Electrophoretic deposition of phthalocyanine in organic solutions containing trifluoroacetic acid

The absorption spectra of copper phthalocyanine (CuPc) 1,2-dichloroethane (DCE) solutions containing trifluoroacetic acid (TFAA) shows that the number of protons coordinating to the CuPc molecule was 1 and 2 for the first and second proton adducts, respectively, which indicates the formations of CuPcH(+) and CuPcH(2)(2+). This CuPc molecule may act as a catalyst to dissociate TFAA into trifluoroacetate anion (A(-)) and H(+) and form the proton adducts. The electrical conductivity dependence of the solution on CuPc concentration also supports this mechanism. A dense film of CuPc was deposited on an indium tin oxide cathode plate by electrophoresis of the solution. Similar dense films of a wide variety of phthalocyanines (MPc; M = Cu, H(2), Fe, Ni, Zn, Pb, VO) were also deposited using this method. Similar films of CuPc were also formed using dichloromethane (DCM) and 1,1,1-trichloroethane (TCE) in place of DCE. Depositions are ascribed to the migration of positively charged monomers (i.e., protonated MPc). Scanning electron microscopy revealed that these films are composed of fibrous crystallites, size of which was found to increase with the electrophoresis time, the strength of the applied electrical field and the concentration of CuPc in the bath. The influence of the dielectric constant of the organic solvent on the film growth is discussed.     

Adsorption of polyacrylic acid and its copolymers with acrylonitrile on zinc oxide particles

Adsorption of polyacrylic acid and its copolymers with acrylonitrile, containing different quantities of carboxyl groups, on the dispersion of zinc oxide was investigated. The kinetics of polymer desorption was investigated based on data concerning the change in concentration of free carboxylic groups of polymer and zinc ions in solution. The concentration of free carboxyl groups decreases and the concentration of zinc ions in the liquid phase above the residue after separation of zinc oxide particles increases with time, reaching a constant value. The dependence of the concentration of free carboxyl groups and zinc ions in the liquid phase on the initial concentration of polymer in the plateau section of the kinetic curve was investigated. Adsorption isotherms of copolymers depend on their solubility in water and can be described by different mathematical models.     

Electrophoretic transport of latex particles in lipid nanotubes

Lipid vesicles can be connected by membrane nanotubes to build networks with promising bioanalytical properties. Here we characterize electrophoretic transport in such membrane tubes, with a particular eye to how their soft-material nature influences the intratube migration. In the absence of field, the tube radius is 110 +/- 26 nm, and it remains in this range during electrophoresis even though the applied electric field causes a slight decrease in the tube radius (approximately 6-11%). The electrophoretic velocity of the membrane wall (labeled with quantum dots) varies linearly with the field strength. Intratube migration is studied with latex spheres of radii 15, 50, 100, and 250 nm. The largest particle size does not enter the tube at fields strengths lower than 1250 V/m because the energy cost for expanding the tube around the particles is too high. The smaller particles migrate with essentially the same velocity as the membrane at low fields. Above 250 V/cm, the 15 nm particles exhibit an upward deviation from linear behavior and in fact migrate faster than in free solution whereas the 100 nm particles deviate downward. We propose that these nonlinear effects arise because of lipid adsorption to the particles (dominating for 15 nm particles) and a pistonlike compression of the solvent in front of the particles (dominating for 100 nm). As expected from such complexities, existing theories for a sphere migrating in a rigid-wall cylinder cannot explain our velocity results in lipid nanotubes.     

聚丙烯酸/氧化石墨烯复合水凝胶摩擦学性能研究

通过自由基聚合制备了聚丙烯酸(PAA)水凝胶。在水凝胶体系中掺入氧化石墨烯(GO),改善其机械强度。用往复摩擦试验机,在面-面接触的条件下考察了在不同载荷、速度、接触面积下,摩擦力和摩擦系数变化。实验结果表明,PAA水凝胶摩擦行为不遵从传统的固体摩擦定律(Amonton’s law)。通过与铜(Ⅱ)离子络合和去络合作用可实现摩擦系数从极低到较高的可逆调节。     

Electrophoretic deposition and characterization of self-doped SrTiO3 thin films

Herein, titanium (Ti³⁺) self-doped strontium titanate (SrTiO₃), so-called blue SrTiO₃, with a bandgap of 2.6 eV and favorable photocatalytic characteristics was fabricated through a facile and effective method. For electrochemical investigations, the electrophoretic deposition was applied to produce SrTiO₃ thin films on (fluorine-doped tin oxide) FTO conductive substrates. The electrophoretic voltage of 20 V and a process duration of 10 min were optimized to reach transparent and uniform coatings on FTO. The blue SrTiO₃ reveals lower resistance (charge transfer resistance of 6.38 Ω cm^-2) and higher electron mobility (current density value of 0.25 mA cm^-2) compared to a pure SrTiO₃ electrode. These findings may provide new insights for developing high-performance visible light photocatalysts.     

