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Nuclear magnetic resonance was used to probe the distribution of water and ionic species in a microstructured poly(methyl methacrylate) (PMMA) polymer optical fiber (MPOF), with a plan to assess the suitability of these fibers for aqueous chemosensing. The NMR spectra and the measurements of proton spin relaxation in hydrated fibers demonstrated the presence of two distinct pools of water: water residing in the microstructure channels and the hydration water residing in the polymer matrix of the fiber. No facile chemical exchange between these two pools was present. The NMR peaks of the two pools of water were separated by 1.53 ppm. Relaxation measurements of the fiber samples doped with aqueous copper sulfate showed that charged ions freely entered the microstructure channels but were completely excluded from the polymer matrix of the fiber. Measurements of the apparent diffusion coefficient of water along the axial direction of the fiber showed that water molecules moved unimpeded along the channels. This is the first reported magnetic-resonance study of microstructured optical fibers. The findings suggest that microstructured PMMA fibers are compatible with ionic aqueous solutions and could provide a robust and durable platform for chemical-sensing applications.
ACS Appl Mater Interfaces 2009 Jan
PMID:Magnetic-resonance evaluation of the suitability of microstructured polymer optical fibers as sensors for ionic aqueous solutions. 2035 72

The first peripheral postfunctionalization of a hyperbranched polyimide by nonlinear optic chromophores (DR1 derivative) was achieved using two different routes. The first one consists in the esterification of the terminal carboxylic acid groups, whereas the second is based on copper-catalyzed Huisgen reaction of the terminal propargylic ester groups. The resulting polymers display good solubility in classical organic solvents and good filmability because thick films can be prepared (up to 2.7 mum). The second-order nonlinear optical properties were measured by SHG at 1064 nm and we show that these hyperbranched polymers exhibit good poling efficiency and good thermal stability since the electro-optic activity remains stable up to 130 degrees C. These results illustrate the potential of hyperbranched polymers to host second-order nonlinear optical chromophores to replace dendrimers or classical linear polymers generally used in this area.
ACS Appl Mater Interfaces 2009 Aug
PMID:Synthesis and nonlinear optical properties of a peripherally functionalized hyperbranched polymer by DR1 chromophores. 2035 97

Seeding polymer substrates for the attachment and growth of metallic contacts is an important problem in modern microcircuit fabrication. A new method to effect such polymer metallization is described in which the polymer is first treated with vapor of zirconium or titanium tetra-tert-butoxide and then thermalyzed to give several monolayers of zirconium or titanium oxides that are attached to the polymer surfaces. The thickness of this layer can be controlled by the vapor exposure time. The thin oxide layers withstand removal by strenuous flexing of the polymers, and they absorb copper sulfate from an aqueous solution. Upon simple treatment with dialkylaminoborane or sodium borohydride, the polymer is metallized with copper. The tetra-tert-butoxides can be deposited through a mask, and patterned metallization of the polymers is easily accomplished.
ACS Appl Mater Interfaces 2009 Oct
PMID:A nanoscale metal alkoxide/oxide adhesion layer enables spatially controlled metallization of polymer surfaces. 2035 44

The transport of a Newtonian liquid through a smooth pipe or tube is dominated by the frictional drag on the liquid against the walls. The resistance to flow against a solid can, however, be reduced by introducing a layer of gas at or near the boundary between the solid and liquid. This can occur by the vaporization of liquid at a surface at a temperature above the Leidenfrost point, by a cushion of air (e.g. below a hovercraft), or by producing bubbles at the interface. These methods require a continuous energy input, but a more recent discovery is the possibility of using a superhydrophobic surface. Most reported research uses small sections of lithographically patterned surfaces and rarely considers pressure differences or varying flow rates. In this work we present a method for creating a uniform superhydrophobic nanoribbon layer on the inside of round copper tubes of millimetric internal radius. Two types of experiments are described, with the first involving a simultaneous comparison of four tubes with different surface finishes (as received, as received with hydrophobic coating, nanoribbon, and nanoribbon with a hydrophobic coating) under constant flow rate conditions using water and water-glycerol mixtures. The results show that the superhydrophobic nanoribbon with a hydrophobic coating surface finish allows greater flow at low pressure differences but that the effect disappears as the pressure at the inlet of the tube is increased. The second experiment is a simple visual demonstration of the low-pressure behavior using two nominally identical tubes in terms of length and cross-section, but with one tube possessing a superhydrophobic internal surface finish. In this experiment a reservoir is allowed to feed the two tubes with open ends via a T-piece and it is observed that, once flow commences, it preferentially occurs down the superhydrophobic tube.
ACS Appl Mater Interfaces 2009 Jun
PMID:Superhydrophobic copper tubes with possible flow enhancement and drag reduction. 2035 28

