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The patterning of biologically active materials has been accomplished by the use of imprint lithography of functional photopolymer resins to create controlled nanoscale patterns of a cross-linked photopolymer containing embedded initiator groups. Functionalized polymer brushes consisting of polystyrene and poly(N,N-dimethylacrylamide) were grown from these patterned layers by nitroxide-mediated polymerization. Chain-end functionalization of the brush layer was accomplished by nitroxide radical exchange during the polymerization. Accordingly, brush layers terminated by pyrene and biotin functional groups were obtained by exchange with the appropriate alkoxyamines. The presence of pyrene functionality at the chain ends of the brushes was confirmed by fluorescent emission measurements. Fluorescently labeled streptavidin protein was selectively attached with high selectivity to the patterned biotinylated brush layer through biotin-streptavidin interactions. The functionalized polymer grafted surfaces and nanopatterns have been successfully characterized using a fluorescence spectrophotometer, AFM, SEM, confocal microscopy, and water contact angle measurements.
ACS Nano 2008 Apr
PMID:Chain-end functionalized nanopatterned polymer brushes grown via in situ nitroxide free radical exchange. 1920 3

The synthesis and characterization of colloidal mesoporous silica (CMS) functionalized with vinyl-, benzyl-, phenyl-, cyano-, mercapto-, aminopropyl- or dihydroimidazole moieties is reported. Uniform mesoporous particles ranging in size from 40 to 150 nm are generated in a co-condensation process of tetraethylorthosilicate (TEOS) and organotriethoxysilanes (RTES) in alkaline aqueous media containing triethanolamine (TEA) in combination with cetyltrimethylammonium chloride (CTACl) serving as a structure-directing agent. The materials are obtained as colloidal suspensions featuring long-term stability after template removal by ion exchange with an ethanolic solution of ammonium nitrate or HCl. The spherical particles exhibit a wormlike pore system with defined pore sizes and high surface areas. Samples are analyzed by a number of techniques including TEM, SEM, DLS, TGA, Raman, and cross-polarized (29)Si-MAS NMR spectroscopy, as well as nitrogen sorption measurements. We demonstrate that co-condensation and grafting methods result in similar changes in the nitrogen adsorption behavior, indicating a successful internal lining of the pores with functional groups through both procedures.
ACS Nano 2008 Apr
PMID:Colloidal suspensions of functionalized mesoporous silica nanoparticles. 1920 12

This paper describes the synthesis and electrical properties of self-organized Sb-, Nb-, and Ta-doped SnO(2) thin films with adjustable doping levels. These transparent conducting oxides (TCOs) were prepared using a poly(ethylene-co-butylene)-b-poly(ethylene oxide) diblock copolymer as well as a novel polyisobutylene-b-poly(ethylene oxide) as organic templates. All samples are highly crystalline and have ordered cubic pore-solid architectures after removal of the polymer template by calcination; however, the electrical conductivity is not identical. The films are characterized by a combination of small- and wide-angle X-ray diffraction/scattering, SEM/TEM imaging, and X-ray photoelectron spectroscopy. Resistivity measurements conducted on the mesoporous frameworks show that the electrical properties strongly depend on both the degree of crystallinity and the elemental makeup. Considerable enhancements of the electrical properties result when the films are doped with antimony and treated in N(2) at elevated temperatures. Such TCO materials show electrical resistivities which are--despite the mesoporous morphology--only 1 order of magnitude higher than reported values for dense Sb-doped SnO(2) films.
ACS Nano 2009 Jun 23
PMID:Ordered mesoporous Sb-, Nb-, and Ta-doped SnO2 thin films with adjustable doping levels and high electrical conductivity. 1943 71

Herein we report on the alignment of mesoporous silica, a potential host for sub-10 nm nanostructures, by controlling its deposition within patterned substrates. In-depth characterization of the correlation lengths (length of a linear porous channel), defects of the porous network (delamination), and how the silica mesopores register to the micrometer-sized substrate pattern was achieved by means of novel focused ion beam (FIB) sectioning and in situ SEM imaging, which to our knowledge has not previously been reported for such a system. Our findings establish that, under confinement, directed deposition of the sol within channeled substrates, where the cross-sectional aspect ratio of the channels approaches unity, induces alignment of the mesopores along the length of the channels. The pore correlation length was found to extend beyond the micrometer scale, with high pore uniformity from channel to channel observed with infrequent delamination defects. Such information on pore correlation lengths and defect densities is critical for subsequent nanowire growth within the mesoporous channels, contact layout (electrode deposition etc.), and possible device architectures.
ACS Nano 2009 Aug 25
PMID:Pore directionality and correlation lengths of mesoporous silica channels aligned by physical epitaxy. 1959 14

