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Synthesis and characterization of NiFe{sub 2}O{sub 4}–Pd magnetically recyclable catalyst for hydrogenation reaction

Graphical abstract: Display Omitted Highlights: ► Novel superparamagnetic NiFe{sub 2}O{sub 4}–Pd magnetically recyclable catalyst was fabricated through co-precipitation. ► It could be reused several times without significant loss in catalytic activity for hydrogenation reaction. ► No further modification of the NiFe{sub 2}O{sub 4}–Pd magnetically recyclable catalyst is necessary for utilization as catalyst. -- Abstract: Herein we report the fabrication and characterization magnetically recyclable catalysts of NiFe{sub 2}O{sub 4}–Pd nanocomposite as highly effective catalysts for reduction reactions in liquid phase. The reduction Pd{sup 2+} was accomplished with polyethylene glycol 400 (PEG-400) instead of sodium borohydride (NaBH{sub 4}) and NiFe{sub 2}O{sub 4} nanoparticles was prepared by sonochemically using FeCI{sub 3}·6H{sub 2}O and NiCl{sub 2}. The chemical characterization of the product was done with X-ray diffractometry, Infrared spectroscopy, transmission electron microscopy, UV–Vis spectroscopy, thermal gravimetry and inductively coupled plasma. Thus formed NiFe{sub 2}O{sub 4}–Pd MRCs showed a very high activity in reduction reactions of 4-nitro aniline and 1,3-dinitrobenzene in liquid phase. It was found out that the catalytic activity of NiFe{sub 2}O{sub 4}–Pd MRCs on the reduction of 4-nitro aniline and 1,3-dinitrobenzene in liquid phase are between 99–93% and 98–93%, respectively. Magnetic character of this system allowed recovery and multiple use without significant loss of its catalytic activity. It is found that NiFe{sub 2}O{sub 4}–Pd MRCs showed very efficient catalytic activity and multiple usability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Simple solvothermal synthesis of hydrophobic magnetic monodispersed Fe{sub 3}O{sub 4} nanoparticles

Graphical abstract: A facile method to produce monodispersed magnetite nanoparticles is based on the solvothermal reaction of iron acetylacetonate (Fe(acac)3) decomposition. The sizes ranged from 7 to 12 nm, which could be controlled by adjusting the volume ratio of oleylamine to n-hexane. Display Omitted Highlights: ► The solvethermal reaction of Fe(acac){sub 3} decomposition was carried out at mild temperature in the presence of oleylamine and n-hexane. ► The size of nanocrystals is controlled by adjusting the volume ratio of oleylamine to n-hexane. ► The low-boiling-point solvent n-hexane offered autogenous pressure parameter after gasified in the reaction temperature. ► The as prepared hydrophobic monodisperse Fe{sub 3}O{sub 4} NPs can be used to prepare the magnetic micelles for future biomedical applications. -- Abstract: A new solvothermal method is proposed for the preparation of Fe{sub 3}O{sub 4} nanoparticles (NPs) from iron acetylacetonate in the presence of oleylamine and n-hexane. The products are characterized by X-ray powder diffraction, infrared (IR) spectroscopy, transmission electron microscopy, thermogravimetry/differential thermogravimetry (TG/DTG) analysis, and vibrating sample magnetometery. The new procedure yields superparamagnetic monodispersed Fe{sub 3}O{sub 4} particles with sizes ranging from 7 nm to 12 nm. The nanocrystal sizes are controlled by adjusting the volume ratio of oleylamine to n-hexane. IR and TG/DTG analyses indicate that the oleylamine molecules, as stabilizers, are adsorbed on the surface of Fe{sub 3}O{sub 4} NPs as bilayer adsorption models. The surface adsorption quantities of oleylamine on 7.5 and 10.4 nm-diameter Fe{sub 3}O{sub 4} NPs are 18% and 11%, respectively. The hydrophobic surface of the obtained nanocrystals is passivated by adsorbed organic solvent molecules. These molecules provide stability against agglomeration, enable solubility in nonpolar solvents, and allow the formation of magnetic polymer micelles.

