Untersuchungen in den Dreistoffen: Cr−W−Si und Mo−W−Si

Zusammenfassung Der Schnitt: Me₃Si (Me=Cr, W bzw. Mo, W) wird an Hand heißgepreßter und in Argon homogenisierter Legierungen untersucht; es läßt sich weder das metastabile W₃Si, noch eine W-reiche Mischphase von diesem Typ beobachten. Cr₃Si nimmt bei 1500°C etwa 20 Mol%, W₃Si auf, während Mo₃Si selbst bei 1900°C praktisch kein W₃Si löst (ev. wenige Mol%). Dagegen bestehen lückenlose Mischreihen zwischen den Me₅Si₃-Phasen mit W₅Si₃-Typ. Die grundsätzliche Aufteilung der Phasenfelder ist damit möglich.Mit 2 Abbildungen     

Sol–gel technology and template synthesis in thin gelatin films

Processes of sol–gel technology of template synthesis of 3d-element metal macrocyclic complexes that occurs in thin films of metalhexacyanoferrate(II) gelatin-immobilized matrix implants under their contact with water solutions containing various (N,O,S)-donor atomic and (C=O) containing organic compounds, have been discussed. It was noted that, in a series of cases, sol–gel technology of template synthesis in the given specific conditions allows to realize such metal macrocyclic complexes formation processes that are not typical at the complexing in solutions or solid phase.     

Optical absorption in solution processed thin films of calcia–alumina binary compounds

UV–visible optical spectra were obtained at room temperature in air for solution-processed thin films of 12CaO·7Al₂O₃(C12A7) on the MgO <100> single crystal substrates after the post-deposition heat treatment at 1,100 °C. Two absorption peaks were observed at 5.3 and 6.1 eV and their presence was attributed to the complex electronic structure of C12A7 and its different energy levels due to the extra-framework species and the framework itself. The peak at 5.3 eV is believed to be associated with O²⁻-Cage Conduction Band type transition whereas the Framework Valence Band to Framework Conduction Band transition is responsible for the peak at 6.1 eV. The nature of electronic transition was found to be direct from the analysis due to Tauc’s law.     

Proton conduction in nanopores of sol–gel-derived porous glasses and thin films

Nanoporous glasses and nanoporous thin films were prepared using sol–gel method, and proton conductivities in nanopores of sol–gel-derived porous glasses and thin films are overviewed in this paper. Proton motions inside nanopores were monitored by impedance and nuclear magnetic resonance (NMR) spectroscopies. The impedance data is correlated with the proton motion in bulk scale, whereas NMR data is correlated with that in nanometer scale, respectively. From the comparison of the activation energies obtained from impedance and NMR spectroscopies, percolation of proton conducting path and its relation to the amount of absorbed water molecules are shown. In the case of nanoporous thin films, directions of pores can be controlled by using cationic and non-ionic surfactants. Relationship between direction of pores and proton conductivity is discussed based on impedance test results.     

Sol–gel thin films for optics and photonics

Thin films have wide applications in the area of optics and photonics. Conventional thin film processing is usually followed for deposition, but the sol–gel route is unique as it can be applied very easily in a cost effective way on desired substrates of any shape for specific applications. In this review, the basic optical designs of antireflection, high reflection, different types of optical filters, coloured coatings, etc. have been discussed with some typical examples of sol–gel products. The importance of coloured coatings and low thermal emissivity coatings on window glass has also been highlighted. In addition, the use of sol–gel processing for different types of film formation which are effective for photonic applications such as non-linearity in optics, ferromagnetism in transparent dilute magnetic semiconductors (DMS), generation of quantum dots as phosphor, grating coupler waveguide in optical sensors are discussed. The basic characterizations of a few sol–gel products which may be used for photonic applications have also been highlighted.     

