Search results for: silica thin films

Authors: Lucero Gonzalez, Salvador Alfaro

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Carbon dioxide (CO2) and methane (CH4) are considered as the compounds with higher abundance among the greenhouse gases (CO2, NOx, SOx, CxHx, etc.), due to its higher concentration, this two gases have a greater impact in the environment pollution and provokes global warming. So, recovery, disposal and subsequent reuse, are of great interest, especially from the ecological and health perspective. By one hand, porous inorganic materials are good candidates to capture gases, because these type of materials are higher stability from the point view of thermal, chemical and mechanical under adsorption gas processes. By another hand, during the design and the synthetic preparation of the porous materials is possible add other intrinsic properties (physicochemical and structural) by adding chemical compounds as dopants or using structured directed agents or surfactants to improve the porous structure, the above features allow to have alternative materials for separation, capture and storage of greenhouse gases. In this work, ordered mesoporous materials base silica were prepared using Surfynol as surfactant. The surfactant micelles are commonly used as self-assembly templates for the development of new structure porous silica’s, adding a variety of textures and structures. By another hand, the Surfynol is a commercial surfactant, is non-ionic, for that is necessary determine its critical micelles concentration (cmc) by the pyrene I1/I3 ratio method, before to prepare silica particles. One time known the CMC, a precursor gel was prepared via sol-gel process at room temperature using TEOS as silica precursor, NH4OH as catalyst, Surfynol as template and H2O as solvent. Then, the gel precursor was treatment hydrothermally in a Teflon-lined stainless steel autoclave with a volume of 100 mL and kept at 100 ºC for 24 h under static conditions in a convection oven. After that, the porous silica particles obtained were impregnated with lithium to improve the CO2 adsorption capacity. Then the silica particles were characterized physicochemical, morphology and structurally, by XRD, FTIR, BET and SEM techniques. The thermal stability and the CO2 adsorption capacity was evaluated by thermogravimetric analysis (TGA). According the results, we found that the Surfynol is a good candidate to prepare silica particles with an ordered structure. Also the TGA analysis shown that the particles has a good thermal stability in the range of 250 °C and 800 °C. The best materials had, the capacity to adsorbing 70 and 90 mg per gram of silica particles and its CO2 adsorption capacity depends on the way to thermal pretreatment of the porous silica before of the adsorption experiments and of the concentration of surfactant used during the synthesis of silica particles. Acknowledgments: This work was supported by SIP-IPN through project SIP-20161862.

Keywords: CO2 adsorption, lithium as dopant, porous silica, surfynol as surfactant, thermogravimetric analysis

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Authors: Hikmet Cicek

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Transition metal nitrides are widely used as protective coatings on machine parts and cutting tools to protect the surfaces from abrasion and corrosion for decades. In this study, the ternary TiNbVN thin coatings were produced with closed field unbalanced magnetron sputtering system and their structural, mechanical and fatigue-like (multi-pass scratch test) properties were investigated. Two different substrates (M2 and H13 steels) were used to explore substrates effects. X-Ray diffractometer, scanning electron microscope, and energy dispersive spectroscopy were used for the structural and chemical analysis of the coatings. Nanohardness tests were proceed for mechanical properties. The fatigue-like properties of the coatings obtained from the multi-scratch test under three different cycle passes. The results showed that TiNbVN films have excellent fatigue resistance and the coatings deposited on M2 steel substrate have higher hardness and better fatigue resistance.

Keywords: physical vapor deposition, fatigue, metal nitride, multipass scratch test

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Authors: Pemika Ketsuwan, Pitt Supaphol, Manit Nithitanakul

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A typical used of ethylene methyl acrylate (EMA) gasket is in the manufacture of optical lens, and often, they are deteriorated rapidly due to high temperature during the process. The objective of this project is to improve the thermal stability of the EMA copolymer gasket by preparing EMA with cellulose and silica composites. Hydroxy propyl methyl cellulose (HPMC) and Carboxy methyl cellulose (CMC) were used in preparing of EMA/cellulose composites and fumed silica (SiO2) was used in preparing EMA/silica composites with different amounts of filler (3, 5, 7, 10, 15 wt.%), using a twin screw extruder at 160 °C and the test specimens were prepared by the injection molding machine. The morphology and dispersion of fillers in the EMA matrix were investigated by field emission scanning electron microscopy (FESEM). The thermal stability of the composite was determined by thermal gravimetric analysis (TGA), and differential scanning calorimeter (DSC). Mechanical properties were evaluated by tensile testing. The developed composites were found to enhance thermal and mechanical properties when compared to that of the EMA copolymer alone.

Keywords: ethylene methyl acrylate, HPMC, Silica, Thermal stability

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Authors: P. C. Okafor, A. J. Ekpunobi

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Mn doped copper sulphide (CuS:Mn) nano-films were deposited on indiums coated tin oxide (ITO) glass substrates using electrodeposition method. Electrodeposition was carried out using bath of PH = 3 at room temperature. Other depositions parameters such as deposition time (DT) are kept constant while Mn doping was varied from 3% to 23%. Absorption spectra of CuS:Mn films was obtained by using JENWAY 6405 UV-VIS -spectrophotometer. Optical band gap (E_g ), optical conductivity (σo) and electrical conductivity (σe) of CuS:Mn films were determined using absorption spectra and appropriate formula. The effect of Mn doping % on these properties were investigated. Results show that film thickness (t) for the 13.27 nm to 18.49 nm; absorption coefficient (α) from 0.90 x 1011 to 1.50 x 1011 optical band gap from 2.29eV to 2.35 eV; optical conductivity from 1.70 x 1013 and electrical conductivity from 160 millions to 154 millions. Possible applications of such films for solar cells fabrication and optoelectronic devices applications were also discussed.

