemical method using two different structural directing agents like CTAB and P123. The phase formation and functional group analysis are carried out using X-ray diffraction (XRD) and fourier transform infra red (FT-IR) spectra, respectively. Using Scherrer equation the calculated grain sizes are 27 nm, 24 nm and 20 nm corresponding to NdVO₄ synthesized by without surfactant, with CTAB and P123, respectively. The TEM images revealed that the shape of NdVO₄ particles is rice-like and rod shaped particles while using CTAB and P123 as surfactants. The growth mechanism of NdVO₄ nanoparticles is elucidated with the aid of TEM analysis. From electrical analysis, the conductivity of NdVO₄ nanoparticles synthesized without surfactant showed a higher conductivity of 5.5703 × 10⁻⁶ S cm⁻¹. The conductivity of the material depends on grain size and increased with increase in grain size due to the grain size effect. The magnetic measurements indicated the paramagnetic behavior of NdVO₄ nanoparticles.     

Catalytic dechlorination of 2,4-dichlorophenol by Ni/Fe nanoparticles prepared in the presence of ultrasonic irradiation

In this study, nickle/iron (Ni/Fe) nanoparticles were synthesized by liquid phase reductive method in the presence of 20 kHz ultrasonic irradiation to improve nanoparticles’ disparity and avoid agglomeration. The characterized results showed that this method has obviously modified most of the particles in term of sizes and specific surface areas. Meanwhile, the improved nanoscale Ni/Fe particles were employed for the reductive dechlorination of 2,4-dichlorophenol (2,4-DCP) as a function of some influential factors (Ni content, Ni/Fe nanoparticles dosage, reaction temperature and initial pH values) and degradation path. Experimental results showed that 2,4-DCP was first adsorbed by Ni/Fe nanoparticles, then quickly reduced to o-chlorophenol (o-CP), p-chlorophenol (p-CP), and finally to phenol (P). The application of ultrasonic irradiation for Ni/Fe nanoparticles synthesis was found to significantly enhance the removal efficiency of 2,4-DCP. Consequently, the phenol production rates increased from 68% (in the absence of ultrasonic irradiation) to 87% (in the presence of ultrasonic irradiation) within 180 min. Nearly 96% of 2,4-DCP was removed after 300 min reaction with these optimized conditions: Ni content over Fe⁰ 3 wt%, initial 2,4-DCP concentration 20 mg L⁻¹, Ni/Fe dosage 3 g L⁻¹, initial pH value 3.0, and reaction temperature 25 °C. The degradation of 2,4-DCP followed pseudo-first-order kinetics reaction and the apparent pseudo-first-order kinetics constant was 0.0737 min⁻¹. This study suggested that the presence of ultrasonic irradiation in the synthesis of nanoscale Ni/Fe particles could be a promising technique to enhance nanoparticle’s disparity and avoid agglomeration.     

Improved synthesis of aluminium nanoparticles using ultrasound assisted approach and subsequent dispersion studies in di-octyl adipate

The present work reports on an efficient and simple one pot synthetic approach for aluminium nanoflakes and nanoparticles based on the intensification using ultrasound and provides a comparison with the conventional approach to establish the cutting edge process benefits. In situ passivation of aluminium particles with oleic acid was used as the method of synthesis in both the conventional and ultrasound assisted approaches. The aluminium nanoflakes prepared using the ultrasound assisted approach were subsequently dispersed in di-octyl adipate (DOA) and it was demonstrated that a stable dispersion of aluminium nanoflakes into di-octyl adipate (DOA) is achieved. The morphology of the synthesized material was established using the transmission electron microscopy (TEM) analysis and energy dispersive X-ray analysis (EDX) and the obtained results confirmed the metal state and nano size range of the obtained aluminium nanoflakes and particles. The stability of the aluminium nanoflakes obtained using ultrasound assisted approach and nanoparticles using conventional approach were characterized using the zeta potential analysis and the obtained values were in the range of −50 to +50 mV and −100 to +30 mV respectively. The obtained samples from both the approaches were also characterized using X-ray diffraction (XRD) and particle size analysis (PSA) to establish the crystallite size and particle distribution. It was observed that the particle size of the aluminium nanoflakes obtained using ultrasound assisted approach was in the range of 7–11 nm whereas the size of aluminium nanoparticles obtained using conventional approach was much higher in the range of 1000–3000 nm. Overall it was demonstrated that the aluminium nanoflakes obtained using the ultrasound assisted approach showed excellent morphological characteristics and dispersion stability in DOA showing promise for the high energy applications.     