36 MATERIALS SCIENCE↗

Facile synthesis of QD-anchored composite particles with magnetite cluster cores ({sup n}Fe{sub 3}O{sub 4}@SiO{sub 2}@QDs)

Highlights: ► Triple layered Fe{sub 3}O{sub 4}/SiO{sub 2}/QDs were designed as fluorescent magnetic nanocomposites. ► Magnetite cluster-embedded silica exhibited strong and controllable magnetism. ► Effective conjugation between QDs and magnetic silica occurred at pH3. - Abstract: Magnetism-controlled fluorescent composite particles ({sup n}Fe{sub 3}O{sub 4}@SiO{sub 2}@QDs) were prepared as QD-anchored silica nanoparticles with magnetite cluster cores. First, citrate-capped magnetites (C-Fe{sub 3}O{sub 4}) were prepared by the co-precipitation method and subsequently complexed with 3-aminopropyl-trimethoxysilane (APTMS) at room temperature, consequently leading to the formation of magnetite clusters (A-{sup n}Fe{sub 3}O{sub 4}) with alkoxy terminated interfaces. The sol–gel reaction between A-{sup n}Fe{sub 3}O{sub 4} and tetraethoxysilane (TEOS) produced the core-shell {sup n}Fe{sub 3}O{sub 4}@SiO{sub 2}. The resulting core-shell particles exhibited superparamagnetic properties and controllable magnetism simply by adjusting the thickness of nonmagnetic silica layer. After then, amine-terminated {sup n}Fe{sub 3}O{sub 4}@SiO{sub 2} (NH{sub 2}–{sup n}Fe{sub 3}O{sub 4}@SiO{sub 2}) was conjugated with carboxy quantum dots (QDs) using an EDC coupling agent. The QD conjugation with NH{sub 2}–{sup n}Fe{sub 3}O{sub 4}@SiO{sub 2} of lower pH exhibited the higher photoluminescence (PL) intensity, and the resulting composite particles ({sup n}Fe{sub 3}O{sub 4}@SiO{sub 2}@QDs) can be a useful biomedical agent. This chemical strategy can be further applied to prepare the core-shell magnetic nanostructure with various oxide layers for specific applications.

36 MATERIALS SCIENCE↗

One-step room temperature synthesis of very small γ-Fe{sub 2}O{sub 3} nanoparticles

Graphical abstract: - Highlights: • One-step synthesis of 3 nm maghemite nanoparticles is reported. • Maghemite nanoparticles can be synthesized from a ferric solution. • γ-Fe{sub 2}O{sub 3} NPs can be obtained if the precursor has Fe(III) in tetrahedral interstices. • HR-TEM, Mössbauer, XAFS and magnetometry analysis proved the maghemite existence - Abstract: Very small maghemite nanoparticles (∼3 nm) are obtained through a one-step synthesis at room temperature. The fast neutralization reaction of a ferric solution in a basic medium produces an intermediate phase, presumably two-line ferrihydrite, which in oxidizing conditions is transformed to maghemite nanoparticles. The synthesis of maghemite, as final product of the reaction, was characterized by High-Resolution Transmission Electron Microscopy (HR-TEM), X-ray Absorption Fine Structure (XAFS), Mössbauer spectroscopy, and magnetometry. The XAFS technique allowed the analysis of the crystallographic variations into maghemite nanoparticles as a result of modification in its surface/volume ratio. Mössbauer spectroscopy at low temperature (4.2 K) confirms the presence of Fe(III) in tetrahedral and octahedral interstices, in the stoichiometry corresponding to maghemite. The specific magnetization, M vs H (3 K and 300 K, up to 7 T) and temperature dependence of the magnetization (50 Oe by ZFC mode, 2 K ≤ T ≤ 300 K) indicate that maghemite nanoparticles of 3 nm are in superparamagnetic state with a blocking temperature close to 36 K.