Crystal growth kinetics of Sb2S3 in Ge–Sb–S amorphous thin films

Sb₂S₃ crystal growth kinetics in (GeS₂) _x (Sb₂S₃)_1?Cx thin films (x?=?0.4 and 0.5) have been investigated through this study by optical microscopy in the temperature range of 575?C623?K. Relative complex crystalline structures composed of submicrometer-thin Sb₂S₃ crystal fibers develop linearly with time. The data on temperature dependence of crystal growth rate exhibit an exponential behavior. Corresponding activation energies were found to be E _G?=?279?±?7?kJ?mol^?1 for x?=?0.4 and E _G?=?255?±?5?kJ?mol^?1 for x?=?0.5. These values are similar to activation energies of crystal growth in bulk glasses of the same compositions. The crystal growth is controlled by liquid?Ccrystal interface kinetics. It seems that the 2D surface-nucleated growth is operative in this particular case. The calculated crystal growth rate for this model is in good agreement with experimental data. The crystal growth kinetic characteristic is similar for both the bulk glass and thin film for x?=?0.4 composition. However, it differs considerably for x?=?0.5 composition. Thermodynamic and kinetic aspects of crystal growth are discussed in terms of Jackson??s theory of liquid?Ccrystal interface.     

Initial dynamic thermal dissipation modes enhance heat dissipation in gold nanoparticle–polydimethylsiloxane thin films

Journal of Thermal Analysis and Calorimetry - Plasmonic nanocomposite materials have exhibited value for applications ranging from biological hyperthermia to optical sensing and waveguiding. Energy...     

Fluorescent nanocrystals grown in sol–gel thin films for generic stable and sensitive sensors

Through the sol–gel route, we have well-controlled the preparation of fluorescent organic nanocrystals grown in silicate thin films. This process is based on the confined nucleation and growth of dyes in the pores of wet gels. The resulting nanocomposite sol–gel thin films, coated onto low-cost substrates, exhibit coupled properties: transparency, stability, easy shaping of sol–gel thin films and high fluorescence intensity coming from organic nanocrystals. The sensitivity of the fluorescence intensity of nanocrystals to their environments can be exploited for the development of optical sensors. Indeed, Förster Resonance Energy Transfer can inhibit nanocrystal fluorescence when probe molecules are adsorbed or grafted on the nanocrystal surface after their diffusion through the pores of the sol–gel matrix. We investigated by time-resolved fluorescence spectroscopy the effect of nanocrystal size and probe concentration on the fluorescence quenching in presence of Methylene Blue used in this study as molecular probe. As strong fluorescence quenchings can be achieved, even for low probe concentrations, these hybrid organic–inorganic nanocoposites are promising for the development of sensor devices by increasing their fluorescence contrasts under specific chemical or biological environments.     

Deposition of silica thin films formed by sol–gel method

Deposition of silica thin films on silicon wafer was investigated by in situ mass measurements with a microbalance configured for dip coating. Mass change was recorded with respect to deposition time when the substrate was fully immersed in the silica sol. Mass gain during deposition was higher than predicted from monolayer coverage of silica nano particles. This implied that deposition was facilitated by gelling of the nanoparticles on the substrate. The rate of deposition was enhanced by increasing the particle concentration in the sol and by decreasing the particle size from 12 to 5 nm. Increasing the salt concentration of the silica sol at constant pH enhanced the deposition of the silica particles. Reducing the pH of the sol from 10 to 6 decreased the deposition rate due to aggregation of the primary silica particles.     

Preparation of nanostructured titania thin films by sol–gel technology

This study is concerned with the preparation of hydrolytically active heteroligand complex [Ti(OC₄H₉)_3.61(O₂C₅H₇)_0.39] from titanium butoxide and acetylacetone and with the gel formation kinetics in a solution of this complex upon hydrolysis and polycondensation. Single-layer and double-layer thin films of a solution of this precursor were coated on polished silicon substrates using the dip-coating method. The crystallization of nanostructured titania films during the heat treatment of these xerogel coatings was studied using various protocols; the anatase–rutile phase transition temperature was found to depend on the film thickness. The effects of the precursor solution viscosity on the film thickness and crystallite size were determined.     

Resistive switching behavior in amorphous and crystalline TiO2 thin films by sol–gel process

We present recent studies on amorphous and crystalline TiO₂ resistive switching nonvolatile memory devices. A chemical sol–gel process is demonstrated for preparing amorphous and crystalline TiO₂ thin films with different calcination temperature. Glass/SnO₂:F/TiO₂/Cu sandwich structures are fabricated and their current–voltage characteristics are examined. We found that the switching voltage goes from 4.8 to 3.5 V and the current compliance also drops from 10 to 1 mA when calcination temperatures increased. Smooth surface of TiO₂ thin films are also observed by XRD, AFM and XPS.     

