Deposition of boron-containing coatings by electron-beam evaporation of boron-containing targets

Boron-containing films are promising materials for improving the hardness, wear-resistance and durability of mechanical parts used in industry. We describe a novel approach for deposition of such coatings – by using electron-beam evaporation of boron-containing target material (pure boron or boron nitride) in inert (helium) or chemically-active (oxygen, nitrogen, residual atmosphere) gases at medium vacuum. Boron-containing films deposited on titanium substrates were characterized using a nanohardness tester and a non-contact 3D profilometer. Elemental composition of the coatings was studied using raster electron microscope equipped with a device for EDX analysis. All boron-containing coatings provided significant improvement (by a factor of 4–16) in the microhardness of the substrate surface.     

Surfactant‐dispersed carbon black in polyimide nanocomposites: Spectroscopic monitoring of the dispersion state in the polymer matrix

The effects of an anionic surfactant on the dispersion of carbon black (CB) for the purpose of forming conducting composite films were examined with ultraviolet–visible (UV–vis) absorption spectroscopy. To obtain a good dispersion and size reduction of aggregated CB in a polymer matrix, sodium dodecyl sulfate (SDS), used as a surfactant, was introduced into a CB suspension. A set of concentrations with various ratios of CB to SDS (ranging from 1 : 0.4 to 1 : 10) was established before mixing with poly(amic acid) (PAA), a precursor of pyromellitic dianhydride and oxydianiline, was performed. The CB/PAA solution mixtures were submerged under an ultrasonic bath for several hours, then cast onto dry plate glasses, and finally subjected to thermal imidization to produce CB/polyimide (PI) nanocomposite films with various CB weight fractions ranging from 0.025 to 0.50 wt %. A method for evaluating the absorbance at 500 nm of the CB/PI nanocomposite films was established. The absorbance of CB/PI nanocomposite samples of various thicknesses was also normalized to get rid of the effects of the different thicknesses. UV–vis spectra showed that the minimum weight ratio of CB to SDS in the nanocomposite films that achieved well‐dispersed CB and still had transparent properties was 1 : 2.0. Transmission electron microscopy demonstrated that CB was dispersed homogeneously in the PI matrix, and the size of the aggregated CB was affected by the amount of the surfactant. The dielectric properties of the nanocomposite films without the surfactant increased by approximately 2 orders of magnitude with an increasing mass weight fraction of CB and decreased when the surfactant was added. The surfactant also reduced the tensile strength of the CB/PI nanocomposites when the CB/SDS ratio was higher than 1 : 2.0. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Cathodoluminescence from Implanted and Anodized Polycrystalline Silicon Films

Luminescence emission of LPCVD polycrystalline silicon films has been studied by cathodoluminescence (CL) in the scanning electron microscope. As-deposited films show visible luminescence with dominant blue band. The relative intensity of blue emission is enhanced by implantation and by slight anodization treatments. Our investigations are consistent with previous PL results and indicate that the origin of blue emission is related to quantum confinement effects. On the other hand, the effect of annealing in these samples is a reduction of the CL signal that could be related to the increase of the nanocrystals size.     

Structural evolution of β – iPP during uniaxial stretching studied by in–situ WAXS and SAXS

Polymorphism and crystal transition are of great significance for property mediation in polymer materials. Isotactic polypropylene (iPP) with β – crystal has been widely utilized for the preparation of high performance plastics or films. In the present work, the structural evolution of initially isotropic β – nucleated iPP (β – iPP) during uniaxial stretching at different temperatures was investigated by in–situ X – ray scattering using synchrotron radiation. The wide – angle X – ray scattering (WAXS) results confirmed that the β – crystal transformed either to the mesophase at lower temperature (30 °C) or to the α – crystal at higher temperature (60, 100 and 120 °C) during stretching. An interesting orientation of β – crystal with molecular chains perpendicular to the tensile direction was identified. As revealed by small – angle X – ray scattering (SAXS), cavitation took place in β – iPP stretched at temperatures lower than 120 °C. The size and shape of the cavities were observed by scanning electron microscope. A deformation mechanism of β – iPP combining the crystal transition, cavitation and orientation was proposed.     