Halloysite clay nanotubes were investigated as a tubular container for the corrosion inhibitor benzotriazole. Halloysite is a naturally occurring cylindrical clay mineral with an internal diameter in the nanometer range and a length up to several micrometers, yielding a high-aspect-ratio hollow tube structure. Halloysite may be used as an additive in paints to produce a functional composite coating material. A maximum benzotriazole loading of 5% by weight was achieved for clay tubes of 50 nm external diameters and lumen of 15 nm. Variable release rates of the corrosion inhibitor were possible in a range between 5 and 100 h, as was demonstrated by formation of stoppers at tube openings. The anticorrosive performance of the sol-gel coating and paint loaded with 2-5% of halloysite-entrapped benzotriazole was tested on copper and on 2024-aluminum alloy by direct exposure of the metal plates to corrosive media. Kinetics of the corrosion spot formation at the coating defects was analyzed by the scanning vibrating electrode technique, and an essential damping of corrosion development was demonstrated for halloysite-loaded samples.
ACS Appl Mater Interfaces 2009 Jul
PMID:Halloysite tubes as nanocontainers for anticorrosion coating with benzotriazole. 2035 46

The paper reports the use of self-assembled monolayers (SAMs) of dithiols to induce electroless copper deposition on a gold substrate. The metallization catalyst, palladium nanoparticles, is bound on the dithiol SAM. The assembly process is followed by IR and X-ray photoelectron spectroscopies to confirm the formation of a monolayer with bound catalyst. Electroless metallization is then carried out with a steady deposition rate of 130 nm/min. Additionally, microcontact printing of the catalyst on the SAM by poly(dimethylsiloxane) stamps is used to localize copper deposits. Resulting metallization is selective and allows for a high resolution.
ACS Appl Mater Interfaces 2009 Mar
PMID:Selective electroless copper deposition on self-assembled dithiol monolayers. 2035 79

By applying an indirect strategy, a new rhodamine-based dye (I) was successfully developed as a colorimetric chemosensor for the sensitive detection of cyanide. In the presence of copper ions, the colorless solution of compound I changed to magenta; however, upon the addition of trace cyanide, the magenta color faded to colorless immediately, with a detection limit as low as 0.013 ppm (DeltaA = 0.054), much lower than the Maximum Contaminant Level for cyanide in drinking water (0.20 ppm) set by the US Environmental Protection Agency. Other anions, including Cl(-), I(-), IO(3)(-), SO(4)(2-), NO(2)(-), Br(-), H(2)PO(4)(-), F(-), SCN(-), HSO(4)(-), and ClO(4)(-), had nearly no influence on the probing behavior of dye I toward cyanide.
ACS Appl Mater Interfaces 2009 Nov
PMID:A new rhodamine-based colorimetric cyanide chemosensor: convenient detecting procedure and high sensitivity and selectivity. 2035 23