Keywords: copper sulphide (CuS), Manganese (Mn) doping, electrodeposition, optical band gap, optical conductivity, electrical conductivity

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Authors: Jihyun Park, Tae Il Lee, Jae-Min Myoung

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A Silver (Ag) thin film is introduced as a template and doping source for vertically aligned p–type ZnO nanorods. ZnO nanorods were grown using a ammonium hydroxide based hydrothermal process. During the hydrothermal process, the Ag thin film was dissolved to generate Ag ions in the solution. The Ag ions can contribute to doping in the wurzite structure of ZnO and the (111) grain of Ag thin film can be the epitaxial temporal template for the (0001) plane of ZnO. Hence, Ag–doped p–type ZnO nanorods were successfully grown on the substrate, which can be an electrode or semiconductor for the device application. To demonstrate the potentials of this idea, p–n diode was fabricated and its electrical characteristics were demonstrated.

Keywords: hydrothermal process, Ag–doped ZnO nanorods, p–type ZnO

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Authors: Ane Escobar, Paula Angelomé, Mihaela Delcea, Marek Grzelczak, Sergio Enrique Moya

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The antibacterial capacity of bone-anchoring implants can be improved by the use of antibiotics that can be delivered to the media after the surgery. Mesoporous films have shown great potential in drug delivery for orthopedic applications, since pore size and thickness can be tuned to produce different surface area and free volume inside the material. This work shows the synthesis of mesoporous titania films (MTF) by sol-gel chemistry and evaporation-induced self-assembly (EISA) on top of glass substrates. Pores with a diameter of 12nm were observed by Transmission Electron Microscopy (TEM). A film thickness of 100 nm was measured by Scanning Electron Microscopy (SEM). Gentamicin was used to study the antibiotic delivery from the film by means of High-performance liquid chromatography (HPLC). The Staphilococcus aureus strand was used to evaluate the effectiveness of the penicillin loaded films toward inhibiting bacterial colonization. MC3T3-E1 pre-osteoblast cell proliferation experiments proved that MTFs have a good biocompatibility and are a suitable surface for MC3T3-E1 cell proliferation. Moreover, images taken by Confocal Fluorescence Microscopy using labeled vinculin, showed good adhesion of the MC3T3-E1 cells to the MTFs, as well as complex actin filaments arrangement. In order to improve cell proliferation Bone Morphogenetic Protein-2 (BMP-2) was adsorbed on top of the mesoporous film. The deposition of the protein was proved by measurements in the contact angle, showing an increment in the hydrophobicity while the protein concentration is higher. By measuring the dehydrogenase activity in MC3T3-E1 cells cultured in dually functionalized mesoporous titatina films with gentamicin and BMP-2 is possible to find an improvement in cell proliferation. For this purpose, the absorption of a yellow-color formazan dye, product of a water-soluble salt (WST-8) reduction by the dehydrogenases, is measured. In summary, this study proves that by means of the surface modification of MTFs with proteins and loading of gentamicin is possible to achieve an antibacterial effect and a cell growth improvement.

Keywords: antibacterial, biocompatibility, bone morphogenetic protein-2, cell proliferation, gentamicin, implants, mesoporous titania films, osteoblasts

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Authors: Nalla Somaiah, Praveen Kumar

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Scaling of transistors and, hence, interconnects is very important for the enhanced performance of microelectronic devices. Scaling of devices creates significant complexity, especially in the multilevel interconnect architectures, wherein current crowding occurs at the corners of interconnects. Such a current crowding creates hot-spots at the respective corners, resulting in non-uniform temperature distribution in the interconnect as well. This non-uniform temperature distribution, which is exuberated with continued scaling of devices, creates a temperature gradient in the interconnect. In particular, the increased current density at corners and the associated temperature rise due to Joule heating accelerate the electromigration induced failures in interconnects, especially at corners. This has been the classic reliability issue associated with metallic interconnects. Herein, it is generally understood that electromigration induced damages can be avoided if the length of interconnect is smaller than a critical length, often termed as Blech length. Interestingly, the effect of non-negligible temperature gradients generated at these corners in terms of thermomigration and electromigration-thermomigration coupling has not attracted enough attention. Accordingly, in this work, the interplay between the electromigration and temperature gradient induced mass transport was studied using standard Blech structure. In this particular sample structure, the majority of the current is forcefully directed into the low resistivity metallic film from a high resistivity underlayer film, resulting in current crowding at the edges of the metallic film. In this study, 150 nm thick Cu metallic film was deposited on 30 nm thick W underlayer film in the configuration of Blech structure. Series of Cu thin strips, with lengths of 10, 20, 50, 100, 150 and 200 μm, were fabricated. Current density of ≈ 4 × 1010 A/m² was passed through Cu and W films at a temperature of 250ºC. Herein, along with expected forward migration of Cu atoms from the cathode to the anode at the cathode end of the Cu film, backward migration from the anode towards the center of Cu film was also observed. Interestingly, smaller length samples consistently showed enhanced migration at the cathode end, thus indicating the existence of inverse Blech length effect in presence of temperature gradient. A finite element based model showing the interplay between electromigration and thermomigration driving forces has been developed to explain this observation.

