In this work, sol–gel-based non-stick ceramic coating formulations were prepared and coated onto aluminum panels in order to investigate their surface properties. The effect of the addition of optimal amount of fluorine-containing silane compound (FAS) on the surface and adhesion properties were also investigated. The morphology, structure, and elemental chemical composition of the coatings were characterized by scanning electron microscopy, atomic force microscopy (AFM), energy dispersion spectrum (SEM/EDAX), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS), respectively. Moreover, several properties of the coatings such as cross-cut adhesion, hardness, gloss, and contact angle (CA) were determined. When fluorine was introduced, the pencil hardness was increased to 6H. Fluorinated non-stick ceramic coatings were found to have good adhesion on the aluminum substrates.
MgF2 coating solutions were solvothermally treated at 160?°C for different time periods, this procedure induced crystallization and particle growth. Antireflection coatings prepared on glass from these solutions were compared to films derived from untreated precursor material. Ellipsometric porosimetry (EP) was employed to characterize structural features of coatings on glass as function of annealing temperature. Based on precursor solutions that had undergone solvothermal treatment antireflective coatings with a peak transparency exceeding 99% were prepared on PMMA substrates.
Solvothermal treatment of MgF2 precursor solutions results in crystallization of particles that can directly be applied to PMMA substrates for λ/4 antireflective films.
Light-activated antimicrobial coatings were obtained by the covalently immobilizing photo-sensitizers in a hybrid organic/inorganic matrix. These coatings were deposited via sol-gel chemistry using epoxy and methyl functional silanes. The light-activated chromophores used in this study were Methylene Blue, Toluidine Blue O, and Rose Bengal. The immobilized photo-sensitizers did not leach from the coatings. The mechanically durable hybrid coatings comprising 2.5% by weight of Rose Bengal had a good adhesion to the glass surface. These coatings were tested for the photo-deactivation of Escherichia coli and Staphylococcus aureus using illumination by a commercial fluorescent lamp. Log reduction of E. coli and S. aureus were >4 when illuminated by the fluorescent lamp in 1 and 3?h, respectively. Due to its high mechanical durability and chemical resistance, such light-activated hybrid coatings are promising candidates for indoor applications in healthcare facilities.
In this paper, we reported the design and preparation of a double-layer antireflective (AR) coating, which possessed relatively high transmittance at 351, 527, and 1053?nm. The refractive indices and film thicknesses of the under layer and upper layer of the simulated AR coating were determined as 1.27, 95?nm and 1.18, 106?nm, respectively. The under layer of the double-layer coating dip-coated from a mixture of base-catalyzed and acid-catalyzed silica sols had a refractive index of 1.27. The upper layer fabricated by the deposition of methylated silica nanoparticles by simply adding methyltriethoxysilane into the base-catalyzed silica sols possessed a refractive index of 1.18. The hydrophobicity of coatings could be dramatically improved with the water contact angle increasing from 23.4° to 150.0°, and the refractive indices of the pure base-catalyzed silica coatings were easily decreased from 1.20 to 1.12 through the surface treatment of silica nanoparticles. Thus, we have successfully prepared a double-layer AR coating, which had a high transmittance of 99.8%, 96.1%, and 99.7% at 351, 527, and 1053?nm, respectively.
For the first time, the hydrophilicity of hemp shiv was modified without the compromise of its hygroscopic properties. This research focused on the use of sol–gel method in preparation of coatings on the natural plant material, hemp shiv, that has growing potential in the construction industry as a thermal insulator. The sol–gel coatings were produced by cohydrolysis and polycondensation of tetraethyl orthosilicate (TEOS) using an acidic catalyst. Methyltriethoxysilane (MTES) was added as the hydrophobic precursor to provide water resistance to the bio-based material. Scanning electron microscopy (SEM) and focused ion beam (FIB) have been used to determine the morphological changes on the surface as well as within the hemp shiv. It was found that the sol–gel coatings caused a reduction in water uptake but did not strongly influence the moisture sorption behaviour of hemp shiv. Fourier transformed infrared (FTIR) spectroscopy shows that the coating layer on hemp shiv acts a shield, thereby lowering peak intensity in the wavelength range 1200–1800?cm?1. The sol–gel coating affected pore size distribution and cumulative pore volume of the shiv resulting in tailored porosity. The overall porosity of shiv decreased with a refinement in diameter of the larger pores. Thermal analysis was performed using TGA and stability of coated and uncoated hemp shiv have been evaluated. Hemp shiv modified with sol–gel coating can potentially develop sustainable heat insulating composites with better hygrothermal properties.