Chloroethene dehalogenation with ultrasonically produced air-stable nano iron

Zerovalent iron (ZVI) has been demonstrated to be suitable for the dehalogenation of environmental pollutants such as chloroethenes. The construction of ZVI reactive barriers by conventional engineering measures is expensive and limited to shallow aquifers. The use of nanosized ZVI particles opens new opportunities to construct ZVI barriers with less invasive techniques. However, nanosized particles of pure ZVI are pyrophoric and react spontaneously with atmospheric oxygen.In this study, nanosized air-stable ZVI particles were produced by applying ultrasound to a solution of Fe(CO)₅ in edible oil. The resulting iron nanoparticles were dispersed in a carbon matrix, and coated with a non-crystalline carbon layer of approx. 2.5 nm. Although, these nanoparticles are non-pyrophoric and stable in air, dechlorination of tetrachloroethene was demonstrated in synthetic aqueous medium and in polluted groundwater. Additionally, hydrogen was formed. Due to the larger surface area, significantly higher mass-normalized reaction rates of the novel carbon-coated nanoparticles were obtained as compared to conventional bulk ZVI material. Surface normalized pseudo-first-order-reaction rates of k_SA = 3.49 × 10^?3 L h^?1 m^?2 and 2.33 × 10^?2 L h^?1 m^?2 were calculated for the nano-ZVI and the bulk ZVI, respectively. Dechlorination reaction products of the novel nano-ZVI were trichloroethene, cis-dichloroethene, vinyl chloride, ethene, and ethane.     

Magnetic properties of marine tertiary tephra investigated over a wide temperature range

We report on a detailed investigation of the magnetic properties of tertiary tephra as a function of temperature and magnetic field, over a wide temperature. The tertiary tephra were chosen from two marine sites in the South Indian Ocean. The measurements were made using the electron spin resonance (ESR) technique in the temperature range 4–1100 K and a SQUID magnetometer at temperatures from 4 to 300 K.We show that the magnetic properties of the studied ashes are mainly due to two contributions, a ferrimagnetic one and a paramagnetic one. At moderate magnetic fields, B<1 T, in the large temperature interval, 20 K<T<1000 K, the magnetic response is dominated by the ferrimagnetic component present in the ashes. The experimental data concerning the hysteresis cycles and the Curie temperatures allow us to suggest that (titano-)magnetite and a haematite-like phase could be responsible for the observed ferrimagnetic behaviour. In addition, by electron microscopy investigations, two types of morphologies containing Fe ions have been detected: vitreous splinters, in which embedded crystallised nanoparticles (60–200 nm) are present, and smectite flakes which are crystallised and in which the Fe concentration is higher than in the splinters. We speculate that the ferrimagnetic contribution is due to the nanoparticles and the paramagnetic one results from lamellar flake-like particles.     

Synthesis and characterization of L10 FePt nanoparticles from Pt–Fe3O4 core-shell nanoparticles

Pt/Fe₃O₄ core-shell nanoparticles have been prepared by a modified polyol method. Pt nanoparticles were first prepared via the reduction of Pt(acac)₂ by polyethylene glycol-200 (PEG-200), and layers of iron oxide were subsequently deposited on the surface of Pt nanoparticles by the thermal decomposition of Fe(acac)₃. The nanoparticles were characterized by XRD and HR-TEM. The as-prepared Pt/Fe₃O₄ nanoparticles have a chemically disordered FCC structure and transformed into chemically ordered fct structure after annealing in reducing atmosphere (4% H₂, 96% Ar) at 700 °C. The ordered fct FePt phase has high magnetic anisotropy with coercivity reaching 7.5 kOe at room temperature and 9.3 kOe at 10 K.     

