Effects of synthesis variables on the magnetic properties of CoFe2O4 nanoparticles

Cobalt ferrite nanoparticles (CoFe₂O₄) have been synthesized using precipitation in water solution with polyethylene glycol as surfactant. Influence of various synthesis variables included pH, reaction time and annealing temperature on the magnetic properties and particle sizes has also been studied. Structural identification of the samples was carried out using Thermogravimetric and Differential thermal analysis, X-ray diffraction, Fourier transform infrared spectroscopy, Scanning electron microscopy, High resolution transmission electron microscopy. Vibrating sample magnetometer was used for the magnetic investigation of the samples. Magnetic properties of nanoparticles show strong dependence on the particle size. The magnetic properties increase with pH of the precipitating medium and annealing temperature while the coercivity goes through a maximum, peaking at around 25 nm.     

Structure and magnetic properties of nanoparticles encapsulated in carbon shells

Ni₂Y and Nd–Fe–Nb–B catalysts were used for the processing of nanoparticles by arc discharge between graphite electrodes. The products were collected from the cathode (deposit and collar) and reactor walls (soot). The ferromagnetic nanoparticles have size in the range of 10–50 nm and are encapsulated in carbon shells. The chemical composition, structure and magnetic properties of the nanoparticles have been studied. For the Ni₂Y catalyst we found that the arc discharge results in decomposition of the intermetallic Ni₂Y phase and formation of Ni nanoparticles encapsulated in carbon shells in the collar and soot, whereas yttrium oxide was found in the deposit. For the Nd–Fe–Nb–B catalysts the magnetic properties depend on the collection place and erosion rate. Fe and Fe–Nd–Nb nanoparticles were found in the soot and deposit, respectively.     

The effect of surfactants on the magnetic and optical properties of Co-doped SnO2 nanoparticles

A series of Co-doped SnO₂ nanoparticles have been synthesized by the co-precipitation route. Different amounts of surfactant have been used in order to study the effect of surfactants (CTAB) on the magnetic and optical properties. Structural analyses reveal that Co dopants are substituted into rutile SnO₂ nanoparticles without forming any secondary phase. The increase of the surfactant promotes the adsorption of organic molecules on the surfaces of nanoparticles. Meanwhile, both the ferromagnetism and the orange emission drop progressively. The dependence of ferromagnetic properties on the surfactant concentration could be explained based on the bound magnetic polaron, where the carriers are provided by oxygen vacancies. XANES spectra reveal that the electrons transfer from Co 3d bands to the surfactant ions. Such electron-transfer process suppresses the formation of oxygen vacancies and leads to the decline of the ferromagnetism and optical emission.     

Effect of reaction condition on microstructure and properties of (NiCuZn)Fe2O4 nanoparticles synthesized via co-precipitation with ultrasonic irradiation

Nano-spinel ferrites synthesized via chemical co-precipitation method are small in size and have serious agglomeration phenomenon, which makes separation difficult in the subsequent process. Ni_0.4Cu_0.2Zn_0.4Fe₂O₄ ferrites nanoparticles were synthesized via co-precipitation assisted with ultrasonic irradiation produced by ultrasonic cleaner with 20 kHz frequency using chlorinated salts and KOH as initial materials. The effects of ultrasonic power (0, 40 W, 60 W, 80 W) and reaction temperature on the microstructure and magnetic properties of ferrite nanoparticles were investigated. The structure analyses via XRD revealed the successful formation of pure (NiCuZn)Fe₂O₄ ferrites nanospinel without any impurity. The crystallites sizes were less than 40 nm and the lattice constant was near 8.39 Å. The TEM showed ferrite particle polygonal. M−H analyses performed the saturation magnetization and coercivity of ferrite nanoparticles obtained at the reaction temperature of 25℃ were higher than at 50℃ with same power. The samples exhibited the highest values of Ms 55.67 emu/g at 25℃ and 47.77 emu/g at 50℃ for 60 W and the lowest values of Hc 71.23 Oe at 25℃ for 40 W and 52.85 Oe at 50℃ for 60 W. The squareness ratio (SQR) were found to be lower than 0.5, which revealed the single magnetic domain nature (NiCuZn)Fe₂O₄ nanoparticles. All the outcomes show the ultrasonic irradiation has positive effects on improving the microstructure and increasing magnetic properties.     