Nano noble metal coating on surface patterned mesoporous semiconductor thin film can play an important role in enhancing visible light harvesting efficiency (LHE) towards improvement in photoelectrochemical (PEC) activity of the material. In this work, one-dimensional (1D) and two-dimensional (2D) mesoscale surface patterns have been created on sol–gel-based titanium tin oxide (TSO) nanostructured thin film on pure silica/indium tin oxide-coated glass by soft lithography. The TSO film matrix is observed to be mesoporous and semicrystalline as evidenced from the structural characterization by transmission electron microscopy and measurement of atmospheric ellipso-porosimetry, respectively. The 2D patterned film exhibits maximum LHE value in visible wavelength region. Further film surface modification has been carried out by depositing nano Au coating onto the bare patterned TSO films by a low temperature solution technique. Under visible light, a significant improvement in PEC activity is found and the gold-coated patterned 2D film shows higher visible LHE as well as >2.7 times higher photocurrent density than bare 2D film. This facile fabrication strategy can create an avenue toward improvement in LHE vis-à-vis the PEC activity of mesoporous mixed metal oxide semiconductor thin film.
Two series of TiO2 thin films were prepared based on soluble precursor powders: The first run originated directly from an alcohol-based coating solution whereas for the second batch the aqueous precursor powder sol had previously undergone a hydrothermal treatment. The respective microstructures were characterized by electron microscopy, the phase evolution was monitored by X-ray diffraction. Ellipsometric porosimetry (EP) was employed to reveal changes of porosity and pore size induced by thermal treatment of the films.
Soluble TiO2 precursor powders were hydrothermally treated to yield coating solutions. Films from these sols were compared with those directly obtained by dissolving the precursor powders. Results indicate that crystallization to anatase is induced under hydrothermal conditions and the resulting films mostly maintain their porosity throughout thermal treatment. In contrast to that coatings processed from as-dissolved precursor powders undergo more extensive densification
CdO thin films were deposited on glass, quartz, FTO, silicon wafers of p-type and n-type at 200?°C of substrate temperature employing spray pyrolysis technique using nebulizer. As deposited cadmium oxide thin films were analyzed to find crystallite size, morphology of the substrate, elemental composition and band gap using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDAX) and UV–Vis spectrophotometer. Nature of the thin film was found to be polycrystalline with face centered cubic structure with (111) preferential orientation and evaluated structural parameters show significant effect of used substrates. Spherical sized grains were observed on the surface of the thin films using SEM. The EDAX analysis confirmed that cadmium and oxygen were present in the sample. Direct allowed transition with band gap values lying in the range 2.34–2.44?eV for all the films deposited on various substrates. Among, these thin film coated on FTO substrate was found to have high crystallinity with a narrow band gap, which may be more suitable for opto-electronic applications.
The absorption co-efficient spectra and inset of transmittance spectra with wavelength of CdO thin films at different substrates (Glass, Quartz and FTO).