Growth of SnO2 nanoparticles via thermal evaporation method

Tin oxide (SnO₂) nanoparticles were fabricated by evaporation of Sn powers at 1000 °C in air pressure. The as-deposited SnO₂ particles were single crystal structure, which were mostly spherical shape, the diameter of particles was ranging from 200 to 600 nm. The photoluminescence (PL) spectrum showed that a sharp emission peak at around 393 nm with the excitation wavelength at 325 nm, which suggested possible applications in nanoscaled optoelectronic devices. It was also found that the holding time affects the morphology of the products. The formation mechanism of SnO₂ particles was discussed.     

Preparation of magnetic FeCo nanoparticles by coprecipitation route

Magnetic FeCo nanoparticles with high saturation magnetization (M_s = 148 emu/g) at 15 kOe were prepared by a coprecipitation route. The value of M_s for FeCo nanoparticles depends on the ratio of Fe to Co components. The size of the nanoparticles was confirmed by transmission electron microscopy (TEM) images, and morphology of the nanoparticles was obtained by field emission scanning electron microscopy (FE-SEM) images. The crystal structure of the nanoparticles dependent on annealing was characterized by X-ray diffraction data. The magnetic properties were characterized by saturation magnetization from a hysteresis loop by VSM.     

Large-scale synthesis and magnetic properties of cubic CoO nanoparticles

We present the synthesis, microstructural and magnetic characterization of cubic CoO nanoparticles with well-controlled size and shape. The as-synthesized CoO nanoparticles are stable because of the organic coating that occurred in situ. The Néel temperature is 225 and 280 K for the 42 and 74 nm CoO particles, respectively. The CoO nanoparticles exhibit anomalous magnetic properties, such as large moments, coercivities and loop shifts. These results provide evidence for the formation of spin compensated random system in CoO. The structurally distorted and magnetically disordered surface layer ferromagnetic phase played an important role in the magnetic behavior of CoO nanoparticles. The smaller is the particle size, the stronger is the contribution of the ferromagnetic phase and the more is the surface layer helpful to enhance the observed coercivity and the exchange bias.     

Temperature dependent structural and optical properties of tin oxide nanoparticles

Nanocrystalline tin oxide (SnO₂) powders were synthesized through wet chemical route using tin metal as precursor. The morphology and optical properties, as well as the effect of sintering on the structural attributes of SnO₂ particles were analyzed using Transmission electron microscopy (TEM), UV–visible spectrophotometry (UV–vis) and X-ray diffraction (XRD), respectively. The data revealed that the lattice strain plays a significant role in determining the structural properties of sintered nanoparticles. The particle size was found to be 5.8 nm, 19.1 nm and 21.7 nm for samples sintered at 300 °C, 500 °C, and 700 °C, respectively. Also, the band gaps were substantially reduced from 4.1 eV to 3.8 eV with increasing sintering temperatures. The results elucidated that the structural and optical properties of the SnO₂ nanoparticles can be easily modulated by altering sintering temperature during de novo synthesis.     

Iron and Cobalt-based magnetic fluids produced by inert gas condensation

Iron and cobalt nanoparticle fluids have been prepared by inert-gas condensation into an oil/surfactant mixture. Superparamagnetic iron fluids (mean particle size=11.6±0.4 nm) and ferromagnetic cobalt fluids (mean particle size=51.6±3.4 nm) produced by this technique are promising candidates for magnetic targeting and hyperthermia applications.     