Preparation and characterization of silicon oil based ferrofluid

Stable silicon oil based ferrofluid was prepared in the present investigation. Silicon oil surfactant ethoxy terminated polydimethylsiloxane was used to modify the Fe₃O₄ nanoparticles. The Fe₃O₄ nanoparticles were firstly coated with a SiO₂ layer by the hydrolysis of tetraethoxysilane. Then using the active hydroxyl groups on the surface of the SiO₂, silicon oil surfactant was covalently grafted onto the Fe₃O₄ nanoparticles surface. The ethoxy terminated polydimethylsiloxane has similar molecular chain structure and good compatibility with that of the carrier liquid, thus ensuring stable dispersion of modified Fe₃O₄ in the carrier silicon oil. The interaction between Fe₃O₄ and the modifier was characterized by IR and XPS. The crystal structure and the magnetic properties of the Fe₃O₄ nanoparticles were determined by XRD and VSM, respectively. The size and morphology of the particles were observed using TEM. The properties of the silicon oil based ferrofluid were characterized by Gouy magnetic balance. The results indicated that the ferrofluid had high magnetism and good stability. The rheological properties and thermostability of the ferrofluid were also investigated.     

Deposition of conductive TiN shells on SiO<Subscript>2</Subscript> nanoparticles with a fluidized bed ALD reactor

Conductive TiN shells have been deposited on SiO₂ nanoparticles (10–20 nm primary particle size) with fluidized bed atomic layer deposition using TDMAT and NH₃ as precursors. Analysis of the powders confirms that shell growth saturates at approximately 0.4 nm/cycle at TDMAT doses of >1.2 mmol/g of powder. TEM and XPS analysis showed that all particles were coated with homogeneous shells containing titanium. Due to the large specific surface area of the nanoparticles, the TiN shells rapidly oxidize upon exposure to air. Electrical measurements show that the partially oxidized shells are conducting, with apparent resistivity of approximately ~11 kΩ cm. The resistivity of the powders is strongly influenced by the NH₃ dose, with a smaller dose giving an order-of-magnitude higher resistivity.     

Functionalization of carbon encapsulated iron nanoparticles

Carbon-encapsulated magnetic nanoparticles are a new class of materials where the core magnetic nanoparticle is protected from reactions with its environment by graphite shells. Having a structure similar to carbon nanotubes, these nanoparticles could be potentially functionalized using methods which are already applied to those structures. We present the effects of acidic treatments based on HCl, HNO₃, and H₂SO₄ on these nanoparticles highlighting the impact on their magnetic and surface properties. We show that acidic treatments based on HNO₃ can be successfully applied for the generation of carboxylic groups on the surface of the nanoparticles. Using methylamine as a model, we demonstrate that these functional groups can be used for further functionalization with amino-containing biomolecules via diimide-activated amidation.     

Acoustic wave in a suspension of magnetic nanoparticle with sodium oleate coating

The ultrasonic propagation in the water-based magnetic fluid with doubled layered surfactant shell was studied. The measurements were carried out both in the presence as well as in the absence of the external magnetic field. The thickness of the surfactant shell was evaluated by comparing the mean size of magnetic grain extracted from magnetization curve with the mean hydrodynamic diameter obtained from differential centrifugal sedimentation method. The thickness of surfactant shell was used to estimate volume fraction of the particle aggregates consisted of magnetite grain and surfactant layer. From the ultrasonic velocity measurements in the absence of the applied magnetic field, the adiabatic compressibility of the particle aggregates was determined. In the external magnetic field, the magnetic fluid studied in this article becomes acoustically anisotropic, i.e., velocity and attenuation of the ultrasonic wave depend on the angle between the wave vector and the direction of the magnetic field. The results of the ultrasonic measurements in the external magnetic field were compared with the hydrodynamic theory of Ovchinnikov and Sokolov (velocity) and with the internal chain dynamics model of Shliomis, Mond and Morozov (attenuation).     

