Nanofibrous polyaniline thin film prepared by plasma‐induced polymerization technique for detection of NO2 gas

A nanofibrous polyaniline (PANI) thin film was fabricated using plasma‐induced polymerization method and explored its application in the fabrication of NO₂ gas sensor. The effects of substrate position, pressure, and the number of plasma pulses on the PANI film growth rate were monitored and an optimum condition for the PANI thin film preparation was established. The resulting PANI film was characterized with UV–visible spectrophotometer, FTIR, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The PANI thin film possessed nanofibers with a diameter ranging from 15 to 20 nm. The NO₂ gas sensing behavior was studied by measuring the change in electrical conductivity of PANI film with respect to NO₂ gas concentration and exposure time. The optimized sensor exhibited a sensitivity factor of 206 with a response time of 23 sec. The NO₂ gas sensor using nanofibrous PANI thin film as sensing probe showed a linear current response to the NO₂ gas concentration in the range of 10–100 ppm. Copyright © 2009 John Wiley & Sons, Ltd.     

Self-Organization and Analysis of the Morphology of Vacuum Evaporated Polyaniline Films

By using formal estimation methods, it is shown that heterogeneous redox structures, which are formed in the course of oxidation of vacuum evaporated thin polyaniline layers in the temperature range of 0–30°C, become more ordered with the increase in the oxidation temperature.     

Fast determination of evaporation enthalpies of solvents and binary mixtures using a microsilicon chip device with integrated thin film transducers

A silicon chip device with two types of integrated platinum thin film resistors was applied for microcaloric measurements. It was shown that the device is capable of fast characterization of liquid evaporation behaviour and allows the determination of evaporation enthalpies for pure liquids and mixtures. The applicability was demonstrated for a wide range of solvents from nonpolar aliphatic solvents over polar organics to protic solvents (e.g. iso-octane, toluene, acetone, ethanol, methanol and water). The sample volumes were in the range of about 2-5 μL. The determination of transient times, in case of constant power mode, or the power integral over time was used for the fast estimation of binary liquid mixtures. Thermo-resistive measurements of 5 μL droplets of solvent mixtures like methanol/iso-propanol, ethanol/water, iso-octane/iso-propanol and iso-octane/1,4-dioxane showed significant changes in temperature characteristics and evaporation enthalpies in dependence on composition. The applied heating power was about 1 W, which corresponds to measurement times between a few seconds and a minute.     

Formation of poly-p-phenylene thin films and their composites with fullerene by discrete evaporation in vacuum

The effect of parameters of discrete evaporation of poly-p-phenylene (PPP) and C₆₀ on quality of the films formed was studied, PPP and PPP/C₆₀ composite films and heterostructures based on these materials were prepared. It was established that the conjugation length of PPP macromolecules consists of –9–10 units, and they can be electrochemically transformed into the radical cation state at a potential of 2.10 V. Glassy carbon-PPP-C₆₀-Al heterostructures with a rectification ratio of 10⁶–10⁸ were formed.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No, 12, pp, 2918–2921, December, 1996.     

Structural and impedance studies on LaF3 thin films prepared by vacuum evaporation

Lanthanum fluoride thin film has been deposited on glass substrates by PVD method at various deposition temperatures (T_s), viz, 300, 473, 573 and 673 K. The hexagonal phase LaF₃ film has been detected by using glancing angle XRD analysis. The structural parameters such as lattice constants, grain size and micro-strain has been calculated from the XRD data. The F⁻ ion conduction through the grain and grain boundary has been analyzed using impedance analysis. The modulus spectra reveals the non-Debye nature and the distribution of relaxation times of the film.     

Raman spectra and structure of multicomponent oxide planar waveguides prepared by sol-gel

This work was aimed at understanding the structure of SiO₂–MO₂ (M = Ti, Zr, Hf) and SiO₂–HfO₂–MO₂ (M = Ti, Zr) materials, used as mixed oxide glass hosts for Er³⁺ ions in the fabrication of optical planar waveguides by sol-gel processing. This structural study was performed by Waveguide Raman Spectroscopy (WRS), complemented with X-ray diffraction (XRD). The admixture of TiO₂ to HfO₂, SiO₂–HfO₂ and HfO₂–ZrO₂ compositions was found to cause precipitation of nanocrystals of tetragonal HfO₂ or ZrO₂, or the formation of hafnia-titania mixed crystals, depending on the HfO₂/TiO₂ molar ratio.     