Keywords: Blech structure, electromigration, temperature gradient, thin films

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Authors: Eun Ju Park, Wendy Rusli, He Tao, Alexander M. Van Herk, Sanggu Kim

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Hollow micro-/nano- structured materials have proven to be promising in wide range of applications, such as catalysis, drug delivery and controlled release, biotechnology, and personal and consumer care. Hollow sphere structures can be obtained through various templating approaches; colloid templates, emulsion templates, multi-surfactant templates, and single crystal templates. Vesicles are generally the self-directed assemblies of amphiphilic molecules including cationic, anionic, and cationic surfactants in aqueous solutions. The directed silica capsule formations were performed at the surface of dioctadecyldimethylammoniumbromide(DODAB) bilayer vesicles as soft template. The size of DODAB bilayer vesicles could be tuned by extrusion of a preheated dispersion of DODAB. The synthesized hollow silica particles were characterized by conventional TEM, cryo-TEM and SEM to determine the morphology and structure of particles and dynamic light scattering (DLS) method to measure the particle size and particle size distribution.

Keywords: characterization, DODAB, hollow silica particle, synthesis, vesicle

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Authors: M. V. Bartashevich

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The problem of heat transfer at thin laminar liquid film is solved numerically. A thin film of liquid flows down an inclined surface under conditions of variable heat flux on the wall. The use of thin films of liquid allows to create the effective technologies for cooling surfaces. However, it is important to investigate the most suitable cooling regimes from a safety point of view, in order, for example, to avoid overheating caused by the ruptures of the liquid film, and also to study the most effective cooling regimes depending on the character of the distribution of the heat flux on the wall, as well as the character of the blowing of the film surface, i.e., the external shear stress on its surface. In the statement of the problem on the film surface, the heat transfer coefficient between the liquid and gas is set, as well as a variable external shear stress - the intensity of blowing. It is shown that the combination of these factors - the degree of uniformity of the distribution of heat flux on the wall and the intensity of blowing, affects the efficiency of heat transfer. In this case, with an increase in the intensity of blowing, the cooling efficiency increases, reaching a maximum, and then decreases. It is also shown that the more uniform the heating of the wall, the more efficient the heat sink. A separate study was made for the flow regime along the horizontal surface when the liquid film moves solely due to external stress influence. For this mode, the analytical solution is used for the temperature at the entrance region for further numerical calculations downstream. Also the influence of the degree of uniformity of the heat flux distribution on the wall and the intensity of blowing of the film surface on the heat transfer efficiency was also studied. This work was carried out at the Kutateladze Institute of Thermophysics SB RAS (Russia) and supported by FASO Russia.

Keywords: Heat Flux, Heat Transfer Enhancement, External Blowing, Thin Liquid Film

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Authors: Fernando G. Torres, Omar P. Troncoso

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A wide range of bacteria synthesizes and secretes polymeric substances composed of a mixture of high-molecular-mass heteropolysaccharides. Nostoc commune cyanobacteria grow in colonial spherules of 10-20 mm in diameter. These spherules are filled with an internal gel made from a variety of polysaccharides known as Nostoc commune exopolysaccharides (NCE). In this paper, we report the use of these exopolysaccharides as a raw material for the preparation of a solid polymer electrolyte. Ammonium iodide and 1-butyl-3-methylimidazolium chloride ([Bmim]Cl) salts were used to provide NCE films with ionic conductivity. In addition, a carboxymethylation treatment was used to further increase the conductivity of NCE films. The structural characterization of the NCE films was assessed by FTIR, XRD, and DSC tests. Broadband dielectric spectroscopy (BDS) and dielectric thermal analysis (DETA) were used to evaluate the ionic conductivity of the samples. The results showed that NCE can be used to prepare solid polymer electrolyte films and that carboxymethylation improves their ionic conductivity. These NCE films can be used in the development of novel energy storage devices such as flat batteries or supercapacitors.

Keywords: polymer electrolyte, Nostoc commune, cyanobacteria, exopolysaccharides

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Authors: Debabrata Bhadra, B. K. Chaudhuri

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The operation of organic thin film transistors (OFETs) with low voltage is currently a prevailing issue. We have fabricated anthracene thin-film transistor (TFT) with an ultrathin layer (~450nm) of Poly-vinylidene fluoride (PVDF)/CuO nanocomposites as a gate insulator. We obtained a device with excellent electrical characteristics at low operating voltages (<1V). Different layers of the film were also prepared to achieve the best optimization of ideal gate insulator with various static dielectric constant (εr ). Capacitance density, leakage current at 1V gate voltage and electrical characteristics of OFETs with a single and multi layer films were investigated. This device was found to have highest field effect mobility of 2.27 cm2/Vs, a threshold voltage of 0.34V, an exceptionally low sub threshold slope of 380 mV/decade and an on/off ratio of 106. Such favorable combination of properties means that these OFETs can be utilized successfully as voltages below 1V. A very simple fabrication process has been used along with step wise poling process for enhancing the pyroelectric effects on the device performance. The output characteristic of OFET after poling were changed and exhibited linear current-voltage relationship showing the evidence of large polarization. The temperature dependent response of the device was also investigated. The stable performance of the OFET after poling operation makes it reliable in temperature sensor applications. Such High-ε CuO/PVDF gate dielectric appears to be highly promising candidates for organic non-volatile memory and sensor field-effect transistors (FETs).

Keywords: organic field effect transistors, thin film transistor, gate dielectric, organic semiconductor

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Authors: M. Khlifa, A. Youssef, A. F. Zaed, A. Kraft, V. Arrighi

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A series of PS-nanoparticles were prepared by grafting PS from both aggregated silica and colloidally silica using atom-transfer radical polymerisation (ATRP). The mechanical behaviour of the nanocomposites have been examined by differential scanning calorimetry (DSC)and dynamic mechanical thermal analysis (DMTA).