36 MATERIALS SCIENCE↗

A novel solvethermal method for the preparation of magnetic monodisperse Fe{sub 3}O{sub 4} nanoparticles II: High-surface-activity ferrihydrite used as precursor

Graphical abstract: The magnetic monodisperse Fe{sub 3}O{sub 4} nanoparticles (NPs) were prepared by novel solvethemal method at moderate temperature using high surface active ferrihydrit and iron powder as precursors in orgnic solvent. - Highlights: • Facile synthesis of organic ligands-coated monodisperse Fe{sub 3}O{sub 4} nanoparticles at low temperature. • Low-cost high surface active ferrihydrit and reductive iron powder were used as precursors. • N{sub 2}-free reaction environment. • Organic ligands act as reductive. - Abstract: Magnetic monodisperse Fe{sub 3}O{sub 4} nanoparticles (NPs) were prepared from ferrihydrite and iron powder by a novel solvethermal method at moderate temperatures in aqueous and organic solvent media. The effects of temperature and solvent medium on the phase and particle size of Fe{sub 3}O{sub 4} NPs were investigated. The products were characterized by X-ray powder diffraction, infrared spectroscopy, differential scanning calorimetry–thermogravimetric analysis, transmission electron microscopy, and vibrating sample magnetometry. At 120 °C in the organic medium, uniform organic-ligand-coated superparamagnetic Fe{sub 3}O{sub 4} NPs were produced; the particle size increased with the temperature, and the calculated mean particle size was 8.9 nm. At 180 °C in the aqueous medium, pure-phase Fe{sub 3}O{sub 4} was obtained. Thus, the organic solvent did not only serve as a solvent but also participated in the reaction. Fe{sub 3}O{sub 4} production in the aqueous and organic solvent media had different mechanisms.

36 MATERIALS SCIENCE↗

Magnetic properties of nanocrystalline ε-Fe{sub 3}N and Co{sub 4}N phases synthesized by newer precursor route

Graphical abstract: Nanocrystalline ε-Fe{sub 3}N and Co{sub 4}N nitride phases are synthesized first time by newer chemical routes. The ε-Fe{sub 3}N phase crystallizes in hexagonal structure with unit cell parameters, a = 4.76 Å and c = 4.41 Å. The Co{sub 4}N phase crystallizes in face centred cubic (fcc) structure with unit cell parameters, a = 3.55 Å. The estimated crystallite size for ε-Fe{sub 3}N and Co{sub 4}N phases are 29 nm and 22 nm, respectively. The values of saturation magnetization for ε-Fe{sub 3}N and Co{sub 4}N phases are found to be 28.1 emu/g and 123.6 emu/g respectively. The reduction of magnetic moments in ultrafine materials compared to bulk materials has been explained by fine particle size and surface effects. We have synthesized the high moment ε-Fe{sub 3}N and Co{sub 4}N nitride with reduced coercivity which may find applications as soft magnetic materials. - Highlights: • Nanocrystalline ε-Fe{sub 3}N and Co{sub 4}N nitride phases are synthesized. • The ε-Fe{sub 3}N and Co{sub 4}N crystallizes in hexagonal and fcc structure respectively. • The observed magnetic parameters indicate soft magnetic properties. • The magnetic properties have been explained on the basis of fine particle magnetism. - Abstract: Nanocrystalline ε-Fe{sub 3}N and Co{sub 4}N nitride phases are synthesized first time by using tris(1,2-diaminoethane)iron(II) chloride and tris(1,2-diaminoethane)cobalt(III) chloride precursors, respectively. To prepare ε-Fe{sub 3}N and Co{sub 4}N nitride phases, the synthesized precursors were mixed with urea in 1:12 ratio and heat treated at various temperatures in the range of 450–900 °C under the ultrapure nitrogen gas atmosphere. The precursors are confirmed by FT-IR study. The ε-Fe{sub 3}N phase crystallizes in hexagonal structure with unit cell parameters, a = 4.76 Å and c = 4.41 Å. The Co{sub 4}N phase crystallizes in face centred cubic (fcc) structure with unit cell parameters, a = 3.55 Å. The estimated crystallite size for ε-Fe{sub 3}N and Co{sub 4}N phases are 29 nm and 22 nm, respectively. The scanning electron microscopy (SEM) studies confirm the nanocrystalline nature of the materials. The values of saturation magnetization for ε-Fe{sub 3}N and Co{sub 4}N phases are found to be 28.1 emu/g and 123.6 emu/g, respectively. The reduction of magnetic moments in ultrafine materials compared to bulk materials have been explained by spin pairing effect, lattice expansion, superparamagnetic behaviour and canted spin structures at the surface of the particles.