One of the promising candidates to replace the chromate conversion coatings for corrosion protection of aluminium alloy AA7075 are the hybrid sol–gel coatings. In the present work hybrid silica sol–gel coatings doped with cerium nitrate were prepared and characterized. Tetraethoxysilane (TEOS) and 3-glycidoxypropyl-trimethoxysilane (GPTMS) were used as precursors. Silica SiO2 (Ludox) particles were added to achieve a barrier properties of coating, while Ce(NO3)3·6H2O was added in order to obtain an active corrosion protection. Optimization of sol synthesis was based on the results of ATR-FTIR spectroscopy and UV–vis–NIR spectroscopy. Opening of epoxy rings and completion of hydrolysis and the condensation reactions during the synthesis process were confirmed. Coatings were characterized through thickness, water contact angle, roughness, adhesion, electrochemical properties (potentiodynamic and electrochemical impedance spectroscopy) and the response to prolonged immersion time in 0.1?M NaCl. The high degree of cross-linking of Si–O–Si network structure and high density was achieved during the synthesis of the sol. Moreover, the results showed that the curing process and the incorporation of cerium nitrate into the hybrid sol–gel coating affected to the corrosion properties of the coating. The observed enhancement in corrosion protection properties is attributed to the combination of the barrier properties of the silica matrix with the active protection of the cerium nitrate.
DBTL as neutral polycondensation catalyst was employed to obtain organic modified silanes (ORMOSILs), which were studied as anticorrosive films for aluminum at saline corrosion. The ORMOSILs were synthesized using TEOS as silica precursor, different alkylalkoxysilanes (trimethoxy(methyl)silane, triethoxy(octyl)silane, 3-aminopropyl(triethoxy)silane and DBTL-catalyst were employed under the free solvent sol–gel process. Results of chemical characterization of ORMOSILs coatings show that under SEM technique coatings have homogenous films, and there are a crosslinking between silica and organic modified under the Infrared spectroscopy and 29Si CPMAS-NMR techniques. On the other hand, Brinell hardness and Pull-Off adhesion tests show that all ORMOSILs increase the aluminum surface hardness between 1 and 10%, and the ORMOSILs critical forces for adhesion are in the range of 106–132?N; therefore, the ORMOSILs coatings have an excellent adhesion to aluminum surface, furthermore, the saline corrosion test shows that organic modified silica avoid the pitting aluminum corrosion; corrosion rate decreases about 60–85%; the anticorrosive behavior according to modified-silica was determined as: SiO2–NH2?>?SiO2–Me?～?SiO2–Octyl.
Cobalt (Co) is a potential therapeutic ion used to enhance angiogenesis through a stabilizing effect on hypoxia-inducible factor 1 alpha (HIF-1α), and its incorporation into the structure of bioactive glass is a promising strategy to enable sustained local delivery of Co to a wound site or bone defect. Here Co-releasing bioactive glasses were obtained through the sol–gel method, comparing cobalt nitrate and cobalt chloride as precursors. The effect of using different Co precursors on the sol–gel synthesis and in the obtained bioactive glass structure, chemical composition, morphology, dissolution behaviour, hydroxycarbonate apatite (HCA) layer formation was investigated. When the chloride salt was used as Co precursor, evidence of crystalline cobalt (II, III) oxide (Co3O4) phase formation was found, along with the presence of Co3+ species as evaluated by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), whereas an amorphous glass containing mainly Co2+ species was obtained when the nitrate salt was the Co source. The presence of a crystalline phase decreased the surface area and pore volume of the final glass, consequently reducing the Co-release rate. Evidence of HCA layer formation after immersion in simulated body fluid (SBF) was still found when different precursors were used, although the rate of formation was reduced by the presence of Co. Therefore, this study showed that Co incorporation and the proper selection of the precursor could affect the final material structure, and properties, and should be considered when designing new bioactive glass compositions for tissue engineering applications.
Boron Nitride (BN) particles were functionalized with vinyl-trimethoxysilane (VTMS) and incorporated into a hybrid polymer (ORMOCER®) resin. The thermal conductivity and mechanical properties of the resulting composite were compared to materials prepared using unmodified particles. Results indicate that the chemical bonding between grain surface and ORMOCER® matrix has a pronounced effect on the final performance of the respective compounds.
The surface of BN particles was functionalized prior to their incorporation into a hybrid polymer (ORMOCER®) matrix, thermal, electrical and mechanical properties of the resulting composites were characterized.