A general method is described for the deposition of metal nanoparticles selectively either inside or outside of carbon nanotubes (CNTs). The method is based on the difference in the interface energies of organic and aqueous solutions with the CNT surface. Because of their lipophilic character, the organic solvent better wets the surface of the nanotubes compared to water and penetrates into the inner volume. The precise control of the volume of each phase allows filling the CNT with the organic phase and covering its outer surface with the aqueous one. Hence, metal nanoparticles can be put with high selectivity either inside or outside the CNT, just by choosing in which solvent the metal precursor is dissolved. SEM, TEM, and 3D-TEM investigations show that a selectivity in localization close to 75% can be reached by this technique. The nanoparticles are homogeneously dispersed and present a narrow size distribution, centered on 5 nm. In this way, one can decorate either the inner or the outer surface of open CNTs, without the need of discriminating the diameter of the opening and without any further step of functionalization than a treatment with nitric acid.
ACS Nano 2009 Aug 25
PMID:Selective deposition of metal nanoparticles inside or outside multiwalled carbon nanotubes. 1970 19

Activated carbons have been prepared from jute sticks by chemical activation using ZnCl(2) and physical activation using steam for the removal of Brilliant Green dye from aqueous solution. The activated carbons and charcoal prepared from jute sticks were characterized by evaluating the surface chemistry, structural features and surface morphology. The maximum BET surface area was obtained to be 2304 m(2)/g for chemical activated carbon (ACC) while it is 730 and 80 m(2)/g for steam activated carbon (ACS) and charcoal, respectively. The FT-IR spectra exhibited that the pyrolysis and steam activation of jute sticks resulted in the release of aliphatic and O-containing functional groups by thermal effect. However, the release of functional groups is the effect of chemical reaction in the ZnCl(2) activation process. A honeycomb-type carbon structure in ACC was formed as observed on SEM images. Although charcoal and ACC were prepared at 500 degrees C the ACC exhibited much lower Raman sensitivity due to the formation of condensed aromatic ring systems. Due to high surface area and high porous structure with abundance of functional groups, the ACC adsorbed dye molecules with much higher efficiency than those of ACS and charcoal.
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PMID:Chemical and structural evaluation of activated carbon prepared from jute sticks for Brilliant Green dye removal from aqueous solution. 1981 39

The alpha-Fe(2)O(3) with various morphologies has been successfully synthesized via an ionic liquid-assisted hydrothermal synthetic method. The samples are characterized by X-ray diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscope (FE-SEM), transmission electron microscopy, and high-resolution transmission electron microscopy. The results indicate that the as-prepared samples are alpha-Fe(2)O(3) nanoparticles, mesoporous hollow microspheres, microcubes, and porous nanorods. The effects of the ionic liquid 1-n-butyl-3-methylimidazolium chloride ([bmim][Cl]) on the formation of the alpha-Fe(2)O(3) with various morphologies have been investigated systematically. The proposed formation mechanisms have also been investigated on the basis of a series of FE-SEM studies of the products obtained at different durations. Because of the unique porous structure, the potential application in water treatment of the alpha-Fe(2)O(3) porous nanorods was investigated. The UV-vis measurements suggest that the as-synthesized pure alpha-Fe(2)O(3) with various morphologies possess different optical properties depending on the shape and size of the samples. The magnetic hysteresis measurements indicate the interesting magnetic property evolution in the as-prepared alpha-Fe(2)O(3) samples, which is attributed to the superstructure or the shape anisotropy of the samples. This method is expected to be a useful technique for controlling the diverse shapes of crystalline inorganic materials for a variety of applications, such as sensors, gas and heavy metal ion adsorbents, catalytic fields, hydrogen and Li ion storage, and controlled drug delivery, etc.
ACS Nano 2009 Nov 24
PMID:Hematite (alpha-Fe2O3) with various morphologies: ionic liquid-assisted synthesis, formation mechanism, and properties. 1987 95

