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Uniform high-quality iron oxide thin films can be formed from the spin coating of iron oxide/hydroxide sol-gels on a silicon substrate. Thermal processing of the films at temperatures of approximately 300 degrees C results in the transformation of films into a ternary layered structure with iron oxide, Fe(2)O(3), at the surface, characterized by Mossbauer spectroscopy, and reduced, metallic iron characterized by depth profiling of the surface by X-ray photoelectron spectroscopy as a function of Ar(+) etching. Imaging of the etched surface by scanning electron microscopy reveals two distinct regions at the interface, nanoparticles that are very iron-rich separated by an unstructured region that is somewhat less iron-rich. The results demonstrate a synthetic protocol for the spontaneous formaton of a ternary layered structure from a simple one-step preparation.
ACS Appl Mater Interfaces 2009 Sep
PMID:Sol-gel-derived iron oxide thin films on silicon: surface properties and interfacial chemistry. 2035 2

Here we report the fabrication of magnetically responsive calcium carbonate microcrystals produced by coprecipitation of calcium carbonate in the presence of citrate-stabilized iron oxide nanoparticles. We demonstrate that the calcite microcrystals obtained possess superparamagnetic properties due to incorporated magnetite nanoparticles and can be manipulated by an external magnetic field. The microcrystals doped with magnetic nanoparticles were utilized as templates for the fabrication of hollow polyelectrolyte microcapsules, which retain the magnetic properties of the sacrificial cores and might be spatially manipulated using a permanent magnet, thus providing the magnetic-field-facilitated delivery and separation of materials templated on magnetically responsive calcite microcrystals.
ACS Appl Mater Interfaces 2009 Sep
PMID:Magnetically responsive calcium carbonate microcrystals. 2035 3

Epitaxial indium-tin oxide (ITO) thin films were fabricated on a yttria-stabilized zirconia (YSZ) substrate by pulsed-laser deposition using magnetite (Fe(3)O(4)) nanoparticle dispersed ITO powders as a target. Magnetoresistance of the film at a field of 1 T was 39% at 45 K, and it stayed at 3% above 225 K. The film demonstrated cooling hysteresis in the temperature dependence of direct-current magnetization. Transmission electron microscopy revealed that phase-separated Fe(3)O(4) nanocrystals with widths of approximately 40-150 nm and heights of approximately 10-25 nm precipitated and grew epitaxially on the substrate in the film. Both the Fe(3)O(4)(111) and ITO(001) planes were parallel to the YSZ(001) plane. The Fe(3)O(4)(11-2) and -(1-10) planes were parallel to the ITO(100) and -(010) planes, respectively, and the planes connected smoothly at the grain boundary. The contour map of the electron density for the Fe(3)O(4)(111) plane by the first-principles electronic structure computation was similar to that for the ITO(001) plane. The [111]-oriented Fe(3)O(4) nanocrystals played the role of spin aligner for charge carriers of the epitaxial ITO film.
ACS Appl Mater Interfaces 2009 Sep
PMID:Magnetoresistance and microstructure of magnetite nanocrystals dispersed in indium-tin oxide thin films. 2035 11