Keywords: ATRP, nanocomposites, polystyrene, reinforcement

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Authors: Moosa Mazloom, Hojjat Hatami

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The aim of this article is to access the optimal mix design of self-compacting light weight concrete. The effects of magnetic water, superplasticizer based on polycarboxylic-ether, and silica fume on characteristics of this type of concrete are studied. The workability of fresh concrete and the compressive strength of hardened concrete are considered here. For this purpose, nine mix designs were studied. The percentages of superplasticizer were 0.5, 1, and 2% of the weight of cement, and the percentages of silica fume were 0, 6, and 10% of the weight of cement. The water to cementitious ratios were 0.28, 0.32, and 0.36. The workability of concrete samples was analyzed by the devices such as slump flow, V-funnel, L box, U box, and Urimet with J ring. Then, the compressive strengths of the mixes at the ages of 3, 7, 28, and 90 days were obtained. The results show that by using magnetic water, the compressive strengths are improved at all the ages. In the concrete samples with ordinary water, more superplasticizer dosages were needed. Moreover, the combination of superplasticizer and magnetic water had positive effects on the mixes containing silica fume and they could flow easily.

Keywords: magnetic water, self-compacting light weight concrete, silica fume, superplasticizer

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Authors: Ali Garba Danjani, Abdulrasheed Halliru Usman

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Due to the rapidly increasing biological applications and antibacterial properties of versatile chitosan composites, the effects of chitosan/polyvinyl chloride composites film were investigated. Chitosan/polyvinyl chloride films were prepared by a casting method. Polyethylene glycol (PEG) was used as a plasticizer in the blending stage of film preparation. Characterizations of films were done by Scanning Electron microscopy (SEM), Fourier transforms infrared spectroscopy (FTIR), and thermogravimetric analyzer (TGA). Chitosan composites incorporation enhanced the antibacterial activity of chitosan films against Escherichia coli and Staphylococcus aureus. The composite film produced is proposed as packaging or coating material because of its flexibility, antibacterial efficacy, and good mechanical strength.

Keywords: chitosan, polymeric nanocomposites, antibacterial activity, polymer blend

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Authors: Ping Ren, Mao Wen, Kan Zhang, Weitao Zheng

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The improvement of comprehensive properties including hardness, toughness, wear, and corrosion resistance in the transition metal carbides/nitrides TMCN films, especially avoiding the trade-off between hardness and toughness, is strongly required to adapt to various applications. Although incorporating ductile metal DM phase into the TMCN via thermally-induced phase separation has been emerged as an effective approach to toughen TMCN-based films, the DM is just limited to some soft ductile metal (i.e. Cu, Ag, Au immiscibility with the TMCN. Moreover, hardness is highly sensitive to soft DM content and can be significantly worsened. Hence, a novel preparation method should be attempted to broaden the DM selection and assemble much more ordered nanocomposite structure for improving the comprehensive properties. Here, we provide a new strategy, by activating solid-state dewetting during layered deposition, to accomplish the self-assembly of ordered TaC@Ta core-shell-like nanocomposite film consisting of TaC nanocrystalline encapsulated with thin pseudocrystal Ta tissue. That results in the superhard (~45.1 GPa) dominated by Orowan strengthening mechanism and high toughness attributed to indenter-induced phase transformation from the pseudocrystal to body-centered cubic Ta, together with the drastically enhanced wear and corrosion resistance. Furthermore, very thin pseudocrystal Ta encapsulated layer (~1.5 nm) in the TaC@Ta core-shell-like structure helps for promoting the formation of lubricious TaOₓ Magnéli phase during sliding, thereby further dropping the coefficient of friction. Apparently, solid-state dewetting may provide a new route to construct ordered TMC(N)@TM core-shell-like nanocomposite capable of combining superhard, high toughness, low friction, superior wear with corrosion resistance.

Keywords: corrosion, nanocomposite film, solid-state dewetting, tribology

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Authors: Hiroyuki Aoki, Toru Asada, Tomomi Tanii

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The properties of a spin-cast film of a polymer material are different from those in the bulk material because the polymer chains are frozen in an un-equilibrium state due to the rapid evaporation of the solvent. However, there has been little information on the un-equilibrated conformation and dynamics in a spin-cast film at the single chain level. The real-space observation of individual chains would provide direct information to discuss the morphology and dynamics of single polymer chains. The recent development of super-resolution fluorescence microscopy methods allows the conformational analysis of single polymer chain. In the current study, the conformation of a polymer chain in a spin-cast film by the super-resolution microscopy. Poly(methyl methacrylate) (PMMA) with the molecular weight of 2.2 x 10^6 was spin-cast onto a glass substrate from toluene and chloroform. For the super-resolution fluorescence imaging, a small amount of the PMMA labeled by rhodamine spiroamide dye was added. The radius of gyration (Rg) was evaluated from the super-resolution fluorescence image of each PMMA chain. The mean-square-root of Rg was 48.7 and 54.0 nm in the spin-cast films prepared from the toluene and chloroform solutions, respectively. On the other hand, the chain dimension in a bulk state (a thermally annealed 10- μm-thick sample) was observed to be 43.1 nm. This indicates that the PMMA chain in the spin-cast film takes an expanded conformation compared to the unperturbed chain and that the chain dimension is dependent on the solvent quality. In a good solvent, the PMMA chain has an expanded conformation by the excluded volume effect. The polymer chain is frozen before the relaxation from an un-equilibrated expanded conformation to an unperturbed one by the rapid solvent evaporation.