The mesoporous silica samples with different concentrations of phosphonic acid groups on the surface were obtained by direct template synthesis. The block-copolymer Pluronic P123 was used as a template, and sodium meta-silicate with diethylphosphatoethyltriethoxysilane as precursors. According to the SAXS diffractograms, mesoporous silica samples have a p6mm hexagonal symmetry. In addition, we used sol–gel method to synthesize xerogel with the same groups for comparison. All samples possess high values of specific surface area 615–730?m2/g and sorption pore volume. FTIR and potentiometric titration methods were used to investigate the surface layer of these samples. Sorption properties of the samples with phosphonic acid groups were studied in respect to a row of metal cations, among which we focused on lead(II), cadmium(II), and dysprosium(III) cations.
New silica-based particles embedding iron were synthesized following a freeze-drying-assisted sol–gel route. The samples were preliminary characterized in view of potential applications as theranostic magnetic resonance imaging (MRI) contrast agents and for hyperthermia treatment. The structural changes induced by iron addition were studied by X-ray diffraction, Fourier transform infrared and electron paramagnetic resonance spectroscopies. The addition of Fe2O3 impedes the SiO2 crystallization denoting that iron plays, in this case, the role of a glass network stabilizer. The composition on surface and nearby was analyzed by X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy both before and after samples immersion in simulated body fluid. The results suggest the nominal composition with 5?mol% Fe2O3 added to 0.7SiO2?0.3Na2O matrix of interest for further investigations as potential MRI contrast agent and hyperthermia vector.
Fiber needle felt–silica aerogel composite was successfully prepared by via sol–gel process based on water glass. The thermal conductivity show V-type variation tendency with the increase of water to Si. Thermogravimetric analysis-differential scanning calorimetry analysis revealed that the thermal stability was up to approximately 390.58?°C. It has been found that the fire hazard of the composites decreased with the increased ratio of water to Si according to the cone calorimeter test, which can be characterized by peak heat release rate, fire performance index, and fire growth rate index. The fiber needle felt/aerogels present greatly improved compressive and flexural strength (elastic modulus: 0.1–0.97?MPa; flexural modulus: 0.33–0.66?MPa) while keeping inherent properties of pure silica aerogel: low bulk density (0.166?g/cm3), low thermal conductivity of 0.0236?W/m·K, and high specific surface area (1091.62?m2/g). As a result, the as-prepared composite shows a great potential to be applied in the thermal insulation field.
An optical biosensor for the determination of catechol, a widely used yet toxic and carcinogenic molecule, is proposed using a crude extract of desert truffle (Terfezia leonis Tul.) as an enzymatic source of tyrosinase. The biosensor is constructed by the immobilization of tyrosinase crude extract in a bi-layered silica gel film prepared by dip-coating of an alkoxide/colloidal silica solution containing the enzyme on glass slide. Encapsulation has a moderate effect of the enzyme optimal pH stability but largely increases its thermal stability. Immobilized enzymes have a higher substrate affinity towards catechol but smaller maximum conversion velocity. The optical biosensor provides a linear response for catechol in the concentration range of 50–400?µM and a limit of detection was 52?µM. AFM studies show that the enzymes impact on the silica gel structure, preventing further deposition of additional layers. Comparison with similar dopamine biosensors points out that the impact of encapsulation on enzymatic activity may depend on the considered substrate.