Photoluminescence study on amino functionalized dysprosium oxide–zinc oxide composite bifunctional nanoparticles

An organic dispersion of 9–15 nm size stable dysprosium oxide incorporated zinc oxide nanocomposites exhibiting luminescence in the visible region has been synthesised by a wet chemical precipitation technique at room temperature. Tetraethoxysilane TEOS [(C₂H₅O)₄Si], (3-aminopropyl) trimethoxysilane (APTS) and a 1:1 mixture of TEOS–APTS have been used as capping agents to control the particle size as well as to achieve uniform dispersion of composite nanoparticles in methanol medium. X-ray diffractometer (XRD) analysis reveals the formation phase of amino-functionalised colloidal dysprosium oxide incorporated ZnO composite nanoparticles to be of zincite structure. The Transmission Electron Microscopy (TEM) images show that the particles are spheroids in shape, having average crystalline sizes ranging from 9 to 15 nm. The photoluminescence (PL) observed in these composites has been attributed to the presence of near band edge excitonic emission and existence of defect centres. The time correlated single photon counting studies of the composite nanoparticles exhibited three decay pathways. The enhanced PL emission intensity of solid state fluorescence spectra of samples is attributed to the absence of vibrational relaxation process.     

Feasibility study of iron mineral separation from red mud by high gradient superconducting magnetic separation

The disposal of bayer red mud tailings now seriously threats the environment safety. Reduction and recycling of red mud is now an urgent work in aluminum industry. High gradient superconducting magnetic separation (HGSMS) system was applied to separate the extreme fine RM particles (<100 μm) into high iron content part and low iron content part. Two sorts of RM were fed in the HGSMS. The iron oxide contents in concentrates were about 65% and 45% when RM 1# and RM 2# were fed respectively. Meanwhile, the residues contained 52.0% or 14.1% iron oxide in residues after eight separation stages when RM 1# and RM 2# were fed respectively. The mass recovery of iron concentrates was about 10% after once separation process regardless of RM 1# or RM 2# was fed. Extreme fine particles (<10 μm) could be captured in the HGSMS. Intergrowth of Fe and other elements is disadvantages for iron mineral separation from RM by HGSMS. Some improvement should be studied to enhance the efficiency of iron separation. It is possible for HGSMS to separate RM into high iron content part and low iron content part, the former part could be used in iron-making furnace and the later part could be recycling to sintering process for alumina production or used as construction material.     

Intensification of ultrasound-assisted process for the preparation of spindle-shape sodium zinc molybdate nanoparticles

In the present work, sodium zinc molybdate (SZM) nanoparticles were prepared using conventional and an innovative ultrasound assisted co-precipitation of sodium molybdate, zinc oxide and HNO₃ at different temperatures. Prepared product was characterized by XRD, TEM, FT-IR, particle size distribution (PSD), TGA and DTA techniques. TEM analysis shows the spindle-shaped morphology of the formed SZM nanoparticles. The average particle size of SZM nanoparticles is found to be lower in case of sonochemical method (78.3 nm) compared to conventional method (340.2 nm) which is attributed to faster solute transfer rate due to ultrasonic irradiation leading to rapid nucleation and restricted growth of SZM nanoparticles. Further, the kinetics of synthesis of SZM nanoparticles are studied using the sonochemical method at different operating temperature and conventional method at 80 °C. It is shown that the rate of reaction is significantly faster at 40 °C compared to other temperatures and also conventional method. This can be attributed to intense cavity collapse at lower temperature (low vapour pressure) compared to higher temperature (high vapour pressure) of the reaction mixture.     

Site-directed research of magnetic nanoparticles in magnetic drug targeting

The targeting of ferrofluids composed of 20 nm magnetic particles was studied through simulation and animal experiment. The results showed that some magnetic particles were concentrated in the target area depending on the applied magnetic field. Through theoretical analysis, the retention of the magnetic nanoparticles in a target area is due to large magnetic liquid beads formed by the magnetic field.