Iron oxide nanoparticles and VO(x)/Hexadecylamine nanotubes composite

In this work, we present the synthesis and characterization of a hybrid nanocomposite constituted by iron oxide nanoparticles and vanadium oxide/Hexadecylamine (VO(x)/Hexa) nanotubes. Transmission Electron Microscopy (TEM) images show small particles (around 20 nm) in contact with the external wall of the multiwall tubes, which consist of alternate layers of VO(x) and Hexa. By Energy Dispersive Spectroscopy (EDS), we detected iron ions within the tube walls and we have also established that the nanoparticles are composed of segregated iron oxide. The samples were studied by Electron Paramagnetic Resonances (EPR) and dc-magnetization as a function of the magnetic field. The analysis of the magnetization and EPR data confirms that a fraction of the V atoms are in the V(4+) electronic state and that the nanoparticles exhibit a superparamagnetic behavior. The percentage of V and Fe present in the nanocomposite was determined using Instrumental Neutron Activation Analysis (INAA). (C) 2008 Elsevier B.V. All rights reserved.

Formation Mechanism via a Heterocoagulation Approach of FePt Nanoparticles Using the Modified Polyol Process

Herein, we report a new approach of an FePt nanoparticle formation mechanism studying the evolution of particle size and composition during the synthesis using the modified polyol process. One of the factors limiting their application in ultra-high-density magnetic storage media is the particle-to-particle composition, which affects the A1-to-L1(0) transformation as well as their magnetic properties. There are many controversies in the literature concerning the mechanism of the FePt formation, which seems to be the key to understanding the compositional chemical distribution. Our results convincingly show that, initially, Pt nuclei are formed due to reduction of Pt(acac)(2) by the diol, followed by heterocoagulation of Fe cluster species formed from Fe(acac)(3) thermal decomposition onto the Pt nuclei. Complete reduction of heterocoagulated iron species seems to involve a CO-spillover process, in which the Pt nuclei surface acts as a heterogeneous catalyst, leading to the improvement of the single-particle composition control and allowing a much narrower compositional distribution. Our results show significant decreases in the particle-to-particle composition range, improving the A1-to-L1(0) phase transformation and, consequently, the magnetic properties when compared with other reported methods.

PEGylated polyethyleneimine-entrapped gold nanoparticles for enhanced and targeted gene delivery applications

Gene therapy, which involves the transfer of nucleic acid into target cells in patients, has become one of the most important and widely explored strategies to treat a variety of diseases, such as cancer, infectious diseases and genetic disorders. Relative to viral vectors that have high immunogenicity, toxicity and oncogenicity, non-viral vectors have gained a lot of interest in recent years. This is largely due to their ability to mimic viral vector features including the capacity to overcome extra- and intra-cellular barriers and to enhance transfection efficiency. Polyethyleneimine (PEI) has been extensively investigated as a non-viral vector. This cationic polymer, which is able to compact nucleic acid through electrostatic interactions and to transport it across the negatively charged cell membranes, has been shown to effectively transfect nucleic acid into different cell lines. Moreover, entrapment of gold nanoparticles (Au NPs) into such an amine-terminated polymer template has been shown to significantly enhance gene transfection efficiency. In this work, a novel non-viral nucleic acid vector system for enhanced and targeted nucleic acid delivery applications was developed. The system was based on the functionalization of PEI with folic acid (FA; for targeted delivery to cancer cells overexpressing FA receptors on their surface) using polyethylene glycol (PEG) as a linker molecule. This was followed by the preparation of PEI-entrapped Au NPs (Au PENPs; for enhancement of transfection efficiency). In the synthesis process, the primary amines of PEI were first partially modified with fluorescein isothiocyanate (FI) using a molar ratio of 1:7. The formed PEI-FI conjugate was then further modified with either PEG or PEGylated FA using a molar ratio of 1:1. This process was finally followed by entrapment of Au NPs into the modified polymers. The resulting conjugates and Au PENPs were characterized by several techniques, namely Nuclear Magnetic Resonance, Dynamic Light Scattering and Ultraviolet-Visible Spectroscopy, to assess their physicochemical properties. In the cell biology studies, the synthesized conjugates and their respective Au PENPs were shown to be non-toxic towards A2780 human ovarian carcinoma cells. The role of these materials as gene delivery agents was lastly evaluated. In the gene delivery studies, the A2780 cells were successfully transfected with plasmid DNA using the different vector systems. However, FA-modification and Au NPs entrapment were not determinant factors for improved transfection efficiency. In the gene silencing studies, on the other hand, the Au PENPs were shown to effectively deliver small interfering RNA, thereby reducing the expression of the B-cell lymphoma 2 protein. Based on these results, we can say that the systems synthesized in this work show potential for enhanced and targeted gene therapy applications.