Control of optical properties of gel-derived oxide coating films containing fine metal particles

Control of the optical properties of gel-derived oxide films containing fine metal particles is described. The duration of the aging of Si(OC₂H₅)₄-derived sols and the amount of water for hydrolyzing Si(OC₂H₅)₄ were found to greatly affect the size and the shape of Au particles formed in the silica matrix, and accordingly the optical absorption of the Au/SiO₂ composite films. Employing dielectric media with high refractive indices like TiO₂ was shown to shift the absorption peak of Au particles to longer wavelengths. Pd/TiO₂ and Pt/TiO₂ composite films showed absorption in the visible region.     

Synthesis and characterization of palladium containing membranes based upon polyacrylic acid

Different methods are described to synthesize a highly porous polymer membrane with fine dispersed metal-nanoparticles. The preparation of the porous catalytic membranes happens by crosslinking of polyacrylic acid dispersions with bifunctional crosslinker in presence of palladium particles. Palladium-nanoparticles, stabilized with the block copolymer polystyrene-block-polyethyleneoxide, can be immobilized in the polymer network in different ways. The polymer/metal network can be prepared in the form of thin flat membranes and dried under retention of the porosity and three-dimensional network structure. Different reduction and preparation methods were applied in order to obtain differences in particle size and distribution of the palladium. The morphology of the material was investigated by scanning electron microscopy. Transmission electron microscopy was employed to show the size and distribution of the metal-nanoparticles in the polymeric matrix. The catalytic activity of the obtained membranes was investigated for the gas phase hydrogenation of cyclohexene and propyne.     

Microcrystalline composite particles of carbon nanotubes and calcium carbonate

Coprecipitation of urea-melt modified carbon nanotubes and calcium carbonate from an aqueous solution by two methods yielded microcrystalline composite particles. Powders obtained by colloidal crystallization from a supersaturated solution that were isolated and dried soon after precipitation were a mixture of raspberry-shaped and rhombohedral particles. These were shown by infrared and X-ray diffraction analyses to be mainly calcite. Particles that were kept wet for 1 day or longer before being isolated were typically entirely rhombohedral with edge lengths in the range of 5-30 microm. Scanning electron microscopy investigations revealed that the nanotubes were adsorbed on the particle surface and also incorporated into the interior matrix. Removal of the calcium carbonate component by treating the particles with acid yielded nanotube shells whose size and shape reflected those of the original particles.     

Thermal properties of films of polyethylene with graft polyacrylic acid

The processes of thermal and thermal-oxidative degradation taking place in polyethylene (PE) films modified by graft polyacrylic acid (PAA) have been studied by TG and DTA. The mutual influence of the components on the degradation of the macromolecules present in the graft copolymer has been revealed. The increase in thermal stability of PE in the graft copolymers is explained by the decrease in the molecular mobility in PE amorphous regions containing microphase particles of graft PAA.

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Zusammenfassung Die bei der thermischen und thermisch-oxydativen Zersetzung in durch pfropfpolymerisierte Polyacrylsäure (PAA) verstärkten Polyethylen (PE)-Filmen verlaufenden Prozesse wurden mittels TG und DTA untersucht. Es wurde ein gegenseitiger Einfluß der Komponenten auf den Abbau der Pfropfpolymere bildenden Makromoleküle festgestellt. Die Erhöhung der thermischen Stabilität von PE in Pfropfpolymeren wird durch die Abnahme der molekularen Beweglichkeit in Mikrophasenpartikeln von Pfropf-PAA aufweisenden amorphen Bereichen des PE erklärt.

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Nafion-based composite solid electrolytes containing carbon nanotubes

Nafion-based composite solid electrolytes containing multiwalled carbon nanotubes have been studied by impedance spectroscopy. The effect of carbon nanotube morphology on the proton conductivity of the composites has been estimated at low relative humidity. Surface modification of carbon nanotubes with acidic groups increases the proton conductivity.     