Keywords: chain conformation, polymer thin film, spin-coating, super-resolution optical microscopy

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Authors: Ali Zazi, Ouiza Cherifi

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Natural gas currently represents a raw material of choice for the manufacture of a wide range of chemical products via synthesis gas, among the routes of transformation of methane into synthesis gas The reaction of the oxidation of methane by gas vapor 'water. This work focuses on the study of the effect of cerieum on the nickel-based catalyst supported by silica for the methane vapor reforming reaction, with a variation of certain parameters of the reaction. The reaction temperature, the H₂O / CH₄ ratio and the flow rate of the reaction mixture (CH₄-H₂O). Two catalysts were prepared by impregnation of Degussa silica with a solution of nickel nitrates and a solution of cerium nitrates [Ni (NO₃) 2 6H₂O and Ce (NO₃) 3 6H₂O] so as to obtain the 1.5% nickel concentrations. For both catalysts and plus 1% cerium for the second catalyst. These Catalysts have been characterized by physical and chemical analysis techniques: BET technique, Atomic Absorption, IR Spectroscopy, X-ray diffraction. These characterizations indicated that the nitrates had impregnated the silica. And that the NiO and Ce₂O3 phases are present and Ni°(after reaction). The BET surface of the silica decreases without being affected. The catalytic tests carried out on the two catalysts for the steam reforming reactions show that the addition of cerium to the nickel improves the catalytic performances of the nickel. And that these performances also depend on the parameters of the reaction, namely the temperature, the rate of the reaction mixture, and the ratio (H₂O / CH₄).

Keywords: heterogeneous catalysis, steam reforming, Methane, Nickel, Cerium, synthesis gas, hydrogen

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Authors: Rudolf Hrach, Stanislav Novak, Vera Hrachova

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Composite and nanocomposite films represent the class of promising materials and are often objects of the study due to their mechanical, electrical and other properties. The most interesting ones are probably the composite metal/dielectric structures consisting of a metal component embedded in an oxide or polymer matrix. Behaviour of composite films varies with the amount of the metal component inside what is called filling factor. The structures contain individual metal particles or nanoparticles completely insulated by the dielectric matrix for small filling factors and the films have more or less dielectric properties. The conductivity of the films increases with increasing filling factor and finally a transition into metallic state occurs. The behaviour of composite films near a percolation threshold, where the change of charge transport mechanism from a thermally-activated tunnelling between individual metal objects to an ohmic conductivity is observed, is especially important. Physical properties of composite films are given not only by the concentration of metal component but also by the spatial and size distributions of metal objects which are influenced by a technology used. In our contribution, a study of composite structures with the help of methods of computational physics was performed. The study consists of two parts: -Generation of simulated composite and nanocomposite films. The techniques based on hard-sphere or soft-sphere models as well as on atomic modelling are used here. Characterizations of prepared composite structures by image analysis of their sections or projections follow then. However, the analysis of various morphological methods must be performed as the standard algorithms based on the theory of mathematical morphology lose their sensitivity when applied to composite films. -The charge transport in the composites was studied by the kinetic Monte Carlo method as there is a close connection between structural and electric properties of composite and nanocomposite films. It was found that near the percolation threshold the paths of tunnel current forms so-called fuzzy clusters. The main aim of the present study was to establish the correlation between morphological properties of composites/nanocomposites and structures of conducting paths in them in the dependence on the technology of composite films.

Keywords: composite films, computer modelling, image analysis, nanocomposite films

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Authors: Navneet Dabra, Baljinder Kaur, Lakhbir Singh, V. Annapu Reddy, R. Nath, Dae-Yong Jeong, Jasbir S. Hundal

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The ferroelectric properties of fused potassium nitrate (KNO3)- polyvinyl alcohol (PVA) composite films have been investigated. The composite films of KNO3-PVA have been prepared by solvant cast technique and then fused over the brass substrate. The ferroelectric hysteresis loops (P-E) have been obtained at room temperature using modified Sawyer-Tower circuit. Percentage of back switching and differential dielectric constant has been derived from P-V loops. The x-ray diffraction (XRD) studies confirm the formation of ferroelectric phase (phase III) in these composite films. The AFM and FE-SEM studies have been used to study the surface morphology of these composite films. The values of remanemt polarization, coercive field, back switching, crystallite size, lattice parameters, and surface roughness have been estimated and correlated.

Keywords: ferroelectric polymer composite, remanemt polarization, back switching, crystallite size, lattice parameters and surface roughness

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Authors: Suman Singh, Myungho Lee, Insik Park, Yangjai Shin, Youn Suk Lee

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Active antimicrobial films prepared by incorporating AgSiO2, AgZn, and AgZ at 1%, 3%, 5%, 10% (w/w) into polypropylene (PP) matrix. Complete thermal, structural, mechanical and functional characterization were carried out of all formulations and determined the antimicrobial efficiency and returnable antimicrobial efficiency according to the Japanese Industrial Standard method. The morphology of the films showed agglomerates of particles in the composites. The active formulation had decreased elongation compared to the pure PP sample. Thermal analyses indicated that the active formulation compositions had increased thermal stability. The films showed 50% antimicrobial properties after the fifth wash against the tested microorganisms, presenting better activity against Gram negative organisms than Gram positive ones. These findings suggest that PP films with AgSiO2, AgZn, and AgZ particles could provide a significant contribution to the quality and safety of seafood in the distribution chain.