Electrical and optical properties of C46H22N8O4KM (M=Co, Fe, Pb) molecular-material thin films prepared by the vacuum thermal evaporation technique

In this work, the synthesis of new materials formed from metallic phthalocyanines (Pcs) and double potassium salt from 1,8-dihydroxianthraquinone is reported. The newly synthesized materials were characterized by scanning electron microscope (SEM), atomic force microscopy (AFM), infrared (IR) and Ultraviolet-visible (UV-vis) spectroscopy. The powder and thin-film samples of the synthesized materials, deposited by vacuum thermal evaporation, show the same intra-molecular bonds as in the IR spectroscopy studies, which suggests that the thermal evaporation process does not alter these bonds. The effect of temperature on conductivity and electrical conduction mechanism was measured in the thin films (approximately 137 nm thickness). They showed a semiconductor-like behaviour with an optical activation energy arising from indirect transitions of 2.15, 2.13 and 3.6eV for the C(46)H(22)N(8)O(4)KFe, C(46)H(22)N(8)O(4)KPb and C(46)H(22)N(8)O(4)KCo thin films.     

Influence of process parameters on the size distribution of PLA microcapsules prepared by combining membrane emulsification technique and double emulsion-solvent evaporation method

Relatively uniform-sized biodegradable poly(lactide) (PLA) microcapsules with various sizes were successfully prepared by combining a glass membrane emulsification technique and water-in-oil-in-water (w₁/o/w₂) double emulsion-solvent evaporation method. A water phase was used as the internal water phase, a mixture solvent of dichloromethane (DCM) and toluene dissolving PLA and Arlacel 83 was used as the oil phase (o). These two solutions were emulsified by a homogenizer to form a w₁/o primary emulsion. The primary emulsion was permeated through the uniform pores of a glass membrane into the external water phase by the pressure of nitrogen gas to form the uniform w₁/o/w₂ double emulsion droplets. Then, the solid polymer microcapsules were obtained by simply evaporating solvent. The influence of process parameters on the size distribution of PLA microcapsules was investigated, with an emphasis on the effect of oil-soluble emulsifier. A unique phenomenon was found that a large part of emulsifier could adsorb on the interface of internal water phase and oil phase, which suppressed its adsorption on the surface of glass membrane, and led to the successful preparation of uniform-sized double emulsion. Finally, by optimizing the process parameters, PLA microcapsules with various sizes having coefficient of variation (CV) value under 14.0% were obtained. Recombinant human insulin (rhI), as a model protein, was encapsulated into the microcapsules with difference sizes, and its encapsulation efficiency and cumulative release were investigated. The result suggested that the release behavior could be simply adjusted just by changing precisely the diameters of microcapsule, benefited from the membrane emulsification technique.     

The full evaporation technique: a promising alternative for residual solvents analysis in solid samples

The static headspace technique is the most common approach to residual solvent analysis in pharmaceutical and environmental matrices. This paper presents an alternative tool where the volatile impurities are released from the matrix by working directly on a small amount of sample at a high equilibration temperature: the so-called Full Evaporation Technique (FET). The capability of this method was evaluated on a mixture of nine solvents, which belong to Class 3 in the classification of the European Pharmacopoeia Agency for residual solvents, at various levels of concentration: ethanol, acetone, 2-propanol, methyl acetate, 2-butanone, ethyl acetate, tetrahydrofuran, 2-methyl-1-propanol, 1-butanol. Data on linearity, accuracy, precision and sensitivity are reported. Use of an internal standard proved to be necessary when using such a method. The method is then successfully applied to the analysis of solvent traces in permethylated beta-cyclodextrin.     

Structure,microstructure and optical properties of cerium oxide thin films prepared by electron beam evaporation assisted with ion beams

Cerium oxide thin films were prepared by combined electron beam evaporation and ion beam assisted deposition techniques (EBE–IBAD). Their crystallographic structures, microstructures, and optical properties were studied as a function of the substrate temperature (200 °C and 500 °C) and the dose of Ar⁺ or O₂⁺ ion assistance during growth. X-ray diffraction was used to estimate the crystallographic texture, grain size, microstrain and lattice constant. Sample microstructure was studied by scanning electron microscopy. Transmission UV–vis spectroscopy was employed to obtain optical information (band gap, density, and refractive index). All films showed a cubic CeO₂ structure with different preferential growth depending on the preparation conditions. The bombardment with Ar⁺ ions during film deposition proved to be very effective for changing the film structure, hindering columnar growth and producing smaller grain sizes and higher values of microstrain and lattice constant. Films grown at 200 °C and Ar⁺ ion assistance showed the highest density, the smallest grain size (～10 nm) and a high expansion of the lattice constant (up to ～1%). This expansion is related to the presence of Ce³⁺ at the grain boundaries. Ion assistance during the growth leads to films with higher values of refractive index and lower values of band gap.     