We describe the use of hydrophobic poly(aryl ether) dendrons to peripherally functionalize hydrophilic amine-containing superparamagnetic iron oxide microspheres (SPIO-NH2) in one step via imine formation. The reversible formation of imine bonds in the absence/presence of water renders dynamic control of the hydrophilicity and hydrophobicity of the microspheres (SPIO-Gn). The dynamic nature of the imine-containing dendronized microspheres (SPIO-Gn) can be "fixed" by locking the reversible 2,6-diiminopyridyl moieties with metal cations (Zn2+, Co2+, and Ni2+) to afford kinetically stable dendronized microspheres (SPIO-Gn-M). Isolation of these microspheres is facilitated by convenient magnetic separation by an externally applied magnetic field. Characterization of these novel organic-inorganic hybrid microspheres has been performed by various techniques using UV/visible absorption and Fourier transform infrared spectroscopies, transmission electron microscopy, thermogravimetric analysis, and a vibrating sample magnetometer. We have demonstrated the stability and reversible switching of hydrophilicity/hydrophobicity by contact-angle measurements. In particular, the hydrophilic SPIO-NH2 microspheres demonstrated a contact angle of 42 +/- 2 degrees when a drop of water was added to a SPIO-NH2-coated mica surface. On the other hand, the hydrophobic SPIO-Gn-M dendronized microspheres demonstrated a contact angle of 85 +/- 2 degrees , an observation that involves an increase of the contact angle of over 40 degrees . Furthermore, when a drop of water was placed on a dynamic SPIO-Gn-coated mica surface, the contact angle of the water droplet decreased in time. Comparatively, the rate of decrease of the contact angle is H2O > 1% Co(OAc)2/H2O > N,N'-dimethylformamide/H2O (1:1).
ACS Appl Mater Interfaces 2009 Sep
PMID:Reversible switching between hydrophilic and hydrophobic superparamagnetic iron oxide microspheres via one-step supramolecular dynamic dendronization: exploration of dynamic wettability. 2035 26

This study presents a microtubule that responds to a magnetic field. We made such a structure by incorporating iron oxide nanoparticles during the preparation of the microtubule. We found that the microtubule stretches its body when the magnetic field is applied and easily aligns with the direction of the applied magnetic field by rotating its body. When the magnetic field is removed, it loses its orientation and goes back to its original state by contraction. From the analysis of its magnetic response, we estimated that the magnetic microtubule had an elastic modulus of 33 MPa. Further analysis showed that the stretching and contracting of its body are due to its flexibility.
ACS Appl Mater Interfaces 2009 Jun
PMID:Flexible magnetic microtubules structured by lipids and magnetic nanoparticles. 2035 6

We have used a very large scale integration process to generate well-defined patterns of polymerized 2-hydroxyethyl methacrylate (HEMA) on patterned Si(100) surfaces. An atom transfer radical polymerization initiator covalently bonded to the patterned surface was employed for the graft polymerization of HEMA to prepare the poly(2-hydroxyethyl methacrylate) (PHEMA) brushes. After immersing wafers presenting lines of these polymers in water and cyclohexane, we observed brush- and mushroom-like regions, respectively, for the PHEMA brushes, with various pattern resolutions. The PHEMA brushes behaved as "tentacles" that captured ferritin complexes from aqueous solution through entanglement between the brushes and the ferritin proteins, whose ferritins were trapped due to the collapsing of the PHEMA. Using high-resolution scanning electron microscopy, we observed patterned ferritin iron cores on the Si surface after thermal removal of the patterned PHEMA brushes and ferritin protein sheaths.
ACS Appl Mater Interfaces 2009 Jul
PMID:Patterned poly(2-hydroxyethyl methacrylate) brushes on silicon surfaces behave as "tentacles" to capture ferritin from aqueous solution. 2035 56

We present a simple technique for magnetic-field-induced formation, assembling, and positioning of magnetic nanowires in a polymer film. Starting from a polymer/iron oxide nanoparticle casted solution that is allowed to dry along with the application of a weak magnetic field, nanocomposite films incorporating aligned nanocrystal-built nanowire arrays are obtained. The control of the dimensions of the nanowires and of their localization across the polymer matrix is achieved by varying the duration of the applied magnetic field, in combination with the evaporation dynamics. These multifunctional anisotropic free-standing nanocomposite films, which demonstrate high magnetic anisotropy, can be used in a wide field of technological applications, ranging from sensors to microfluidics and magnetic devices.
ACS Nano 2010 Apr 27
PMID:Dynamical formation of spatially localized arrays of aligned nanowires in plastic films with magnetic anisotropy. 2035 62