Solid nanotubes comprising alpha-Fe2O3 nanoparticles were prepared from iron-storage protein ferritin. Their structure, magnetic properties, and photocatalytic activities were characterized. The initial ferritin nanotube precursors were fabricated using alternating layer-by-layer depositions of poly-L-arginine (PLA) and ferritin into a track-etched polycarbonate membrane (pore diameter, 400 nm) with subsequent dissolution of the template. The obtained uniform cylinders of (PLA/ferritin)3 (outer diameter, 410 +/- 14 nm) were calcinated at 500 degrees C under air, yielding reddish-brown iron oxide nanotubes. The one-dimensional hollow structure remained perfect, but its diameter, wall thickness, and maximum length were markedly diminished. Disappearance of the protein shell and the PLA layers were confirmed using IR and EDX spectroscopy. Subsequent SEM, TEM, and XPS measurements showed that the tubular walls comprise fine alpha-Fe2O3 nanoparticles with a 5 nm diameter. These alpha-Fe2O3 nanotubes demonstrated superparamagnetic properties with a blocking temperature of 37 K and efficient photocatalytic activity for degradation of 4-chlorophenol.
ACS Nano 2010 Mar 23
PMID:Solid nanotubes comprising alpha-Fe2O3 nanoparticles prepared from ferritin protein. 2016

Difunctional reactive polymers, telechelics, were used to reactively form multiblock copolymers in situ when melt-blended with a blend of polystyrene and polyisoprene. To quantify the ability of the copolymer to compatibilize the blends, the time evolution of the domain size upon annealing was analyzed by SEM. It was found that the most effective parameter to quantify the ability of the copolymer to inhibit droplet coalescence is K(rel)t(stable), the relative coarsening constant multiplied by the stabilization time. These results indicate that intermediate-molecular-weight telechelic pairs of both highly reactive Anhydride-PS-Anhydride/NH(2)-PI-NH(2) and slower reacting Epoxy-PS-Epoxy/COOH-PI-COOH both effectively suppress coalescence, with the optimal molecular weight being slightly above the critical molecular weight of the homopolymer, M(c). The effects of telechelic loading were also investigated, where the optimal loading concentration for this system was 0.5 wt %, as higher concentrations exhibited a plasticizing effect due to the presence of unreacted low-molecular-weight telechelics present in the blend. A determination of the interfacial coverage of the copolymer shows that a conversion of approximately 1.5-3.0% was required for 20% surface coverage at 5.0 wt % telechelic loading, indicating a large excess of telechelics in this system. At the optimal loading level of 0.5 wt %, a conversion of 15% was required for 20% surface coverage. The results of these experiments provide a clear understanding of the role of telechelic loading and molecular weight on its ability to reactively form interfacial modifiers in phase-separated polymer blends and provide guidelines for the development of similar reactive processing schemes that can use telechelic polymers to reactively compatibilize a broad range of polymer blends.
ACS Appl Mater Interfaces 2009 Oct
PMID:A novel reactive processing technique: using telechelic polymers to reactively compatibilize polymer blends. 2035 50

In this paper, we report the synthesis of a carboxyl-functionalized polypyrrole derivative, a poly(pyrrole-N-propanoic acid) (PPPA) film, by electrochemical polymerization, and the investigation of its basic properties via traditional characterization techniques such as confocal-Raman, FTIR, SEM, AFM, UV-vis, fluorescence microscopy, and contact-angle measurements. The experimental data show that the as-prepared PPPA film exhibits a hydrophilic nanoporous structure, abundant -COOH functional groups in the polymer backbone, and high fluorescent emission under laser excitation. On the basis of these unique properties, further experiments were conducted to demonstrate three potential applications of the PPPA film in chemical and biological sensors: a permeable and permselective membrane, a membrane with specific recognition sites for biomolecule immobilization, and a fluorescent conjugated polymer for amplification of fluorescence quenching. Specifically, the permeability and permselectivity of ion species through the PPPA film are detected by means of rotating-disk-electrode voltammetry; the specific recognition sites on the film surface are confirmed with protein immobilization, and the amplification of fluorescence quenching is measured by the addition of a quenching agent with fluorescence microscopy. The results are in good agreement with our expectations.
ACS Appl Mater Interfaces 2009 Jul
PMID:Functionalized polypyrrole film: synthesis, characterization, and potential applications in chemical and biological sensors. 2035 67


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