Fabrication and characterization of Cd-enriched CdTe thin films by close spaced sublimation

Cd-enriched cadmium telluride (CdTe) polycrystalline films were grown on corning glass substrates by close spaced sublimation (CSS) technique. To our knowledge, Cd-enriched CdTe thin films by CSS have not been reported earlier. The structural investigations performed by means of X-ray diffraction (XRD) technique, scanning electron microscope (SEM), and energy dispersive X-ray spectroscopy (EDX) showed that the deposited films exhibit a polycrystalline structure with 〈111〉 as preferred orientation. The structural, optical, and electrical properties of these films were analyzed as a function of the Cd concentration. For the films having an excess of Cd, the electrical resistivity dropped several orders of magnitude. The deposited films also showed that the value of resistivity decreased with increasing temperature manifesting the semiconducting behavior of the films. The results showed that using this deposition technique, n-type Cd-enriched CdTe polycrystalline film could be produced.     

Photocatalytic performance of highly transparent and mesoporous molybdenum-doped titania films fabricated by templating cellulose nanocrystals

In this paper, the synthesis of mesoporous Mo-doped titania films templated by cellulose nanocrystals (CNCs) and their photocatalytic performance are reported for the first time. The prepared titania composite precursors containing the CNCs and molybdenum chloride were spin-coated on indium tin oxide (ITO) glass substrate, followed by calcining at 400?°C for 1?h. X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), scanning electron microscope (SEM), and UV–vis spectrometer were employed to characterize the phase composition, pore structure, morphology, and optical property of the titania films in relation to CNCs templating and Mo doping. Photocatalytic performances of the titania films were also evaluated on the photodegradation of trichloroethylene under a fluorescent light source. The Mo-doped titania films with CNCs templating were highly transparent and mesoporous, exhibiting only anatase phase, high specific surface areas ranging in 135.4 – 149.0?m²/g, and small crystallite sizes of 9.5 – 11.1?nm. The results indicate that Mo ions were successfully doped by substituting for Ti ions in the titania lattice. The Mo doping stabilized the anatase phase and also increased the surface area of the CNCs-templated titania film while decreasing the mean pore width. Notably, the visible light absorption capacity and photocatalytic activity of the CNCs-templated titania films doped with Mo were dramatically greater than those of the pure and the CNCs-templated titania films, which is ascribed to the decreased recombination rate of photoexcited charges and the increased surface area with aids of the CNCs templating and the Mo doping.     

Investigation on the change in structure of tetrahedral amorphous carbon by a large amount of nitrogen incorporation

The change of the structure of carbon films after nitrogen incorporation is a topic of extensive discussion. Concerning this topic, tetrahedral amorphous carbon (ta-C) prepared by filtered cathodic arc deposition was chosen for the present investigations with up to 29 at.% nitrogen incorporated into the films. Studies on the film microstructure in a high-resolution transmission electron microscope (TEM) showed nanocrystalline structures of nitrogenated carbon from the films with a high nitrogen concentration. The variation of the microstructure of the films was thoroughly emphasized from carbon and nitrogen K-edges using electron energy loss spectroscopy (EELS) as well as near-edge X-ray absorption fine structure (NEXAFS), spectroscopy. In addition, NEXAFS spectra were used to find out the most probable molecular structure of the CN system and have been shown to be consistent with results obtained from EELS.     

Protective Effects of Melatonin and Misoprostol against Experimentally Induced Increases in Intestinal Permeability in Rats

Intestinal mucosal barrier dysfunction caused by disease and/or chemotherapy lacks an effective treatment, which highlights a strong medical need. Our group has previously demonstrated the potential of melatonin and misoprostol to treat increases in intestinal mucosal permeability induced by 15-min luminal exposure to a surfactant, sodium dodecyl sulfate (SDS). However, it is not known which luminal melatonin and misoprostol concentrations are effective, and whether they are effective for a longer SDS exposure time. The objective of this single-pass intestinal perfusion study in rats was to investigate the concentration-dependent effect of melatonin and misoprostol on an increase in intestinal permeability induced by 60-min luminal SDS exposure. The cytoprotective effect was investigated by evaluating the intestinal clearance of ⁵¹Cr-labeled EDTA in response to luminal SDS as well as a histological evaluation of the exposed tissue. Melatonin at both 10 and 100 µM reduced SDS-induced increase in permeability by 50%. Misoprostol at 1 and 10 µM reduced the permeability by 50 and 75%, respectively. Combination of the two drugs at their respective highest concentrations had no additive protective effect. These in vivo results support further investigations of melatonin and misoprostol for oral treatments of a dysfunctional intestinal barrier.     