High mechanical and thermal performance of Sasobit-modified epoxy resin,prepared via vacuum shock technique

In this study, thermal and mechanical properties of novel nanocomposite, epoxy resin reinforced with octadecylamine functionalized graphene oxide (GO-ODA) and Sasobit, prepared via creative vacuum shock technique, were investigated. By introducing 1, 3 and 5 wt% Sasobit to the neat epoxy resin, the tensile strength increased remarkably by 104%, 315% and 266%, respectively due to the unique stiff and crystalline structure of Sasobit. In addition, considerable enhancement of 125% in Young's modulus, 351% in toughness, 562% in impact resistance, ~19 °C in thermal stability and ~7 °C in glass transition temperature of epoxy resin with 3 wt% Sasobit loading was demonstrated. The composite containing 3 wt% Sasobit alone, were found to have even superior properties than GO-ODA/epoxy nanocomposite, as surprisingly 3, 2.9, 2.2 and 2 times more improvement, respectively in tensile strength, toughness, impact strength and thermal stability of epoxy resin compared to reinforcement with GO-ODA were obtained.     

Comparison of the evaporation processes of classical spectrography and optical spectrometry tandem technique for the determination of the relevant environmental elements

The evaporation as a part of the spectrochemical excitation process is a complicated procedure during which different thermo-chemical reactions connected mainly to the formation of carbides are overshot. This one is accelerated namely at the 4000 K on the top of the carrier electrode. The carbide creation markedly affects the evaporation process of single elements of the given matrix and modifies this process. In spite of this it is evident that the intensity of the DC arc has a significant impact on the evaporation of all elements. The evaporation capability of two optical methods, the classical non-controlled direct current (DC) arc spectrography and the PC controlled DC arc optical emission spectrometry, have been compared for the determination of some environmental important elements (Al, Cr, Ni, and V). The experiments were carried out using grating spectrograph PGS-2 and simultaneous multi-channel LECO 750 spectrometer which is connected to a separated evaporation cell and adjusted to the Marinković plasma source. Standardized evaporation curves were designed and the half-time (t_50%) values and the total (t_100%) evaporation time values were calculated. The basic statistical evaluation was done and the main figures of the merit were calculated.     

Fabrication and characterization of TiO2 photocatalytic thin film prepared from peroxo titanic acid sol

A novel sol–gel technique using the PTA (peroxo titanic acid) sol as precursor for the fabrication of TiO₂ photocatalytic thin film is introduced in this paper. The peroxo titanic acid sol was synthesized from titanyl sulfate (TiOSO₄), ammonia and peroxide solution (H₂O₂). The transparent and porous TiO₂ thin film was prepared via a sol–gel technique using PTA sol and polyethylene glycol (PEG) as precursor and template, respectively. The TiO₂ thin film samples were characterized by the X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–visible spectrophotometry (UV–vis), X-ray photoelectron spectrum (XPS) and thermogravimetry and differential thermal analysis (TG-DTA) technique. The PTA sol displayed amorphous TiO₂ below 100 °C. The anatase phase formed at 200 °C to 700 °C. The crystallinity of anatase phase was improved with increasing temperature. The anatase crystals on the surface of TiO₂ film were strip-like, the size being about 100 nm in length and 40 nm in diameter. Addition of PEG to the PTA sol developed porous structures in the film and changed the size and shape of the particles. The surface of the film contained Ti, O and C elements and Na element that diffused into the film from the glass substrate. The photocatalytic performance of TiO₂ film was tested for the degradation of 10 mg/L methyl orange. The degradation of methyl orange solution reached 98.9% after irradiated for 180 min under UV light. The porous TiO₂ thin film exhibited high photocatalytic activity towards degrading methyl orange.     

On the synthesis and characterization of ZnO/MgO nanocomposite by thermal evaporation technique

ZnO/MgO nanocomposites have been synthesized by an easy and cost effective thermal evaporation technique. Various growth temperatures ranging from 800 to 900 °C were tried. It is observed that the process temperature plays a key role in the formation of ZnO/MgO nanocomposite and the proper formation of ZnO/MgO nanocomposite occurs at 875 °C temperature as confirmed by X-ray diffraction studies. Scanning electron microscopic images indicate that the ZnO/MgO nanocomposite is formed as agglomerated nanoparticles distributed over a large area. Energy dispersive X-ray analyses also reveal that the Mg composition in the synthesized nanocomposite strongly depends on the process temperature. Photoluminescence (PL) spectrum exhibits a blue shift for the ZnO/MgO nanocomposite synthesized at 875 °C indicating the incorporation of Mg into the ZnO crystal lattice. A higher PL intensity ratio of band-edge to deep band emission has been observed for this sample indicating the presence of low crystalline defects.     