In vitro study of CD133 human stem cells labeled with superparamagnetic iron oxide nanoparticles

Superparamagnetic iron oxide nanoparticles (SPIONs) are applied in stem cell labeling because of their high magnetic susceptibility as compared with ordinary paramagnetic species, their low toxicity, and their ease of magnetic manipulation. The present work is the study of CD133(+) stem cell labeling by SPIONs coupled to a specific antibody (AC133), resulting in the antigenic labeling of the CD133+ stem cell, and a method was developed for the quantification of the SPION content per cell, necessary for molecular imaging optimization. Flow cytometry analysis established the efficiency of the selection process and helped determine that the CD133 cells selected by chromatographic affinity express the transmembrane glycoprotein CD133. The presence of antibodies coupled to the SPION, expressed in the cell membrane, was observed by transmission electron microscopy. Quantification of the SPION concentration in the marked cells using the ferromagnetic resonance technique resulted in a value of 1.70 x 10 (13) mol iron (9.5 pg) or 7.0 x 10 (6) nanoparticles per cell ( the measurement was carried out in a volume of 2 mu L containing about 6.16 x 10 5 pg iron, equivalent to 4.5 x 10 (11) SPIONs). (c) 2008 Elsevier B.V. All rights reserved.

A systematic study of transfection efficiency and cytotoxicity in HeLa cells using iron oxide nanoparticles prepared with organic and inorganic bases

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Formation Mechanism via a Heterocoagulation Approach of FePt Nanoparticles Using the Modified Polyol Process

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Monodispersed spindle-type goethite nanoparticles from Fe-III solutions

A new synthetic route for producing monodispersed and single crystal acicular goethite particles with small particle size and a high axial ratio adequate for use as a high density magnetic recording media precursor is reported. It essentially consists of the hydrolysis of alkaline Fe-III suspensions in the presence of carbonate by a three-step procedure, the formation of ferrihydrite primary particles, the ferrihydrite dissolution and nucleation of goethite, and the growth of the goethite nuclei. Changing the temperature of heating during ageing achieved a separation of the two last stages. X-Ray diffraction, transmission electron microscopy, infrared spectroscopy and surface area data have been used to determine the mechanism responsible for the formation of goethite particles with controlled size and shape. The best conditions to prepare monodispersed goethite particles have been established. The results show that uniform goethite particles of (a) 60 nm length with an axial ratio of 6 and (b) 230 nm length with a high axial ratio of 10, can be obtained by using an [OH]/[Fe] molar ratio of 0.35 in the initial suspensions with carbonate or sodium hydroxide, respectively. The [OH]/[Fe] molar ratio determines the particle size and elongation by controlling the hydrolysis reaction rate, while the carbonate ions promote a constant [OH] in the solution, keeping the pH around 10 during the entire synthesis process. This procedure, associated with the appropriate temperature control, leads, under certain conditions, to highly homogeneous goethite particles with sizes smaller than those obtained using sodium hydroxide with the same [OH]/[Fe] ratio.

Synthesis and functionalization of magnetite nanoparticles with different amino-functional alkoxysilanes

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Electro-precipitation of Fe(3)O(4) nanoparticles in ethanol

The preparation of superparamagnetic magnetite (Fe(3)O(4)) nanoparticles by electro-precipitation in ethanol is proposed. Particle average size can be set from 4.4 to 9 nm with a standard deviation around 20%. Combination of wide-angle X-ray scattering (WAXS), Electron energy loss spectroscopy (EELS) and Mossbauer spectroscopy characterizations clearly identifies the particles as magnetite single-crystals (Fe(3)O(4)). (C) 2008 Elsevier B.V. All rights reserved.