Electrocoupling process and electrochemical deposition of poly(9-vinylcarbazole-co-4-vinyltriphenylamine) films

Poly(9-vinylcarbazole-co-4-vinyltriphenylamine)s, PVKT21 and PVKT45 with 21 mol% and 45 mol% pendant triphenylamine groups respectively, were electrochemically deposited as crosslinked thin films through electrocoupling of pendant triphenylamine moieties during the oxidation process. The electrocoupling process has been elucidated by electrochemical and spectroelectrochemical investigations which reveal that mainly triphenylamine undergoes electrocoupling. The color of the electrodeposited film changes from colorless (neutral state) to orange (semi-oxidized state) and finally to bluish-green (fully oxidized state) when the applied potential is increased from 0 V to 2 V. Electrodeposited films were characterized by atomic force microscope (AFM) and the results show that their morphology can be controlled by changing the precursor concentrations. Through this method a smooth thin film can be fabricated for the application in electroluminescent devices. The electroluminescent devices using electrodeposited PVKTs as hole-transporting layer effectively enhance device performance.     

银微粉的吸附性能及其悬浮体的分散稳定性

采用液相还原法制备了平均粒径为300nm的银微粉,分别测定了银微粉自不同pH的溶液中对十二烷基硫酸钠(SDS)、十六烷基三甲基溴化胺(CTMAB)及聚乙烯吡咯烷酮(PVP)的吸附等温线,并分别考察了这三种物质的浓度对银微粉Zeta电位和悬浮体稳定性的影响。结果表明:SDS和CTMAB在银微粉表面的吸附等温线为双平台型;PVP在银微粉表面的吸附为多层吸附;发现了银微粉的Zeta电位及悬浮体的稳定性与SDS、CTMAB或PVP浓度的依赖关系。     

High-resolution STM-imaging of highly oriented ultra thin poly(ethylene) films

Poly(ethylene) (PE) ultra thin films drawn from the melt have been deposited on highly oriented pyrolytic graphite (HOPG) substrates for an investigation with the scanning tunneling microscope (STM). Similar to earlier examinations of poly (1-butene) (PB-1) ultra thin films (1), the STM investigations exhibited images of PE flakes extending over some hundered nanometers. Their thickness was determined to be much larger than the normal established tunneling distance between the tip and a good conducting (metallic) sample surface. It is supposed that the STM-tip penetrates the film and reduces its thickness by scanning over the film. Thus, a destruction of the film is likely leaving only a monomolecular layer of PE macromolecules on the graphite surface. At higher resolutions an ordered structure pseudomorphic to the simple chain nature of the PE macromolecule is revealed.     

Influence of sodium dodecyl sulfate and cetyl trimethylammonium bromide upon calcium carbonate precipitation on bacterial cellulose

Calcium carbonate was deposed on bacterial cellulose (BC) never-dried membranes in the presence of different concentrations of sodium dodecyl sulfate (SDS) and cetyl trimethylammonium bromide (CTAB) by a precipitation reaction between aqueous solutions of calcium chloride (CaCl₂) and sodium carbonate (Na₂CO₃) containing, or not, surfactant in their composition. Different shapes of crystals were obtained from rhombohedral ones to flowerlike, depending on surfactant type and concentration. From the two surfactants tested, SDS has a greater influence on calcium carbonate morphology than CTAB. The only polymorph obtained in all studied cases was calcite. The composite films BC-calcite were characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and color measurements. The obtained BC-calcium carbonate composites could be used in paper manufacturing.     

PVP-SDS缔合行为与pH及比浓黏度的关系

非离子聚合物-阴离子表面活性剂溶液的pH和黏度随体系内分子聚集形态的不同而发生改变,据此建立pH法和比浓黏度法研究了聚乙烯吡咯烷酮(PVP)与不同浓度十二烷基硫酸钠(SDS)的缔合行为,结果表明2种方法均可表征PVP-SDS的双临界浓度。比浓黏度曲线上的极小值和极大值使比浓黏度法具有很高的灵敏性和准确性,而pH法表明氢离子对PVP-SDS缔合行为有重要作用。     

Fabrication of low surface free energy automotive clear coats: Mechanical and surface chemistry studies