36 MATERIALS SCIENCE↗

Synthesis of Fe/SiO{sub 2} and iron oxides/SiO{sub 2} nanocomposites by long-term ball milling

Graphical abstract: - Highlights: • Iron–iron oxides/silica composites are synthesized by long term dry ball-milling. • Bcc iron and α-quartz powders are used as precursors. • Surface effects enhance coercivity in iron/silica nanocomposites. • In spite of their small size, about 10 nm, iron particles are ferromagnetic. • Ferro and superparamagnetic particles are found in maghemite/silica composites. - Abstract: Iron oxide/SiO{sub 2} nanocomposites are synthesized by dry ball-milling a mixture of bcc Fe and α-quartz powders for prolonged times. A sequence of nanocomposites is obtained, with small magnetic particles dispersed in a non magnetic, amorphous matrix. The powders are characterized by X-ray diffraction and transmission electron microscopy. The magnetic hysteresis properties are investigated in the range 50–300 K. After 120 h milling, deformed, non-spherical, α-Fe nanocrystallites of about 10 nm in size and very few small (<10 nm) maghemite particles are found. At room temperature, iron particles are ferromagnetic and a large effective magnetic anisotropy is estimated, which is mainly attributed to surface effects. Between 160 and 200 h milling, maghemite nanoparticles are observed while after 220 h grinding, hematite phase appears; after 340 h milling, the sample consists of ferromagnetic hematite particles with a broad size distribution (5–50 nm) embedded in an amorphous matrix.

36 MATERIALS SCIENCE↗

A facile gel-combustion route for fine particle synthesis of spinel ferrichromite: X-ray and Mössbauer study on effect of Mg and Ni content

Highlights: • A novel and facile synthesis route. • Transformation of system from random to inverse spinel. • Appearance of superparamagnetism phase. - Abstract: A novel nitrate–citrate gel combustion route was used to prepare fine particle of a series Mg{sub 1−x}Ni{sub x}FeCrO{sub 4} (0.0 ≤ x ≤ 1.0) and its structural properties were investigated. The in situ oxidizing environment provided by the nitrate ions in the gel increases the rate of oxidation and lowers the decomposition temperature of component. All the samples after sintering were characterized at room temperature by X-ray diffraction (XRD) method and Mössbauer spectroscopy techniques. The X-ray and Mössbauer studies confirmed the single phase cubic spinel structure with all Fe ions in 3+ charge state. XRD and Mössbauer studies revealed that the samples of x = 0.0, and 0.2 are random spinel and show rather broad lines, while x = 0.4–1.0 are inverse spinel.

36 MATERIALS SCIENCE↗

Hyperfine and magnetic properties of a Y{sub x}La{sub 1−x}FeO{sub 3} series (0 ≤ x ≤ 1)

