The magnetic properties of monodisperse FeO-Fe3O4 nanoparticles with different mean sizes and volume fractions of FeO synthesized via decomposition of iron oleate were correlated to their crystallographic and phase compositional features by exploiting high resolution transmission electron microscopy, X-ray diffraction, Mössbauer spectroscopy and field and zero field cooled magnetization measurements. A model describing the phase transformation from a pure Fe3O4 phase to a mixture of Fe3O4, FeO and interfacial FeO-Fe3O4 phases as the particle size increases was established. The reduced magnetic moment in FeO-Fe3O4 nanoparticles was attributed to the presence of differently oriented Fe3O4 crystalline domains in the outer layers and paramagnetic FeO phase. The exchange bias energy, dominating magnetization reversal mechanism and superparamagnetic blocking temperature in FeO-Fe3O4 nanoparticles depend strongly on the relative volume fractions of FeO and the interfacial phase.
Cu2–xTe nanocubes were used as starting seeds to access metal telluride nanocrystals by cation exchanges at room temperature. The coordination number of the entering cations was found to play an important role in dictating the reaction pathways. The exchanges with tetrahedrally coordinated cations (i.e., with coordination number 4), such as Cd2+ or Hg2+, yielded monocrystalline CdTe or HgTe nanocrystals with Cu2–xTe/CdTe or Cu2–xTe/HgTe Janus-like heterostructures as intermediates. The formation of Janus-like architectures was attributed to the high diffusion rate of the relatively small tetrahedrally coordinated cations, which could rapidly diffuse in the Cu2–xTe NCs and nucleate the CdTe (or HgTe) phase in a preferred region of the host structure. Also, with both Cd2+ and Hg2+ ions the exchange led to wurtzite CdTe and HgTe phases rather than the more stable zinc-blende ones, indicating that the anion framework of the starting Cu2–xTe particles could be more easily deformed to match the anion framework of the metastable wurtzite structures. As hexagonal HgTe had never been reported to date, this represents another case of metastable new phases that can only be accessed by cation exchange. On the other hand, the exchanges involving octahedrally coordinated ions (i.e., with coordination number 6), such as Pb2+ or Sn2+, yielded rock-salt polycrystalline PbTe or SnTe nanocrystals with Cu2–xTe@PbTe or Cu2–xTe@SnTe core@shell architectures at the early stages of the exchange process. In this case, the octahedrally coordinated ions are probably too large to diffuse easily through the Cu2–xTe structure: their limited diffusion rate restricts their initial reaction to the surface of the nanocrystals, where cation exchange is initiated unselectively, leading to core@shell architectures. Interestingly, these heterostructures were found to be metastable as they evolved to stable Janus-like architectures if annealed at 200 °C under vacuum.
Hysteresis losses in magnetic nanoparticles constitute the basis of magnetic hyperthermia for delivering a local thermal stress. Nevertheless, this therapeutic modality is only to be realised through a careful appraisal of the best possible intrinsic and extrinsic conditions to the nanoparticles for which they maximise and preserve their heating capabilities. Low frequency (100 kHz) hysteresis loops accurately probe the dynamical magnetic response of magnetic nanoparticles in a more reliable manner than calorimetry measurements, providing conclusive quantitative data under different experimental conditions. We consider here a set of iron oxide or cobalt ferrite nanocubes of different sizes, through which we experimentally and theoretically study the influence of the viscosity of the medium on the low frequency hysteresis loops of magnetic colloids, and hence their ability to produce and dissipate heat to the surroundings. We analyse the role of nanoparticle size, size distribution, chemical composition, and field intensity in making the magnetisation dynamics sensitive to viscosity. Numerical simulations using the stochastic Landau-Lifshitz-Gilbert equation model the experimental observations in excellent agreement. These results represent an important contribution towards predicting viscosity effects and hence to maximise heat dissipation from magnetic nanoparticles regardless of the environment.