Synthesis of anodic silicon oxide films in water-organic solutions containing orthophosphoric acid

Variations in electrophysical properties of anodic silicon oxide at the surface of semiconductor silicon are studied as a function of the composition of electrolytic solutions containing orthophosphoric acid and the conditions of reaching the final formation potential. The optimum conditions for the formation of anodic SiO₂ coatings that include phosphorus-containing admixtures are determined, the coatings being intended for application as diffusates in nanoelectronics.     

Screen-printed enzymatic glucose biosensor based on a composite made from multiwalled carbon nanotubes and palladium containing particles

A composite material consisting of multiwalled carbon nanotubes and palladium containing particles was synthesized and applied to the preparation of bulk-modified screen-printed carbon electrodes (Pd-MWCNT-SPCE) and surface-modified screen-printed carbon electrodes (Pd-MWCNT/SPCE). They were characterized by cyclic voltammetry and hydrodynamic chronoamperometry in solution of pH 7.5. Both electrodes were then modified with glucose oxidase (GOx) by drop-coating a solution of GOx and Nafion® on their surface. Glucose can be determined via enzymatically formed H₂O₂. In an alternative approach, gold nanoparticles (5 nm) were incorporated into the biolayer of the electrodes. The resulting electrodes of type GOx/Pd-MWCNT-SPCE and GOx-Au/Pd-MWCNT-SPCE showed acceptable analytical performance at working potentials between ?0.20 V and ?0.50 V in case of hydrodynamic chronoamperometry. Both electrodes can be operated best at a working potential of ?0.40 V vs SCE, with acceptable linearity of the methods in sub mM concentration ranges and with LOQs of 0.14 mM and 0.07 mM for glucose for the GOx/Pd-MWCNT-SPCE and GOx-Au/Pd-MWCNT-SPCE, respectively. Incorporation of gold nanoparticles prolongs the operational lifetime of the electrodes by two weeks. The GOx/Pd-MWCNT-SPCE based method was applied to the determination of glucose in multifloral honey, and the GOx-Au/Pd-MWCNT-SPCE method to the determination of glucose in blood serum. In both cases there was a good agreement with the results obtained by commercially available equipment for determination of glucose.

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Graphical abstract Schematic of a screen printed carbon biosensor based on the use of multiwalled carbon nanotubes modified with palladium-containing particles and glucose oxidase. It can be applied to the amperometric determination of glucose in blood serum and multifloral honey

     

Electrophoretic deposition of titanate nanotube films with extremely large wetting contrast

A facile electrophoretic deposition (EPD) process has been developed to prepare thin films consisting of titanate nanotubes (TNTs) that were synthesized by a hydrothermal approach. Such an EPD process offers easy control in the film thickness and the adhesion to the substrate was found to be strong. The chemical composition and structure of the products have been characterized by XRD, HRTEM, and FESEM. It was found that the functionalization of TNTs plays a key role on the electrolyte stability and the formation of a uniform TNT film with good adhesion. The as-prepared TNT films show exceptional superhydrophilic behavior with ultra-fast spreading, while it converts to superhydrophobicity yet with strong adhesion after 1H,1H,2H,2H-perfluorooctyl-triethoxysilane modification. This study provides an interesting method to prepare films with extremely high wettability contrast that are useful for producing different types of functional materials.     

Fabrication of polyimide nanotubes and carbon nanotubes containing magnetic iron oxide in confinement

Polyimide nanotubes with tunable wall thickness were fabricated by a precursor impregnation method using an AAO template, and carbon nanotubes containing magnetic iron oxide were obtained using ferric chloride-embedded polyimide precursor by a carbonization process.     

Fully resonant CARS of cresyl violet in polyacrylic acid polymer films

Multi-resonant CARS data for ground and excited electronic state resonances (593.585 cm^?1) of cresyl violet perchlorate in polyacrylic acid are reported. The intensity of the excited state resonance (585 cm^?1) depends on the location of the ω₁-field (ω_as = 2ω₁ ? ω₂) within the severely inhomogeneously broadened absorption profile of the dye. Non-photochemical hole burning is used to determine the vibronic transitions which contribute to the absorption profile. It is argued that the linear electron-phonon interaction is an important mechanism for producing an egalitarian distribution of excited dye sites with a population sufficiently high to permit observation of the excited state resonance. A marked non-photochemical hole burning effect on the intensities of the CARS resonances is used for the assignment of 585 cm^?1 as an excited state resonance. The absence of line narrowing in the CARS and CSRS spectra is reported and discussed. Finally, a novel narrowing of the 593 cm^?1 ground state resonance with increasing temperature is reported and shown to occur only for restricted values (frequency) of ω₁.     