Enhanced photoinduced super-hydrophilicity in sol–gel TiO2 thin films with co-doped Sn/Nb

In this work, Sn and Nb co-doped TiO₂ were coated on glazed porcelain substrates via sol–gel dip coating method. Field emission-scanning electron microscopy, transmission electron microscopy, and UV–vis spectrophotometer were used to evaluate thickness and optical properties of the thin films. Surface chemical state of thin films was examined by atomic X-ray photoelectron spectroscopy. Water contact angle on the film surfaces was measured by a contact angle analyzer under solar light irradiation. The optical results indicated that Sn/Nb dopant in TiO₂ thin film changed the absorption edge from ultraviolet to visible light and exhibited excellent photo-catalytic ability for degradation of methylene blue solution under solar irradiation. Wettability results indicated that Sn and Nb dopant ions had significant effect on the hydrophilicity property of thin films.     

Room temperature ferromagnetism in Mn-doped ZnS nanocrystalline thin films grown by sol–gel dip coating process

Nanocrystalline Zn_1?xMn_xS (x = 0.00, 0.01, 0.02, 0.03, 0.05, and 0.1) thin films having different Mn content were grown by the sol–gel dip coating process. The effect of Mn content on the structural, optical and magnetic properties of Zn_1?xMn_xS nanocrystalline thin films were investigated. X-ray diffraction results showed the presence of single hexagonal phase corresponding to ZnS with a preferred orientation along the ZnS (002) hexagonal plane direction without any detectable secondary phase, suggesting the incorporation of Mn ions into the ZnS lattice. Scanning electron microscope revealed the surface of the nanocrystalline films to be homogeneous and dense and the grains of the film surface were randomly scattered. In ultraviolet–visible measurements, the band gap energy corresponding to the absorption edge estimated were found to be 3.59–3.23 eV depending on the Mn doping ratio. Magnetic measurements showed that a paramagnetic behavior at 5 K and ferromagnetic behavior at 300 K.     

Structural and thermal behavior of polystyrene thin films using ATR–FTIR–NanoDSC measurements

Most studies report a depression of the glass transition temperature in thin polymer films. To gain insight into this behavior, we have simultaneously investigated the structure of materials and their thermal behavior by developing an ATR–FTIR–nano-differential scanning calorimeter (nanoDSC) hybrid instrument consisting of a ZnSe ATR crystal upon which the sample and a DSC-on-a-chip rests. FTIR spectra showed property changes with film thickness; nanoDSC did not. The relative absorbance of an IR peak at 797 cm⁻¹ was found to correlate with aging time in thin films, suggesting that conformational structure of thin films is critical to their thermal behavior.     

Investigation of time-dependent stability and surface defects in sol–gel derived IGZO and IZO thin films

Journal of Sol-Gel Science and Technology - Electrocatalytic hydrogen evolution is an exercisable way to achieve large-scale application of hydrogen energy. It is of great significance to develop...     

Synthesis and properties of Mo and W ions co-doped porous nano-structured VO2 films by sol–gel process

Porous nano-structured vanadium dioxide (VO₂) films doped with Mo and W ions had been synthesized by sol gel process by employing a sol containing ammonium molybdate and ammonium tungstate with the addition of cetyltrimethyl ammonium bromide (CTAB). The effects of molybdenum and tungsten co-doping and CTAB addition on the structure, morphologies, crystalline and optical properties of VO₂ films were investigated systematically in this study. The composition and microstructure were detected by X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy. The Mo and W ions co-doped porous nano-structured VO₂ films showed excellent infrared transmittance (nearly 70 %), large transmittance difference (55 %) before and after the phase transition, low transition temperature (35 °C), wide hysteresis width (22 °C) and fast phase transition. The results suggest that such Mo and W ions co-doped porous nano-structured VO₂ film is an ideal fundamental material for optical data storage.