Keywords: antimicrobial film, properties and characterization, returnable packaging, sea food

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Authors: Sibani Bisoyi, Ute Zschieschang, Alexander Hoyer, Hagen Klauk

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Abstract— Organic thin-film transistors (TFTs) have great potential to be used for various applications such as flexible displays or sensors. For some of these applications, the TFTs must be able to withstand temperatures in excess of 100 °C, for example to permit the integration with devices or components that require high process temperatures, or to make it possible that the devices can be subjected to the standard sterilization protocols required for biomedical applications. In this work, we have investigated how the thermal stability of low-voltage small-molecule semiconductor dinaphtho[2,3-b:2’,3’-f]thieno[3,2-b]thiophene (DNTT) TFTs is affected by the encapsulation of the TFTs and by the ambient in which the thermal stress is performed. We also studied to which extent the thermal stability of the TFTs depends on the channel length. Some of the TFTs were encapsulated with a layer of vacuum-deposited Teflon, while others were left without encapsulation, and the thermal stress was performed either in nitrogen or in air. We found that the encapsulation with Teflon has virtually no effect on the thermal stability of our TFTs. In contrast, the ambient in which the thermal stress is conducted was found to have a measurable effect, but in a surprising way: When the thermal stress is carried out in nitrogen, the mobility drops to 70% of its initial value at a temperature of 160 °C and to close to zero at 170 °C, whereas when the stress is performed in air, the mobility remains at 75% of its initial value up to a temperature of 160 °C and at 60% up to 180 °C. To understand this behavior, we studied the effect of the thermal stress on the semiconductor thin-film morphology by scanning electron microscopy. While the DNTT films remain continuous and conducting when the heating is carried out in air, the semiconductor morphology undergoes a dramatic change, including the formation of large, thick crystals of DNTT and a complete loss of percolation, when the heating is conducted in nitrogen. We also found that when the TFTs are heated to a temperature of 200 °C in air, all TFTs with a channel length greater than 50 µm are destroyed, while TFTs with a channel length of less than 50 µm survive, whereas when the TFTs are heated to the same temperature (200 °C) in nitrogen, only the TFTs with a channel smaller than 8 µm survive. This result is also linked to the thermally induced changes in the semiconductor morphology.

Keywords: organic thin-film transistors, encapsulation, thermal stability, thin-film morphology

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Authors: F. Laatar, S. Ktifa, H. Ezzaouia

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Plasma Enhanced Chemical Vapor Deposition (PECVD) method is used to deposit hydrogenated nanocrystalline silicon films (nc-Si: H) on Porous Anodic Alumina Films (PAF) on glass substrate at different deposition duration. Influence of the deposition time on the physical properties of nc-Si: H grown on PAF was investigated through an extensive correlation between micro-structural and optical properties of these films. In this paper, we present an extensive study of the morphological, structural and optical properties of these films by Atomic Force Microscopy (AFM), X-Ray Diffraction (XRD) techniques and a UV-Vis-NIR spectrometer. It was found that the changes in DT can modify the films thickness, the surface roughness and eventually improve the optical properties of the composite. Optical properties (optical thicknesses, refractive indexes (n), absorption coefficients (α), extinction coefficients (k), and the values of the optical transitions EG) of this kind of samples were obtained using the data of the transmittance T and reflectance R spectra’s recorded by the UV–Vis–NIR spectrometer. We used Cauchy and Wemple–DiDomenico models for the analysis of the dispersion of the refractive index and the determination of the optical properties of these films.

Keywords: hydragenated nanocrystalline silicon, plasma processing chemical vapor deposition, X-ray diffraction, optical properties

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Authors: Phanawan Whangdee, Tomoaki Watanabe, Viritpon Srimaneepong, Dujreutai Pongkao Kashima

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The anodized films formed at high current density or high voltage have been widely prepared for dental implant because it can improve the hydrophilicity to the film. Our attempt is exploring whether low current density and low voltage could enhance the good hydrophilicity to the anodized films or not. Furthermore, UV irradiation would be one of the key factor to enhance their hydrophilicity. The anodized films were performed at low current density of 2 mA/cm2 in 1M H3PO4, 1 mA/cm2 in 1M MCPM and low voltage of 6 V in either 1M H3PO4 or 1M MCPM. All samples were treated with UV for various times up to 24 h. After UV irradiation, the contact angle decreased, the chemical species changed. The Ti 2p and O 1s peaks increased, while the C 1s peak decreased which might be due to removal of hydrocarbon. The functional groups of the films shown as the change of OH groups appeared at wave number 3700 cm-1 and 2900-3000 cm-1, however, the peak of H2O at 1630 cm-1disappeared. It is indicated that UV irradiation might change the stretching modes of OH groups coordinated to surface Ti4+ cation but UV did not affect to the changes in surface morphologies. The surface energies increased after UV irradiation resulting in improving of the hydrophilicity. The anodized films formed at low current density or low voltage after UV irradiation showed a low contact angle as well as the film formed at high current density or high voltage.

Keywords: hydrophilicity, low current density, low voltage, UV irradiation

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Authors: Ariadne C. Catto, Luis F. da Silva, Khalifa Aguir, Valmor Roberto Mastelaro