This paper presents the fabrication of poly(ferrocenylmethylphenylsilane) (PFMPS) patterns by step-and-flash imprint lithography for use as high-contrast etch masks in dry etch processes. PFMPS was spin-coated onto a resist template made by UV nanoimprint lithography to create a reactive ion etch resist layer with a thickness variation corresponding to the imprinted pattern. Etching back the excess of PFMPS by argon sputtering revealed the imprinted organic resist material, which was subsequently removed by oxygen plasma. PFMPS lines down to 30 nm were obtained after removal of the organic resist by oxygen plasma. Because PFMPS contains iron and silicon atoms in its main chain, it possesses a high resistance to oxygen reactive ion etching and, e.g., CHF(3)/O(2) or SF(6)/O(2) reactive ion etch processes. PFMPS patterns formed after imprinting were subsequently transferred into the underlying silicon substrate, and etch rates of 300 nm/min into Si and around 1 nm/min into the PFMPS layer were achieved, resulting in an etch contrast of approximately 300.
ACS Appl Mater Interfaces 2009 Nov
PMID:Nanoscale patterning by UV nanoimprint lithography using an organometallic resist. 2035 38

The preparation, characterization, and application in oxidation reactions of new biomimetic catalysts are reported. Brazilian Sao Simao kaolinite clay has been functionalized with [meso-tetrakis(pentafluorophenyl)porphinato]iron(III), Fe(TPFPP). To obtain the functionalized clay, the natural clay was purified by dispersion-sedimentation, expanded by insertion of dimethyl sulfoxide (DMSO), and functionalized with amino groups by substitution of DMSO with ethanolamine. These previous steps allowed clay functionalization with Fe(TPFPP), leading to a layered material with a basal spacing of 10.73 A. Clay functionalization with the porphyrin was confirmed by formation of the secondary amine, as demonstrated by FTIR bands at 3500-3700 cm(-1). UV-vis spectroscopy revealed a red shift in the Soret band of the iron porphyrin in the functionalized material as compared to the parent iron porphyrin catalyst in solution, indicating Fe(III)P --> Fe(II)P reduction. The catalytic performance of the functionalized clay was evaluated in the epoxidation of cyclooctene, with complete selectivity for the epoxide (100% epoxide yield), and ketonization of cyclohexane, cyclohexanone being the major product. The novel catalyst was also evaluated in the Baeyer-Villiger (BV) oxidation of cyclohexanone, with 85% conversion of cyclohexanone in epsilon-caprolactone, with total selectivity to epsilon-caprolactone.
ACS Appl Mater Interfaces 2009 Nov
PMID:Porphyrin-kaolinite as efficient catalyst for oxidation reactions. 2035 41

We report a facile approach to synthesizing and immobilizing zero-valent iron nanoparticles (ZVI NPs) onto polyelectrolyte (PE) multilayer-assembled electrospun polymer nanofibers for potential environmental applications. In this approach, negatively charged cellulose acetate (CA) nanofibers fabricated by electrospinning were assembled with multilayers of poly(diallyldimethylammonium chloride) (PDADMAC) and polyacrylic acid (PAA) through electrostatic layer-by-layer assembly. The formed PAA/PDADMAC multilayers onto CA nanofibers were then used as a nanoreactor to complex Fe(II) ions through the binding with the free carboxyl groups of PAA for subsequent reductive formation of ZVI NPs. Combined scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, Fourier transform infrared spectroscopy, and thermogravimetry analysis studies demonstrate that the ZVI NPs are successfully synthesized and uniformly distributed into the PE multilayers assembled onto the CA nanofibers. The produced hybrid nanofibrous mats containing ZVI NPs were found to exhibit superior capability to decolorize acid fuchsin, an organic dye in dyeing wastewater. We show that the loading capacity of ZVI NPs can be tuned by changing the number of PE layers and the cycles of binding/reduction process. Increasing the number of the binding/reduction cycles leads to a slight bigger size of the ZVI NPs, which is not beneficial for improving the reactivity of ZVI NPs. The present approach to synthesizing and immobilizing ZVI NPs onto polymer nanofibers opens a new avenue to fabricating various fiber-based composite materials with a high surface area to volume ratio for environmental, catalytic, and sensing applications.
ACS Appl Mater Interfaces 2009 Dec
PMID:Polyelectrolyte multilayer-assisted immobilization of zero-valent iron nanoparticles onto polymer nanofibers for potential environmental applications. 2035 66


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