This work aims at improving the surface chemistry and the mechanical properties of a commercial acrylic–melamine clear coat using a functional siliconized additive. The resistance of films against biological degradation was then investigated using pancreatin (simulated bird droppings) and Arabic gum (simulated tree gum). Variations in the surface and bulk chemical structures, as well as the thermomechanical characteristics of the clear coats at different concentrations of the additive, were investigated by a wide range of techniques inclusive of contact angle measurement, gonio‐spectrophotometery, dynamic mechanical thermal analysis (DMTA), energy‐dispersive spectroscopy, atomic force microscope, optical microscope, and attenuated totalreflectance Fourier transform infrared (ATR‐FTIR) spectroscopy. Negligible effect of additive on color change was revealed. It was shown that even at low loadings of additive it could migrate to the surface, producing hydrophobic films with very low surface free energies with water contact angle exceeding 100°. In addition, it was found by DMTA and ATR‐FTIR studies that the functional additive was covalently attached to the acrylic–melamine chains through its hydroxyl groups. However, phase separation was observed at high concentrations of additive, leading to reduced crosslinking density. The clear coat resistance against pancreatin and Arabic gum was improved using optimum concentrations of the additive. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Studies on the preparation and properties of conductive polymers. Part II. Novel method to prepare metallized plastics from metal chelates of polyamides

New metallized films were obtained by the reduction of polyamide metal chelate films with reducing agents. Polyamide metal chelates films exhibited excellent surface resistivity around 10°–10¹ Ω/cm² when treated with sodium borohydride aqueous solutions. Aqueous solutions of polyamide–formic acid with metal salts, and films prepared from those solutions, were analyzed by UV-visible and IR spectroscopy, respectively, in order to investigate and identify the structure of the polyamide metal chelates. Factors that include kinds and concentrations of metal salts, kinds and concentrations of reducing agents, and reduction time, which may affect the conductivity of metallized films, were investigated. The surfaces of these films were treated with sodium borohydride aqueous solution to form a definite metallic luster appearance. The surfaces of these conductive films were proved to be metallized, by means of ESCA analysis. The strongly adhered metal on the films was believed to be responsible for the improvement in electrical conductivity. The mechanical properties and scanning electron microscope (SEM) observations were also studied.     

Solubilization and micellarenhanced ultrafiltration ofo-cresol by Sodium Dodecyl Sulfate Micelles

The solubilization and the micellar-enhanced ultrafiltration (MEUF) of o-cresol were investigated by using an anionic surfactant, sodium dodecyl sulfate (SDS). In order to study the solubilization behaviour of the solute, the semiequilibrium dialysis (SED) method was employed and stirred-cell ultrafiltration experiments were performed for the test of MEUF. The analysis of the results supported that approximately two surfactant molecules provide a location for the solubilized solute within micelle. In the removal of o-cresol by MEUF, as long as high SDS concentrations in the retentate (>0.2 M) are avoided, relatively good rejection of o-cresol (85 %) could be obtained under the conditions used (initial concentration ratio:[o-cresol]/[SDS]=0.2 and 0.6). Furthermore, the ultrafiltration processes were nearly at equilibrium, so that the permeate concentrations of o-cresol could be predicted from the SED results. The separation efficiency was greater at lower o-cresol concentrations when the SDS concentrations were fixed in the feed, while the rejection increased with increasing the SDS concentrations at constant intramicellar mole fraction of the solute Xc. In addition, as the o-cresol loading of retentate increased, the less SDS in the retentate permeated through ultrafiltration membranes. On the other hand, the higher o-cresol loadings reduced the fluxes of MEUF runs.     

Enhanced dielectric properties of poly(vinylidene fluoride)–surface functionalized BiFeO3 composites using sodium dodecyl sulfate as a modulating agent for device applications

In this work, we prepared a series of poly(vinylidene fluoride) (PVDF)–surface functionalized BiFeO₃ (h‐BFO)–Sodium dodecyl sulfate (SDS) composite films by solvent casting method to investigate the effect of SDS in the composites. The X‐ray diffraction confirmed that the structure of h‐BFO significantly changed in the PVDF‐(h‐BFO)‐SDS composite in comparison with the rhombohedral structure of pure BiFeO₃. The microscopic study illustrated that the composite with a higher percentage of SDS content facilitated the dispersion as well as proper distribution of ceramic particles in the polymer matrix. The presence of different functionalities of respective polymer and the modified fillers was confirmed by FTIR Spectrophotometer. The dielectric and electrical study done by Impedance Analyzer revealed that the SDS treated surface functionalized composites showed relatively higher dielectric properties than that of two phase composites and pure polymer. Finally, the ferroelectric properties of the composite films done by P‐E loop tracer revealed that the SDS‐treated composites showed an enhanced remanent polarization. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45040.     