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Zinc oxide (ZnO) pure or doped are one of the most promising metal oxide semiconductors for gas sensing applications due to the well-known high surface-to-volume area and surface conductivity. It was shown that ZnO is an excellent gas-sensing material for different gases such as CO, O2, NO2 and ethanol. In this context, pure and doped ZnO exhibiting different morphologies and a high surface/volume ratio can be a good option regarding the limitations of the current commercial sensors. Different studies showed that the sensitivity of metal-doped ZnO (e.g. Co, Fe, Mn,) enhanced its gas sensing properties. Motivated by these considerations, the aim of this study consisted on the investigation of the role of Co ions on structural, morphological and the gas sensing properties of nanostructured ZnO samples. ZnO and Zn1-xCoxO (0 < x < 5 wt%) thin films were obtained via the polymeric precursor method. The sensitivity, selectivity, response time and long-term stability gas sensing properties were investigated when the sample was exposed to a different concentration range of ozone (O3) at different working temperatures. The gas sensing property was probed by electrical resistance measurements. The long and short-range order structure around Zn and Co atoms were investigated by X-ray diffraction and X-ray absorption spectroscopy. X-ray photoelectron spectroscopy measurement was performed in order to identify the elements present on the film surface as well as to determine the sample composition. Microstructural characteristics of the films were analyzed by a field-emission scanning electron microscope (FE-SEM). Zn1-xCoxO XRD patterns were indexed to the wurtzite ZnO structure and any second phase was observed even at a higher cobalt content. Co-K edge XANES spectra revealed the predominance of Co2+ ions. XPS characterization revealed that Co-doped ZnO samples possessed a higher percentage of oxygen vacancies than the ZnO samples, which also contributed to their excellent gas sensing performance. Gas sensor measurements pointed out that ZnO and Co-doped ZnO samples exhibit a good gas sensing performance concerning the reproducibility and a fast response time (around 10 s). Furthermore, the Co addition contributed to reduce the working temperature for ozone detection and improve the selective sensing properties.

Keywords: cobalt-doped ZnO, nanostructured, ozone gas sensor, polymeric precursor method

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Authors: Andrea Cretu, Calin Cadar, Maria Miclaus, Lucian Barbu-Tudoran, Siegfried Stapf, Ioan Ardelean

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Additives and mineral admixtures have become an integral part of cement-based materials. It is common practice to add silica fume to cement based mixes in order to produce high-performance concrete. There is still a lack of scientific understanding regarding the effects that silica fume has on the microstructure of hydrated cement paste. The aim of the current study is to develop high-performance materials with low permeability and high resistance to flexural stress using silica fume and an organosilane. Organosilane bonds with cement grains and silica fume, influencing both the workability and the final properties of the mix, especially the pore size distributions and pore connectivity. Silica fume is a known pozzolanic agent which reacts with the calcium hydroxide in hydrated cement paste, producing more C-S-H and improving the mechanical properties of the mix. It is believed that particles of silica fume act as capillary pore fillers and nucleation centers for C-S-H and other hydration products. In order to be able to design cement-based materials with added silica fume and organosilane, it is necessary first to understand the formation of the porous network during hydration and to observe the distribution of pores and their connectivity. Nuclear magnetic resonance (NMR) methods in low-fields are non-destructive and allow the study of cement-based materials from the standpoint of their porous structure. Other methods, such as XRD and SEM-EDS, help create a comprehensive picture of the samples, along with the classic mechanical tests (compressive and flexural strength measurements). The transverse relaxation time (T₂) was measured during the hydration of 16 samples prepared with two water/cement ratios (0.3 and 0.4) and different concentrations or organosilane (APTES, up to 2% by mass of cement) and silica fume (up to 6%). After their hydration, the pore size distribution was assessed using the same NMR approach on the samples filled with cyclohexane. The SEM-EDS and XRD measurements were applied on pieces and powders prepared from the samples that were used in mechanical testing, which were kept under water for 28 days. Adding silica fume does not influence the hydration dynamics of cement paste, while the addition of organosilane extends the dormancy stage up to 10 hours. The size distribution of the capillary pores is not influenced by the addition of silica fume or organosilane, while the connectivity of capillary pores is decreased only when there is organosilane in the mix. No filling effect is observed even at the highest concentration of silica fume. There is an apparent increase in flexural strength of samples prepared only with silica fume and a decrease for those prepared with organosilane, with a few exceptions. XRD reveals that the pozzolanic reactivity of silica fume can only be observed when there is no organosilane present and the SEM-EDS method reveals the pore distribution, as well as hydration products and the presence or absence of calcium hydroxide. The current work was funded by the Romanian National Authority for Scientific Research, CNCS – UEFISCDI, through project PN-III-P2-2.1-PED-2016-0719.

Keywords: cement hydration, concrete admixtures, NMR, organosilane, porosity, silica fume

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Authors: G. Wagner, R. Herrmann

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Cytotoxic platinum compounds play a major role in the chemotherapy of a large number of human cancers. However, due to the severe side effects for the patient and other problems associated with their use, there is a need for the development of more efficient drugs and new methods for their selective delivery to the tumours. One way to achieve the latter could be in the use of nanoparticular substrates that can adsorb or chemically bind the drug. In the cell, the drug is supposed to be slowly released, either by physical desorption or by dissolution of the particle framework. Ideally, the cytotoxic properties of the platinum drug unfold only then, in the cancer cell and over a longer period of time due to the gradual release. In this paper, we report on our first steps in this direction. The binding properties of a series of cytotoxic Pt(II) oxadiazoline compounds to mesoporous silica particles has been studied by NMR and UV/vis spectroscopy. High loadings were achieved when the Pt(II) compound was relatively polar, and has been dissolved in a relatively nonpolar solvent before the silica was added. Typically, 6-10 hours were required for complete equilibration, suggesting the adsorption did not only occur to the outer surface but also to the interior of the pores. The untreated and Pt(II) loaded particles were characterised by C, H, N combustion analysis, BET/BJH nitrogen sorption, electron microscopy (REM and TEM) and EDX. With the latter methods we were able to demonstrate the homogenous distribution of the Pt(II) compound on and in the silica particles, and no Pt(II) bulk precipitate had formed. The in vitro cytotoxicity in a human cancer cell line (HeLa) has been determined for one of the new platinum compounds adsorbed to mesoporous silica particles of different size, and compared with the corresponding compound in solution. The IC50 data are similar in all cases, suggesting that the release of the Pt(II) compound was relatively fast and possibly occurred before the particles reached the cells. Overall, the platinum drug is chemically stable on silica and retained its activity upon prolonged storage.