Highlights: • Y{sub x}La{sub 1−x}FeO{sub 3} (0 ≤ x ≤ 1) was synthesized by mechanochemistry. • Two magnetic contributions were identified in the series. • A paramagnetic state is associated with a fraction of the smallest particles. • A ferromagnetic state is attributed to the larger particles. • Annealing of samples favored the formation of Y{sub 3}Fe{sub 5}O{sub 12} impurities. - Abstract: A series of orthoferrites Y{sub x}La{sub 1−x}FeO{sub 3} in the entire range of composition was synthesized at room temperature by mechanochemical activation of oxide mixtures. Phase composition, structure and microstructure of the obtained powder materials were characterized by X-ray diffraction and field-emission scanning electron microscopy. Hyperfine interactions and magnetic properties were determined by Mössbauer spectroscopy, SQUID and vibrating sample magnetometry. Two magnetic contributions could be identified in the series of materials: a paramagnetic state, associated with a fraction of the smallest particles and a ferromagnetic state, attributed to the larger particles. The results showed that the relative proportion of both contributions is very dependent on x, the Y content of samples. From M vs T measurements, it was possible to estimate the blocking temperature distribution for the end members of the series. Annealing of samples produced the elimination of the superparamagnetic behavior and the formation of Y{sub 3}Fe{sub 5}O{sub 12} impurities.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

The formation and structure of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 6.4}: XRD Rietveld, Mössabuer and XPS analyses

Highlights: • The formation of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} is investigated. • Pre-milling the reactants substantially lowers the formation temperature. • The core and surface structures were studied. • XRD and {sup 57}Fe Mössbauer spectroscopic analyses indicate the δ-value to be 0.60. • XPS shows a complex surface structure for the mechanosynthesized Sr{sub 3}Fe{sub 2}O{sub 7−δ} nanoparticles. - Abstract: The influence of ball milling and subsequent sintering of a 3:1 molar mixture of SrCO{sub 3} and α-Fe{sub 2}O{sub 3} on the formation of Sr{sub 3}Fe{sub 2}O{sub 7−δ} double perovskite is investigated with different analytical techniques. Milling the mixture for 110 h leads to the formation of SrCO{sub 3}-α-Fe{sub 2}O{sub 3} nanocomposites and the structural deformation of α-Fe{sub 2}O{sub 3} via the incorporation of Sr{sup 2+} ions. Subsequent sintering of the pre-milled reactants’ mixture has led to the partial formation of an SrFeO{sub 3} perovskite-related phase in the temperature range 400–600 °C. This was followed by the progressive development of an Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase that continued to increase with increasing sintering temperature until a single-phased nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase was attained at 950 °C (12 h). This temperature is ∼350 °C lower than the temperature at which the material is prepared conventionally using the ceramic method. The evolution of different structural phases during the reaction process is discussed. Rietveld refinement of the X-ray diffraction data shows a value of 0.60 for the oxygen deficiency δ, in consistency with the Fe{sup 3+}/Fe{sup 4+} ratio derived from the {sup 57}Fe Mössbauer data recorded at both 300 K and 78 K. The Mössbauer data suggests that the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles are superparamagnetic with blocking temperatures below 78 K. The surfaces of the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles were shown to have a complex structure and composition relative to those of their cores with traces of SrCO{sub 3}, SrO and SrFeO{sub 3−δ} being detected.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Synthesis, characterization and magnetic property of maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles and their protective coating with pepsin for bio-functionalization

Highlights: • Maghemite nanoparticles were prepared by a modified co-precipitation method. • Nanoparticles were then successfully coated with pepsin for bio-functionlization. • XRD and Mössbauer spectra confirmed the maghemite phase of the nanoparticles. • Magnetic data were analysed to evaluate particle size, anisotropy etc. - Abstract: Maghemite nanoparticles (γ-Fe{sub 2}O{sub 3}) are prepared by co-precipitation method. To obtain bio-functionalized magnetic nanoparticles for magnetically controlled drug delivery, the prepared nanoparticles are successfully coated with pepsin, a bio-compatible polymer and digestive enzyme. Crystallographic phase of the nanoparticles is confirmed by X-ray diffractograms (XRD), high resolution transmission electron microscopy (HRTEM) and {sup 57}Fe Mössbauer spectrometry. The average size of nanoparticles/nanocrystallites is estimated from the (3 1 1) peak of the XRD pattern using Debye–Scherrer formula. Results of HRTEM of coated and bare samples are in good agreement with those extracted from the XRD analysis. The dynamic magnetic properties are observed and different quantities viz., coercive field, magnetization, remanence, hysteresis losses etc., are estimated, which confirmed the presence of superparamagnetic relaxation of nanoparticles. Mössbauer spectra of the samples recorded at both 300 and 77 K, confirmed that the majority of particles are maghemite together with a very small fraction of magnetite nanoparticles.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Structural, magnetic, dielectric and magneto-dielectric properties of (BaTiO3)0.70(Li0.3Zn0.4Fe2.3O4)0.30