Cu0.5Zn0.5Fe2O4 ferrite for application as a soft magnetic material

This work involved the synthesis and characterization of Cu0.5Zn0.5Fe2O4 ferrite powders prepared by combustion reaction for use as soft magnetic materials. The powders were characterized by nitrogen adsorption (BET), XRD, Rietveld refinement, SEM, TEM and magnetic measures. The results indicate that the combustion reaction yielded crystalline powders containing spinel ferrite as the primary phase and traces of Fe2O3 as secondary phase. The crystallite size and lattice microdeformation calculated from Rietveld refinements were 36 and 0.24 nm, respectively. The micrographic analysis revealed particles smaller than 100 nm and fine particle agglomerates. The particles were approximately spherical and their size, calculated by TEM, was 29 nm. The magnetic parameters indicated that the Cu-Zn ferrite powders presented closed hysteresis loops and soft magnetic properties. © (2012) Trans Tech Publications, Switzerland.

Sonochemical synthesis and magnetism in co-doped ZnO nanoparticles

The understanding and control of ferromagnetism in diluted magnetic semiconducting oxides (DMO) is a special challenge in solid-state physics and materials science due to its impact in magneto-optical devices and spintronics. Several studies and mechanisms have been proposed to explain intrinsic ferromagnetism in DMO compounds since the theoretical prediction of room-temperature ferromagnetism. However, genuine and intrinsic ferromagnetism in 3d-transition metal-doped n-type ZnO semiconductors is still a controversial issue. Furthermore, for DMO nanoparticles, some special physical and chemical effects may also play a role. In this contribution, structural and magnetic properties of sonochemically prepared cobalt-doped ZnO nanoparticles were investigated. A set of ZnO samples was prepared varying cobalt molar concentration and time of ultrasonic exposure. The obtained results showed that single phase samples can be obtained by the sonochemical method. However, cobalt nanoclusters can be detected depending on synthesis conditions. Magnetic measurements indicated a possible ferromagnetic response, associated to defects and cobalt substitutions at the zinc site by cobalt. However, ferromagnetism is depleted at higher magnetic fields. Also, an antiferromagnetic response is detected due to cobalt oxide cluster at high cobalt molar concentrations. © 2012 Springer Science+Business Media, LLC.

Flexible magnetic membranes based on bacterial cellulose and its evaluation as electromagnetic interference shielding material

Flexible magnetic membranes with high proportion of magnetite were successfully prepared by previous impregnation of the never dried bacterial cellulose pellicles with ferric chloride followed by reduction with sodium bisulfite and alkaline treatment for magnetite precipitation. Membranes were characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), vibrating magnetometer, field emission scanning electron microscopy (FEG-SEM) and impedance spectroscopy. Microwave properties of these membranes were investigated in the X-band (8.2 to 12.4 GHz). FEG-SEM micrographs show an effective coverage of the BC nanofibers by Fe 3O4 nanoparticles. Membranes with up to 75% in weight of particles have been prepared after 60 min of reaction. Magnetite nanoparticles in the form of aggregates well adhered to the BC fibers were observed by SEM. The average crystal sizes of the magnetic particles were in the range of 10 ± 1 to 13 ± 1 nm (estimated by XRD). The magnetic particles in the BC pellicles presented superparamagnetic behavior with a saturation magnetization in the range of 60 emu g- 1 and coercive force around 15 Oe. These magnetic pellicles also displayed high electrical permittivity and a potential application as microwave absorber materials. © 2013 Elsevier B.V.

Easily handling penicillin G acylase magnetic cross-linked enzymes aggregates: Catalytic and morphological studies

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Characterization of tetraethylene glycol passivated iron nanoparticles

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Preparation and Characterization of Chitosan Nanoparticles for Zidovudine Nasal Delivery

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)