Probing the early stages of solvent evaporation and relaxation in solvent‐cast polymer thin films by spectroscopic ellipsometry

The formation of solvent‐cast, poly(methyl methacrylate) (PMMA) thin films from dilute bromobenzene solutions was studied using an ellipsometry technique. Bromobenzene has a relatively high refractive index (compared to PMMA), which provides contrast in ellipsometry, allowing the concentration to be determined. The solvent also has a relatively low evaporation rate, which makes the film formation slow enough to capture via the technique. The formation of the glassy film is thus studied in situ, and information on solvent and void concentration in the thin film during the film formation process is obtained. There is evidence that nanovoids (representing intramolecular space) develop in the film when solvent evaporates. Copyright © 2011 John Wiley & Sons, Ltd.     

CO-sensing properties of undoped and doped tin oxide thin films prepared by electron beam evaporation

Undoped thin films of tin oxide and those doped with indium oxide and nickel oxides were deposited by electron beam evaporation. The effects of the film thickness and preparation conditions (films prepared with or without the presence of oxygen environment during deposition) on the optical and carbon monoxide sensing properties of the films were studied. The films were characterized using X-ray diffraction and X-ray photoelectron spectroscopy and optical spectroscopy techniques. All the films were found to be amorphous. It was found that the sensitivity of the films to CO increased with the thickness and the porosity of the films. It was found that their selectivity to CO gas relative to CO₂ and SO₂ gases could be improved upon doping the films with indium (or nickel) oxide.     

Electrical and optical properties of copper and nickel molecular materials with tetrabenzo [b,f,j,n] [1,5,9,13] tetraazacyclohexadecine thin films grown by the vacuum thermal evaporation technique

Semiconducting molecular-material thin-films of tetrabenzo (b,f,j,n) {1,5,9,13} tetraazacyclohexadecine copper(II) and nickel(II) bisanthraflavates have been prepared by using vacuum thermal evaporation on Corning glass substrates and crystalline silicon wafers. The films thus obtained were characterized by infrared spectroscopy (FTIR), atomic force microscopy (AFM), ultraviolet–visible (UV–vis) spectroscopy and ellipsometry. IR spectroscopy showed that the molecular-material thin-films exhibit the same intra-molecular bonds as the original compounds, which suggests that the thermal evaporation process does not significantly alter their bonds. The optical band-gap values calculated from the absorption coefficient may be related to non-direct electronic interband transitions. The effect of temperature on conductivity was also measured in these samples. It was found that the temperature-dependent electric current is always higher for the nickel-based material and suggests a semiconductor-like behavior with conductivities in the order of 10^?8 Ω^?1 cm^?1.     

Electrochemical sensor for acetaminophen based on an imprinted TiO2 thin film prepared by liquid phase deposition

An electrochemical sensor based on a molecularly imprinted TiO₂ thin film is proposed for the determination of acetaminophen. The imprinted TiO₂ films were obtained by liquid phase deposition (LPD) in the presence of acetaminophen, the functional monomer and the aqueous solution of (NH₄)₂TiF₆ and H₃BO₃. The results show that acetaminophen is embedded into the imprinted film in the presence of p-tert-butylcalix[6]arene as a functional monomer, and can be removed completely by washing with ethanol. The surface morphology, spectral properties and electrochemical characterizations of the imprinted sensor were investigated in detail. The combination of molecularly imprinted and LPD technique was shown to be a general strategy for constructing a molecular recognition system.     

Synthesis of TiO2 thin film by a modified sol-gel method and properties of the prepared films for photocatalyst

PTA (peroxo titanic acid) gel was prepared by a modified sol-gel method from peroxo titanic acid using TiCl₄/ethanol/water solution as the starting material at room temperature. Physicochemical properties of heat-treated gel were characterized by IR, XRD, TG-DTA and SEM. Optimal preparing conditions were chosen to prepare anatase film for the photocatalytic degradation of methyl orange. The dip-coating technique was used to synthesis the supported anatase film on quartz glass. Photocatalytic efficiency for the degradation of methyl orange under UV irradiation was also examined. It was found that the degradation efficiency of the anatase film synthesized in this paper is higher than commercial titania P25.