Highlights: Microcrystals of BaTiO{sub 3} is incorporated in Li{sub 0.3}Zn{sub 0.4}Fe{sub 2.3}O{sub 4} using sol-gel method. Crystallographic phase and morphology of the composite is investigated. Magnetic ordering originates from the ferrimagnetic matrix of the composite. The dielectric behaviour is originated from the BaTiO{sub 3} particles in the composite. The composite shows strong magneto-electric property, useful for application. - Abstract: Structural, magnetic, dielectric and magneto-dielectric properties of (BaTiO{sub 3}){sub 0.70}(Li{sub 0.3}Zn{sub 0.4}Fe{sub 2.3}O{sub 4}){sub 0.30} [BTO-LZFO] composite are studied. To prepare the composite, microcrystals of BaTiO{sub 3} [BTO] prepared in solid-state reaction are taken along with the precursors of Li{sub 0.3}Zn{sub 0.4}Fe{sub 2.3}O{sub 4} [LZFO], prepared in sol-gel route. X-ray diffraction (XRD) study confirms the phase purity of the composite sample. High-resolution transmission electron microscopy also confirms the formation of the composite state. Analysis of magnetic data confirms the ferrimagnetic nature of the sample along with a fraction of superparamagnetic particles. The ferrimagnetism is explained by Néels’ two-sublattice model. The dielectric spectrum of the sample follows the Cole-Cole relaxation. Interestingly, the ferroelectric and dielectric behaviours of BTO are retained in the composite state of BTO-LZFO, though the magnetization is enhanced drastically. This enhanced magnetic property along with the ferroelectricity and strong magneto-dielectric coupling in the composite state confirms that BTO-LZFO can be used as a multiferroic material in different electronic devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Size selected synthesis of CoFe{sub 2}O{sub 4} nanoparticles prepared in a chitosan matrix

In this paper we report the synthesis and magnetic properties of CoFe{sub 2}O{sub 4} nanoparticles. The nanoparticles with sizes ranging from 6 to 20 nm were prepared in a chitosan matrix. Size selection was achieved by introducing a nonionic surfactant Tween-X, where X={l_brace}20, 60, 80, and 85{r_brace}. Aqueous dispersions of Tween-X show micelles with increasing hydrodynamic sizes as X increases. Moessbauer spectroscopy measurements at 300 K show superparamagnetic behavior for the small particles, changing gradually to a blocked magnetic regime as the particle size increases. Magnetization measurements at 300 K show increasing values for the ratio M{sub r}/M{sub Hmax} and coercive fields (H{sub c}).

36 MATERIALS SCIENCE↗

Magnetoresistance and transport properties of CoFeB/MgO granular systems

Magnetoresistance and transport properties of ultrathin multilayers of CoFeB/MgO prepared by rf and dc magnetron sputtering were studied in the temperature range between 15 and 330 K. Due to the magnetic softness of CoFeB, this system offers a potentially high magnetoresistance at comparably low magnetic fields. At fixed MgO thickness of 0.7 nm, it undergoes a crossover from a granular to a multilayered structure with increasing thickness of CoFeB and metallic conduction is reached at around 0.8 nm. In the granular state, a ferromagnetic to superparamagnetic phase transition was observed at 130 K. Different charge transport phenomena were identified at different temperatures. A sharp increase in the magnetoresistance at low temperature can be attributed to higher order tunneling processes. By proper annealing procedures, an enhanced magnetoresistance of around 6% at room temperature and 14% at low temperature as well as an increase in the resistivity have been achieved.