Electrical and magnetic properties of ε-Fe3N nanoparticles synthesized by chemical vapor condensation process

ε-Fe₃N nanoparticles synthesized by chemical vapor condensation (CVC) are covered with shells of disordered Fe₃O₄ phase, as observed by a transmission electron microscopy. The zero-field cooling and field cooling temperature dependence of magnetization, ac susceptibility as a function of frequency, magnetic hysteresis loops, and the temperature dependence of resistivity of the ε-Fe₃N nanoparticles are systematically studied. The results indicate the existence of complex magnetic properties, such as superparamagnetic behavior, exchange bias, magnetic dipole interaction, and the possible coexistence of ferromagnetic and spin-glass-like states and/or disordered surface spins of the shells at low temperatures. The temperature dependence of resistivity ρ(T) for compacted ε-Fe₃N nanoparticles in a temperature range of 110 K< T< 300 K can be well described by the mechanism of fluctuation-induced tunneling conduction, while that below 110 K can be ascribed to conducting electrons scattered by localized magnetic moments and impurity as well as the influence of freezing of spin-glass-like moments and/or disordered surface spins of the shells.     

Cu1.5[Cr(CN)6]⋅6.5H2O nanoparticles: synthesis, characterization, and magnetic properties

We have synthesized nanoparticles of Cu_1.5[Cr(CN)₆]⋅6.5H₂O of varying size by using poly(vinylpyrrolidone) (PVP) as a protecting polymer. The particle size variation has been achieved by varying the amount of the PVP surfactant with the reactants. The prepared nanoparticles have been investigated by using X-ray diffraction, transmission electron microscopy, and direct-current magnetization techniques. The nanoparticles crystallize in a face centred cubic structure (space group: Fm3m). The approximate particle sizes for the three samples are 18, 9, and 5 nm, respectively. Non-PVP nanoparticles (18 nm) show a magnetic ordering temperature of 65 K. A decrease in the magnetic ordering temperature was observed with decreasing particle size. These nanoparticles are magnetically very soft, showing negligibly small values of the coercivity and remanent magnetization. The maximum magnetization and spontaneous magnetization values at 5 K are found to decrease with decreasing particle size. The observed magnetization behaviour of the nanoparticles has been attributed to the increasing surface spin disorder with decreasing particle size.     

Magnetic nanocomposite spinel and FeCo core-shell and mesoporous systems

The fabrication of condensed silica and mesoporous silica coated spinel CoFe₂O₄ and FeCo alloy magnetic nanocomposites are reported. The encapsulation of well-defined 5 nm thick uniform silica layer on CoFe₂O₄ magnetic nanoparticles was performed. The formation of mesopores in the shell was a consequence of removal of organic group of the precursor through annealing. The NiO nanoparticles were loaded into the mesoporous silica. The mesoporous silica shells leads to a larger coercivity than that of pure CoFe₂O₄ magnetic nanoparticles due to the decrease of interparticle interactions and magneto-elastic anisotropy. In addition, the FeCo nanoparticles were coated by condensed and mesoporous silica. The condensed silica can protect the reactive FeCo alloy from oxidation up to 300 °C. However, saturation magnetization of FeCo nanoparticles coated by silica after 400 °C annealing is dramatically decreased due to the oxidation of the FeCo core. The mesoporous silica coated magnetic nanostructure loaded with NiO as a final product could be used in the field of biomedical applications.     

Characterization of CrO2-poly-vinyl pyrrolidone magnetic nanofluid

Crystalline CrO₂ nanoparticles were synthesized using chemical methods. Nanofluids were synthesized by the dispersion of CrO₂ nanoparticles in poly-vinyl pyrrolidone solution by an ultrasonicator. The structural properties of the nanoparticles were studied with the help of X-ray diffraction. The magnetic properties of the powdered CrO₂ were measured with a vibrating sample magnetometer. The magneto-resistance and ultrasonic parameters of the nanofluid were characterized. The (a) effect of calcination temperature on crystalinity of CrO₂ nanoparticles, (b) influence of sonication time on the nature of the magneto-resistance for the nanofluid, and (c) governing factor/mechanisms responsible to the ultrasonic properties are discussed.     