Metal copper mesh with superhydrophobic and superoleophilic surface had been successfully fabricated via a facile solution-immersion process. The hierarchical structure was prepared on the commercial copper mesh surface by etching with the nitric acid. After being modified by 1-hexadecanethiol (HDT), the as-prepared mesh indicated both superhydrophobic and superoleophilic property simultaneously. This as-prepared metal mesh could then be applied for oil and water mixture separation. The unusual wettability of the as-prepared mesh was stable in corrosive conditions, such as acidic, basic, and salt solutions. The solution-immersion method was simple, time-saving, and inexpensive and therefore exhibited great potential application.
ACS Appl Mater Interfaces 2009 Nov
PMID:Facile approach in fabricating superhydrophobic and superoleophilic surface for water and oil mixture separation. 2035 34

In recent years, cellulose-based materials have attracted significant attention. To broaden the application areas for cellulose, polymers are often grafted to/from the surface to modify its properties. This study applies ARGET (activators regenerated by electron transfer) ATRP (atom transfer radical polymerization) when straightforwardly grafting methyl methacrylate (MMA), styrene (St), and glycidyl methacrylate (GMA) from cellulose in the form of conventional filter paper in the presence of a sacrificial initiator. The free polymer, formed from the free initiator in parallel to the grafting, was characterized by (1)H NMR and SEC, showing that sufficient control is achieved. However, the analyses also indicated that the propagation from the surface cannot be neglected compared to the propagation of the free polymer at higher targeted molecular weights, which is an assumption often made. The grafted filter papers were evaluated with FT-IR, suggesting that the amount of polymer on the surface increased with increasing monomer conversion, which the FE-SEM micrographs of the substrates also demonstrated. Water contact angle (CA) measurements implied that covering layers of PMMA and PS were formed on the cellulose substrate, making the surface hydrophobic, in spite of low DPs. The CA of the PGMA-grafted filter papers revealed that, by utilizing either aprotic or protic solvents when washing the substrates, it was possible to either preserve or hydrolyze the epoxy groups. Independent of the solvent used, all grafted filter papers were essentially colorless after the washing procedure because of the low amount of copper required when performing ARGET ATRP. Nevertheless, surface modification of cellulose via ARGET ATRP truly facilitates the manufacturing since no thorough freeze-thaw degassing procedures are required.
ACS Appl Mater Interfaces 2009 Nov
PMID:ARGET ATRP for versatile grafting of cellulose using various monomers. 2035 39

Dialkyldithiophosphates (DTPs) of zinc(II), copper(II), and other metals have been extensively used as multifunctional additives in lubricants to control friction and reduce wear in mechanical systems. Among these DTP compounds, zinc dialkyldithiophosphates (ZnDTPs) are the most common additives extensively used for more than 60 years. These additives form a protective film on steel surfaces and, thus, control friction and reduce wear. However, ZnDTPs contain zinc and large amounts of phosphorus and sulfur, which impair the environment, both directly and indirectly, by adversely affecting the performance of catalytic converters of various automobiles. For this reason, environmental legislation imposes limitations on concentrations of phosphorus, sulfur, and zinc in the lubricants. In this work, we report on zinc-free S-di-n-octoxyboron-O,O'-di-n-octyldithiophosphate (DOB-DTP) lubricant additive with amount of phosphorus and sulfur reduced by half in a molecule as compared with ZnDTPs. DOB-DTP was synthesized by a reaction in two steps under inert nitrogen atmosphere. The final product, a viscous liquid, was characterized by the elemental analysis, FT-IR, multinuclear (1)H, (13)C, (31)P, and (11)B NMR spectroscopy and thermal analyses. Tribological performance of a mineral oil with this new additive was evaluated in comparison with O,O'-di-n-butyl-dithiophosphato-zinc(II) (ZnDTP) using a four-ball tribometer. The surface morphology and the elemental composition of the tribofilms were characterized using scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDS). The results show that DOB-DTP has a considerably better antiwear performance and higher stability of the coefficient of friction with time as compared with ZnDTP. Both phosphorus and sulfur were detected by the EDS on the worn steel surfaces at all concentrations of additives in the base oil.
ACS Appl Mater Interfaces 2009 Dec
PMID:Synthesis, physicochemical, and tribological characterization of S-Di-n-octoxyboron-O,O'-di-n-octyldithiophosphate. 2035 64


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