Self‐assembled dandelion‐like hydroxyapatite (HAp) nanostructures were successfully synthesized via a mild template‐free hydrothermal process, using ethylenediaminetetraacetic acid (EDTA) as the surfactant. The obtained dandelion‐like HAp nanostructures were between 5 and 8 μm in diameter and were composed of radially oriented nanorods with an average diameter of about 200 nm. The X‐ray diffraction analysis and Fourier transform infrared spectroscopy were used to characterize the crystalline phase and purity of the synthesized nanostructures. The Brunauer–Emmett–Teller surface area of the dandelion‐like nanostructures was measured to be about 39 m2/g. The results of thermal analysis revealed that dandelion‐like HAp nanostructures have appropriate thermal stability up to 1200°C. Scanning electron microscopy and transmission electron microscopy analyses showed that EDTA plays an important role in obtaining the dandelion‐like morphology, because without it, only monodispersed HAp nanoparticles with an average diameter of about 125 nm were formed. The mechanism for the formation of dandelion‐like HAp nanostructures was suggested based on the radial self‐assembly of Ca‐EDTA molecular complexes.
Monodispersed single‐crystal hydroxyapatite (HAp) nanorods with nearly uniform diameters and lengths of, respectively, about 25 and 100 nm were rapidly synthesized using a template‐free and convenient microwave irradiation method. Precipitation of HAp occurred directly in a calcium‐phosphate precursor solution containing ethylenediaminetetraacetic acid (EDTA) as a capping agent and using microwave irradiation of 900 W power and 2.45 GHz frequency as the heating source. Transmission electron microscopy observations revealed that faceted surfaces and narrow‐size distribution were two interesting features of the HAp nanorods obtained. The selected area electron diffraction pattern of the nanorods obtained clearly confirmed their single crystalline nature and the growth along the basal (001) planes. Furthermore, the formation mechanism of HAp nanorods was clearly proposed, identifying the influences of EDTA and microwaves in the growth process.
CitationHighly Uniformly sized and shaped iron oxide nanoparticles with a mean size of 25 nm were synthesized via decomposition of ironoleate. High resolution transmission electron microscopy and Mössbauer spectroscopy investigations revealed that the particles are spheres primarily composed of Fe 3 O 4 with a small fraction of FeO. From Mössbauer and static magnetization measurements, it was deduced that the particles are superparamagnetic at room temperature. The hydrophobic particles were successfully transferred into water via PEGylation using nitrodopamine as an anchoring group. IR spectroscopy and thermogravimetric analysis showed the success and efficiency of the phase transfer reaction. After the PEGylation, the particles retained monodisperse and their magnetic core remained intact as proven by photon cross-correlation spectrocopy, ac susceptibility, and transmission electron microscopy. The particle aqueous suspensions revealed an excellent water stability over a month of monitoring and also against temperature up to 40 • C. The particles exhibited a moderate cytotoxic effect on in vitro cultured bone marrow-derived macrophages and no release of inflammatory or anti-inflammatory cytokines. The PEGylated particles were functionalized with Herceptin antibodies via a conjugation chemistry, their response to a rotating magnetic field was studied using a fluxgate-based setup and was compared with the one recorded for hydrophobic and PEGylated particles. The particle phase lag rose after labeling with Herceptin, indicating the successful conjugation of Herceptin antibodies to the particles.
A detection scheme based on magnetic nanoparticle (MNP) dynamics in a rotating magnetic field for a quantitative and easy-to-perform detection of proteins is illustrated. For the measurements, a fluxgate-based setup was applied, which measures the MNP dynamics, while a rotating magnetic field is generated. The MNPs exhibit single iron oxide cores of 25 nm and 40 nm diameter, respectively, as well as a protein G functionalized shell. IgG antibodies were utilized as binding target molecules for the physical proof-of-concept. The measurement results were fitted with a theoretical model describing the magnetization dynamics in a rotating magnetic field. The established detection scheme allows quantitative determination of proteins even at a concentration lower than of the particles. The observed differences between the two MNP types are discussed on the basis of logistic functions.
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