A facile and flexible process of β-cyclodextrin grafted on Fe3O4 magnetic nanoparticles and host-guest inclusion studies

In this study, a kind of novel surface-functionalized magnetic nanoparticles was fabricated by the Fe₃O₄ nanoparticles surface modification with mono-6-deoxy-6-(p-tolylsulfonyl)-cyclodextrin (6-TsO-β-CD), which were employed to interact with uric acid and their behavior was investigated by electrochemical methods. The architecture has been characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA), which confirmed that cyclodextrins have been effectively functionalized on the surface of Fe₃O₄ nanoparticles. The analyses of vibration sample magnetometer (VSM) verified that the nanoparticles owned good magnetic property. The grafted β-cyclodextrin on the Fe3O4 nanoparticles contributed to as a modified electrode for detecting uric acid with cyclic voltammograms. Electrochemical results revealed that the new materials could exhibit excellent molecules recognition ability and show high electrochemical response. The new nanoparticles simultaneously had unique properties of magnetic nanoparticles and cyclodextrins through combining their individual distinct advantages.     

Mössbauer investigations of Fe and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> magnetic nanoparticles for hyperthermia applications

Magnetic nanoparticles of magnetite Fe₃O₄ and Fe synthesized by physical vapor deposition with a fast highly effective method using a solar energy have been studied. Targets have been prepared from tablets pressed from Fe₃O₄ or Fe powders. Relationships between the structure of nanoparticles and their magnetic properties have been investigated in order to understand principles of the control of the parameters of magnetic nanoparticles. Mössbauer investigations have revealed that the nanoparticles synthesized from tablets of both pure iron and Fe₃O₄ consist of two phases: pure iron and iron oxides (γ-Fe₂O₃ and Fe₃O₄). The high iron oxidability suggests that the synthesized nanoparticles have a core/shell structure, where the core is pure iron and the shell is an oxidized iron layer. Magnetite nanoparticles synthesized at a pressure of 80 Torr have the best parameters for hyperthermia due to their core/shell structure and core-to-shell volume ratio.     

One-step synthesis of colloidal Mn<Subscript>3</Subscript>O<Subscript>4</Subscript> and γ-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles at room temperature

A facile room-temperature synthesis has been developed to prepare colloidal Mn₃O₄ and γ-Fe₂O₃ nanoparticles (5 to 25 nm) by an ultrasonic-assisted method in the absence of any additional nucleation and surfactant. The morphology of the as-prepared samples was observed by transmission electron microscopy. High-resolution transmission electron microscopy observations revealed that the as-synthesized nanoparticles were single crystals. The magnetic properties of the samples were investigated with a superconducting quantum interference device magnetometer. The possible formation process has been proposed.     

Structural and magnetic properties of Pt in Co/Pt multilayers

[Co(30 Å)/Pt(x Å)]₂₀ multilayers with the Pt layer thicknesses varying from 5 Å to 20 Å were characterized structurally by high angle X-ray diffraction, X-ray reflectivity, X-ray absorption spectroscopy and magnetically by X-ray magnetic circular dichroism. It is found that the structure and magnetic properties of Pt have a strong correlation with the Pt layer thickness. The 20 Å thickness Pt layer is not almost influenced by the adjacent Co layer and the nearest neighbors are dominated by Pt-Pt shells. With decreasing Pt layer thickness, the nearest neighbors are gradually dominated by Pt-Co shells and the Pt-Co intermixing regions also remarkable increase at the interfaces, especially for the 5 Å thickness Pt layer. The orbital and spin magnetic moments as well as the ratio m_orb/m_spin all decrease systematically with increasing Pt layer thickness, indicating that the interface atoms are polarized by direct Pt-Co hybridization, but that the adjacent layers are polarized by Pt-Pt interactions.     