In sol-gel chemistry, hydrolysis is the key step in the formation of the reactive hydroxide groups that are responsible for the formation of inorganic networks via the occurrence of condensation reactions. Though previous studies have investigated the effect of the hydrolysis conditions on the structure of organically modified silicates (ormosils), no study, to our knowledge, has investigated this variable on the structure of hybrid materials prepared by combinations of an ormosil and a transition metal (TM). Here, we propose to investigate this effect in a hybrid material composed of 3-trimethoxysilylpropylmethacrylate and a zirconium complex. To also highlight the effects of the precursor’s concentrations on the hydrolysis and condensation reactions of the hybrid materials, their relative content was altered along with the hydrolysis degree. The anticorrosion barrier properties were identified by characterisation of coatings deposited on AA2024-T3 substrates and correlation between the structure and the anticorrosion properties of the coatings were performed based on results obtained from structural characterisations (DLS, FTIR, 29Si-NMR, DSC, AFM and SEM) and corrosion testing (EIS and NSS). It is demonstrated that competition in the formation of siloxane and Si-O-Zr bonds takes place and can be controlled by the degree of hydrolysis and the concentration of the zirconium complex. This effect was found to dramatically alter the morphology of the coatings and their subsequent anticorrosion performances. At short-term exposure times, it is found that the most condensed materials exhibited a higher corrosion resistance while over longer periods the performances were found to level. This article highlighted the critical impact of the hydrolysis degree and zirconium concentration on the connectivity of hybrid sol-gel coatings and the impact this has on corrosion performances.
Textiles represent an attractive class of materials for realizing wearable biosensors. Electronic textiles, or smart textiles, describe the convergence of electronics and textiles into fabrics, which are able to sense, compute, communicate, and actuate. As many different electronic systems can be connected to any clothing, a wearable system becomes more versatile, and the user can change its look depending on environmental changes and individual preference. In this review, we want to explain how it is possible to develop the sensing component of a wearable sensor by sol–gel method based on the use of opportune organofunctional trialkoxysilane precursors, such as 3-glycidoxypropyltrimethoxysilane. Results show that the halochromic dyestuffs are completely entrapped in the sol–gel coatings, both through chemical and physical interactions with the textile fabric. Moreover, a certain washing fastness was observed. Sensor films show excellent reproducibility, reversibility, and short response times, with dynamic ranges from pH 4.4–6.0 (Methyl Red), pH 6.0–7.0 (Nitrazine Yellow), and pH 4.5–8.3 (Litmus), respectively.
Rare earth element (i.e.) europium co-doped aluminum zinc oxide (Eu:AZO) thin films were deposited on microscope glass slides by nebulizer spray pyrolysis with different Eu-doping concentrations (0, 0.5, 1, and 1.5%). The deposited films were investigated using X-ray diffraction, AFM, EDAX, FT-Raman, UV–visible, PL, and Hall effect measurements. X-ray confirmed the incorporation of aluminum and europium ions into the ZnO structure. All films have polycrystalline nature with hexagonal wurtzite structure at (002) direction. Topological depictions exhibited minimum surface roughness and low film thickness for pristine AZO thin film. EDAX study authorizes the existence of Zn, O, Al, and Eu in Eu: AZO thin films. Raman spectra exhibited the characteristic of ZnO-wurtzite structure (E2-high) mode at 447?cm?1. The deposited film showed high optical transmittance of ~90% in visible region, and the direct energy gap was around 3.30?eV for pristine AZO thin film. The PL spectra emitted a powerful UV emission situated at 388?nm, and it indicates that the film has good optical quality. The obtained large carrier concentration and less resistivity values are 4.42?×?1021?cm?3 and 3.95?×?10?4?Ω?cm, respectively, for 1.5% Eu-doped AZO thin film. The calculated figure of merit value is 17.29?×?10?3 (Ω/sq)?1, which is more suitable for the optoelectronic device.
Barium zirconium titanate (Ba(ZrxTi1?x)O3, BZT) super smooth thin films are synthesized through modified sol-gel dip coating route on fluorine-doped tin oxide substrates with a suitably low calcination temperature. The Fourier tranformed infrared spectroscopy proves that impurities and starting materials are completely removed in the calcination process. Crystallographic phases of the samples are identified by the X-ray diffractometry and confirms that all samples are crystallized into a single perovskite phase. Introducing zirconium into the structure causes a reduction in dielectric constant of barium titanate. The optical properties of the films are also investigated. The results indicate that all samples are highly transparent and zirconium reduces the absorption coefficient. Moreover, the band gap energy of barium titanate increases when doped with zirconium and the highest band gap energy of about 3.71?eV along with the lowest dielectric constant of 850 at frequency of 100?kHz are obtained in 15 at.% zirconium-doped sample.