Keywords: cytotoxicity, mesoporous silica, nanoparticles, platinum compounds

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Authors: Bilge Bozdogan, Selda T. Sendogdular, Levent Sendogdular

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We report a technique to control chain conformation during the plasticization process to achieve homogeneous and stable thin films, which allows to reduce post-process annealing times along with enhanced properties like controlled irreversible adsorbed layer (Guiselin brushes) formation. In this study, spin coating temperature was considered as a parameter; hence, all equipment, including the spin coater, substrate, vials, and the solution, was kept inside the same heated fume hood where solution was spin-coated after the temperature was stabilized at a desired value. AFM and SEM results revealed severe difference for solid and air interface between ambient and temperature-controlled samples, which suggest that enthalpic contribution dynamically helps to control film stability in a way where chain entanglements and conformational restrictions are avoided before film growing and allowing to control grafting density through spin coating temperature. The adsorbed layer was also characterized with SEM and Raman-spectroscopy technique right after seeding the adsorbed layer with gold nanoparticles. Stabilized gold nanoparticles and their surface distribution manifest the existence of a controllable polymer brush structure. Acknowledgments: This study was funded by Erciyes University Scientific Research Projects (BAP) Funding(Project ID:10058)

Keywords: chain stability, Guiselin brushes, polymer thin film, spin coating temperature

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Authors: Raana Babadi Fathipour

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Food packaging plays a crucial role in protecting food from unwanted external factors. Antibacterial edible films are a promising option for food packaging due to their biodegradability, environmental friendliness, and safety. This paper reviews recent research progress on antimicrobial edible films, focusing on those made from polysaccharides, proteins, and lipids. Polysaccharides and proteins are the primary components of antimicrobial edible films, while lipids primarily serve as plasticizers and carriers for active substances in composite films. For instance, second-generation liposomes have shown great potential as carriers for antimicrobial substances and other bioactive compounds due to their exceptional stability. Furthermore, this paper analyzes recent advancements and future trends in antimicrobial edible films. One promising direction is the integration of antimicrobial edible film materials with delivery systems, such as nanoemulsion and microencapsulation technologies, to ensure stable loading of bioactive substances. Another emerging area of interest is the development of smart and active packaging that allows consumers to assess the freshness of food products without opening the package. pH-sensitive films and smart fluorescent "on-off" sensors for humidity are currently being explored as materials for smart and active packaging to monitor food product freshness, with further exploration anticipated in the future.

Keywords: antimicrobial edible film, biopolymer, antimicrobial agent, encapsulation, antimicrobial assay

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Authors: David Guillermo Piedrahita Marquez, Hector Suarez Mahecha, Jairo Humberto Lopez

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It was necessary to establish which formulation is suitable for the preservation of aquaculture products, that why edible films were made. These were to a characterization in order to meet their morphology physicochemical and mechanical properties, optical. Six Formulations of chitosan and propolis ethanolic extract encapsulated were developed because of their activity against pathogens and due to their properties, which allows the creation waterproof polymer networks against gasses, vapor, and physical damage. In the six Formulations, the concentration of comparison material (1% w/v, 2% pv) and the bioactive concentrations (0.5% w/v, 1% w/v, 1.5% pv) were changed and the results obtained were compared with statistical and multivariate analysis methods. It was observed that the matrices showed a mayor impermeability and thickness control samples and the samples reported in the literature. Also, these films showed a notorious uniformity of the films and a bigger resistance to the physical damage compared with other edible films made of other biopolymers. However the action of some compounds had a negative effect on the mechanical properties and changed drastically the optical properties, the bioactive has an effect on Polymer Matrix and it was determined that the films with 2% w / v of chitosan and 1.5% w/v encapsulated, exhibited the best properties and suffered to a lesser extent the negative impact of immiscible substances.

Keywords: chitosan, edible films, ethanolic extract of propolis, mechanical properties, optical properties, physical characterization, scanning electron microscopy (SEM)

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Authors: Ahmed Tafraoui, Gilles Escadeillas, Thierry Vidal

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The southern Algeria is known for its huge sand dunes that cover part of its territory (Sahara). This sand has features that allow a glimpse of a recovery in the construction field in the form of Ultra High Performance Concrete (UHPC). This type of concrete using a large amount of silica fume, ultra fine addition that gives very high performance but is also relatively rare and expensive. Replacing it with another addition to equivalent properties, such as metakaolin, can also be considered. The objective of this study is to both enhance the sand dunes of Erg south west western Algeria but also reduce manufacturing costs of Ultra High Performance Concrete to incorporating metakaolin to instead of silica fume. Performances to determine mechanical performance are instantaneous, compression and bending. Initially, we characterized the Algerian sand dune. Then, we have to find a formulation of UHPC, adequate in terms of implementation and to replace silica fume by metakaolin. Finally, we studied the actual value of the sand dune. Concrete obtained have very high mechanical performance, up to a compressive strength of 250 MPa, a tensile strength of 45 MPa by bending with the method of heat treatment. This study shows that the enhancement of dune sand studied is quite possible in UHPC, and in particular UHPC bundles and the replacement of silica fume by metakaolin do not alter the properties of these concretes.

Keywords: Ultra High Performance Concrete, sand dune, formulations, silica fume, metakaolin, strength

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