Sonochemical preparation and characterization of photochromic MoO3 nanoparticles

The effect of ultrasound irradiation on molybdenum trioxide has been investigated. Under ultrasonic irradiation, spherical-like MoO₃ nanoparticles were obtained, while bulk-like MoO₃ nanoparticles were prepared without ultrasonic irradiation. The changes in the physicochemical properties of MoO₃ have been investigated using techniques such as X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and ultraviolet and visible spectroscopy (UV-vis). The physicochemical changes of MoO₃ due to ultrasound irradiation have been attributed to the sonochemical cavity collapse onto the molybdenum trioxide particles. The ultrasonically prepared particles can also greatly improve the photochromism efficiency.      

Synthesis and characterization of carboxymethyl dextran-coated Mn/Zn ferrite for biomedical applications

Previous studies have shown that magnetic nanoparticles possess great potential for various in vivo applications such as magnetic resonance imaging contrast enhancement, tissue repair, cancer treatment agents, and controlled drug delivery. Many of these applications require that magnetic nanoparticles be colloidally stable in biological media. The goal of this study was to obtain a magnetic fluid produced by the colloidal suspension of manganese/zinc ferrite (MZF) nanoparticles that could be stably dispersed in aqueous solution throughout the range of physiological pH and ionic strength. These superparamagnetic nanoparticles were stabilized through steric repulsion by coating with biologically compatible carboxymethyl dextran (CMDx). Samples of the resultant magnetic fluid were analyzed using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), X-ray diffraction (XRD), zeta potential measurements, dynamic light scattering, transmission electron microscopy (TEM), and SQUID magnetometry. Results show that we obtained superparamagnetic metal-oxide crystals with composition of Mn_0.24Zn_0.76Fe₂O₄. Cell viability measurements show the material is non-toxic to MCF-7 and CaCo-2 cell lines at concentrations of up to 7.5 mg/mL of particle fraction for contact time of up to 48 h.     

Evidence for magnetic interactions among magnetite nanoparticles dispersed in photoreticulated PEGDA-600 matrix

Magnetite nanoparticles having mean diameter of about 8 nm have been prepared by a thermo-chemical route. Different amounts (5 and 10% wt) of a stable dispersion of magnetite nanoparticles in n-hexane were added to polyethylene glycol diacrylate (PEGDA-600) oligomer containing 2% wt of radicalic photoinitiator. The homogenized mixture was poured on a silica glass substrate and the resulting film was photoreticulated in N₂ atmosphere using a UV lamp. As a result, a polymer-based magnetic nanocomposite was obtained, where the magnetic nanoparticles are dispersed in the diamagnetic matrix, as checked by SEM. Morphology, composition, and size of as-prepared nanoparticles were checked by SEM and X-ray diffraction. The magnetic properties of magnetite nanoparticles prior to and after inclusion in the polymeric matrix have been studied by means of an alternating-gradient magnetometer (T interval: 10–300 K, H_MAX: 18 kOe). FC-ZFC curves were obtained in the same temperature interval. The results show that the nanocomposites cannot be simply described as containing superparamagnetic particles undergoing an anisotropy-driven blocking and that collective magnetic interactions play a non-negligible role. Low-temperature hysteretic properties indicate that the polymeric matrix affects the effective anisotropy of magnetite nanoparticles. Dispersion of magnetite NPs in PEGDA has non-trivial consequences on their magnetic properties.     

Synthesis and Reactivity of Magnetically Diverse Au@Ni Core–Shell Nanostructures

Core–shell bimetallic Au@Ni nanoparticles, with gold cores and thin nickel shells with overall size less than 10 nm, are synthesized and stabilized in pure cubic (fcc) and hexagonal (hcp) phase. Due to their unique crystal, electronic, and geometric structure, they show interesting magnetic and chemical properties. The Au@Ni_fcc is magnetic, whereas Au@Ni_hcp is non‐magnetic. Both the bimetallic nanostructures are stable to surface oxidation until 150 °C and show excellent catalytic activity for p‐nitrophenol reduction reaction.