Plasma-induced deposition of thin films of aluminum oxide

Plasma-induced deposition of wear-protecting A1₂O₃ films has been investigated for two different gas mixtures, one of which is ususally used in thermal CVD. It is shown that, contrary to thermal CVO, the properties of thin films deposited from an AlCl₃/O₂/Ar mixture are superior to those prepared from AICl₃/CO₂/H₂. High Vickers hardness of 1800-2500 and a low chlorine content of 0.7 at. % have been obtained in films deposited from an AICl₃/O₂/Ar mixture at a substrate temperature of 500°C.     

Quantum dot solar cells. Electrophoretic deposition of CdSe-C60 composite films and capture of photogenerated electrons with nC60 cluster shell

Encapsulation with a nC60 cluster shell facilitates capture of photogenerated electrons from CdSe quantum dots following visible light excitation. Electrophoretic deposition of CdSe-C60 composite clusters on optically transparent electrodes (OTE/SnO2) produce photoactive films that exhibit photoelectrochemical activity. The observed photoconversion efficiency (IPCE) of approximately 4% is significantly greater than those observed with CdSe or nC60 films.     

Fabrication of composite films containing zirconia and cationic polyelectrolytes

Composite films were prepared by electrophoretic deposition of poly(ethylenimine) or poly(allylamine hydrochloride) combined with cathodic precipitation of zirconia. Films of up to several micrometers thick were obtained on Ni, Pt, stainless-steel, graphite, and carbon-felt substrates. When the concentration of polyelectrolytes in solutions and the deposition time were varied, the amount of the deposited material and its composition can be varied. The electrochemical intercalation of yttria-stabilized zirconia particles into the composite films has been demonstrated. Obtained results pave the way for the electrodeposition of other polymer-ceramic composites. The deposits were studied by thermogravimetric analysis, X-ray diffraction analysis, scanning electron microscopy, and atomic force microscopy. The mechanisms of deposition are discussed.     

LLDPE films containing monoester of oleic acid grafted to silica particles as durable antifog additives

Antifog additives (AF) are incorporated into polymeric systems to improve their wettability. When added to a polyethylene (PE) film, the AF molecules migrate to the films' surface and their concentration decreases; over time the additive's effect desists. Extended additives' performance is necessary to avoid frequent substitution of PE films for different applications (e.g. greenhouses coverings), as a result, reducing plastics' waste and contributing to environmental sustainability. This paper presents a simple, low cost, one‐step reaction to create durable AF for PE films, as well as a thorough study of AF migration rate, fog activity, and film properties. Films are prepared by compression‐molding (laboratory scale) and cast‐extrusion (pilot scale). FTIR (Fourier Transform IR) and TGA (Thermal Gravimetric Analysis) measurements confirm the existence of AF grafted particles. Aging tests depict a significant decrease of the AF migration rate. An evaluation test procedure for AF performance shows an extended duration of the AF's activity; the cast‐extrusion films exhibit improved AF durability, compared with the compression‐molded films. Copyright © 2016 John Wiley & Sons, Ltd.     

Silica-graphene oxide hybrid composite particles and their electroresponsive characteristics

Silica-graphene oxide (Si-GO) hybrid composite particles were prepared by the hydrolysis of tetraethyl orthosilicate (TEOS) in the presence of hydrophilic GO obtained from a modified Hummers method. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images provided visible evidence of the silica nanoparticles grafted on the surface of GO, resulting in Si-GO hybrid composite particles. Energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) spectra indicated the coexistence of silica and GO in the composite particles. The Si-GO hybrid composite particles showed better thermal stability than that of GO according to thermogravimetric analysis (TGA). The electrorheological (ER) characteristics of the Si-GO hybrid composite based ER fluid were examined further by optical microscopy and a rotational rheometer in controlled shear rate mode under various electric field strengths. Shear stress curves were fitted using both conventional Bingham model and a constitutive Cho-Choi-Jhon model. The polarizability and relaxation time of the ER fluid from dielectric spectra measured using an LCR meter showed a good correlation with its ER characteristics.