Desorption of the surfactant from the particle surface during latex film formation

Properties of latex films are very dependent on the distribution of the surfactants in the film. It has been recognized that distribution itself depends on the desorption characteristics of the surfactant from the particle-water interface during film formation. This article deals with this problem of surfactant desorption in the particular situation of latex film formation. First, FTIR spectroscopic evidence is presented for desorption of hexadecyl pyridinium chloride (HPCI) in poly(2-ethyl hexyl methacrylate) (P2EHMA) latex films. Some consequences of desorption or non-desorption of various surfactants on the structure and properties of P2EHMA latex films are then presented. This concerns the crystallization of cationic surfactants, HPCI and hexadecyl trimethylammonium bromide (HTAB), in the films and the mechanical properties of films containing ethoxylated nonyl phenol with 10 ethoxy segments (NP10) or sodium dodecyl sulphate (SDS). In the last part, the determination of the fraction of SDS desorbing from the particle–water interface in a model poly(styrene–butyl acrylate–methacrylic acid) latex coalescing in water is described. Other methods for studying desorption are proposed.     

Towards facile fabrication of photonics components from inorganic and hybrid sol-gel films. Preparation and optical properties characterization

New trends towards development of integrated optics and miniaturization of photonic devices require fabrication of miniaturized photonic components. Fabrication of waveguiding films with designed optical properties is a fundamental process for production of planar integrated devices.We report here preparation of thin layers based on TiO₂ precursor (TET – titanium(IV) ethoxide) and SiO₂ precursors, namely inorganic (TEOS – tetraethyl orthosilicate) or organically modified (GLYMO ? 3-glycidoxypropyltrimethoxysilane) as candidates for potential application in the planar integrated circuits.The thin layers were deposited on soda-lime glass substrates using the sol-gel method and dip-coating technique and processed at relatively low temperature (up to 300 °C). Several parameters e.g. a) the type of SiO₂ precursor, b) the presence of complexing agent for TET and c) heat treatment temperature were tested for their influence on thickness and refractive index of the obtained films.Furthermore, a few series of sol-gel films activated with luminescent dye (Rhodamine B) was fabricated. The influence of the above-listed parameters on luminescent properties of the films was characterized because of lack of systematic study in the literature in this aspect. Moreover, a spectrum of the light at the output of a chosen luminescent dye-doped waveguiding film excited by laser source was investigated.In addition, the subject of our investigations were films prepared at 200 °C with various amounts of TET and organically modified SiO₂ precursor in concentration range not presented before. Their optical properties such as homogeneity and values of optical band gap of TiO₂ clusters were explored. For selected samples the waveguide properties including the optical losses were evaluated. For the first time, hybrid films with presented composition and refractive index in range of 1.59–1.71 were used for patterning by nanoimprint technique allowing for reproduction of periodic structures, which may serve for example as grating couplers or DFB (distributed feedback) resonators.     

Nanotribological study of PECVD DLC and reactively sputtered Ti containing carbon films

Amorphous carbon film, also known as DLC film, is a promising material for tribological application. It is noted that properties relevant to tribological application change significantly depending on the method of preparation of these films. These properties are also altered by the compositions of these films. DLC films are well known for their self-lubricating properties, as well. In view of this, the objective of the present work is to compare the tribological properties of diamond like carbon (DLC) film obtained by plasma enhanced chemical vapour deposition (PECVD) with the Ti containing nanocrystalline carbon (Ti/a-C:H) film obtained by unbalanced magnetron sputter deposition (UMSD) in nN load range. Towards that purpose, DLC and Ti/a-C:H films are deposited on silicon substrate by PECVD and UMSD processes respectively. The microstructural features and the mechanical properties of these films are determined by scanning electron microscope (SEM), transmission electron microscope (TEM) and nano indenter. The surface topographies and the friction force surfaces of these films are evaluated by means of an atomic force microscope (AFM). The results show that although PECVD DLC film has higher elastic modulus and higher hardness than UMSD Ti/a-C:H film, the surface roughness and the friction coefficient of PECVD film is significantly higher than that of UMSD Ti/a-C:H film.