36 MATERIALS SCIENCE↗

Preparation and Properties of FeCo Nanoparticles

Fe-Co nanoparticles were prepared from the binary Fe-Co oxalate. The formation of FeCo metallic phase begun at 290 deg. C as determined from the X-ray diffraction patterns recorded during heating of the oxalate sample in hydrogen atmosphere. The reduction finished at 500 deg. C by formation of bcc FeCo phase with a mean particle size of about 50 nm. Analysis of the Moessbauer spectra shows that the ferromagnetic FeCo phase is represented by two sextets corresponding to interiors and surfaces of the nanoparticles. In addition, a weak paramagnetic component, represented by the doublet, was observed which was ascribed to fine particles in a superparamagnetic state. TEM images have shown conglomerates of particles with the composition of about 50 at. % Fe and 50 at. % Co.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Single particle detection: Phase control in submicron Hall sensors

We present a phase-sensitive ac-dc Hall magnetometry method which allows a clear and reliable separation of real and parasitic magnetic signals of a very small magnitude. High-sensitivity semiconductor-based Hall crosses are generally accepted as a preferential solution for non-invasive detection of superparamagnetic nanobeads used in molecular biology, nanomedicine, and nanochemistry. However, detection of such small beads is often hindered by inductive pick-up and other spurious signals. The present work demonstrates an unambiguous experimental route for detection of small magnetic moments and provides a simple theoretical background for it. The reliability of the method has been tested for a variety of InSb Hall sensors in the range 600 nm-5 {mu}m. Complete characterization of empty devices, involving Hall coefficients and noise measurements, has been performed and detection of a single FePt bead with diameter of 140 nm and magnetic moment of {mu}{approx_equal}10{sup 8} {mu}{sub B} has been achieved with a 600 nm-wide sensor.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Origin of ferromagnetism in self-assembled Ga{sub 1-x}Mn{sub x}As quantum dots grown on Si

Self-assembled Ga{sub 1-x}Mn{sub x}As magnetic semiconductor quantum dots have been grown on Si (001) substrates using droplet epitaxy by molecular-beam epitaxy. Structural characterization reveals that these dots possess a zinc-blende lattice. The Ga{sub 1-x}Mn{sub x}As quantum dots with 8% Mn content are ferromagnetically soft and slightly anisotropic at low temperature, and show the superparamagnetic behavior with a blocking temperature of 20 K in the in-plane direction. Moreover, the results of x-ray absorption near edge structure provide direct evidences for the substitutional Mn{sup 2+} ion with a half-filled d{sup 5} configuration for the Ga site, suggesting the hole-mediated ferromagnetism in zero-dimensional Ga{sub 1-x}Mn{sub x}As quantum dots.

36 MATERIALS SCIENCE↗

Synthesis, Characterization, and Preliminary Investigation of Cell Interaction of Magnetic Nanoparticles with Catechol-Containing Shells

Superparamagnetic iron oxide cores were synthesized by co-precipitation of Fe(II) and Fe(III) salts and subsequently stabilized by coating with different catechols (levodopa, dopamine, hydrocaffeic acid, dopamine-containing carboxymethyl dextran) known to act as high-affinity, bidentate ligands for Fe(III). The prepared stable magnetic fluids were characterized with regard to their chemical composition (content of iron and shell material, Fe(II)/Fe(III) ratio) and their physical properties (size, surface charge, magnetic parameters). The nanoparticles showed no or only slight cytotoxic effects within 1 and 4 days of incubation with 3T3 fibroblast cells. Preliminary experiments were performed to study the interaction of the prepared nanoparticles with human MCF-7 breast cancer cells and leukocytes. An intense interaction of the MCF-7 cells with these particles was found whereas the leukocytes showed a lower tendency of interaction. Based on these finding, the novel magnetic nanoparticles possess the potential for use in depletion of tumor cells from peripheral blood.

77 NANOSCIENCE AND NANOTECHNOLOGY↗