Characterization of silica-coated silver nanoparticles prepared by a reverse micelle and hydrolysis–condensation process

Described herein is the synthesis of individually silica-coated silver nanoparticles using a reverse micelle method followed by hydrolysis and condensation of tetraethoxysilane (TEOS). The size of a silica-coated silver nanoparticle can be controlled by changing the reaction time and the concentration of TEOS. By maintaining the size of a silver nanoparticle as a core particle at around 7 nm, the size of a silica-coated silver nanoparticle increased from 13 to 28 nm as the reaction time increased from 1 to 9 h due to an increase in silica thickness. The size of silica-coated silver nanoparticles also increased from 15 to 22 nm as the TEOS concentration increased from 7.8 to 40 mM. The size of a silica-coated silver nanoparticle can be accurately predicted using the rate of the hydrolysis reaction for TEOS. Neither the dispersion nor the film of silica-coated silver nanoparticles exhibited any peak shifting during surface plasmon resonance (SPR) at around 410 nm, whereas, without silica coating, the SPR peak of Ag film shifted to 466 nm.     

Hydrophilization by coating of silylated polyoxazoline using sol–gel process

Hybrid films prepared from TEOS and polyoxazolines (Si–POx–Si) crosslinking agents were coated on different substrates in order to modify their surface properties. The film cohesion and adhesion on substrates were expected through the hydrogen bonding of the polyoxazoline crosslinked network. Low molecular-weight α,ω-unsaturated polyoxazolines (DA-PMOx)s were synthesized by a one step cationic ring-opening polymerization (CROP) of 2-methyl-2-oxazoline (MOx) with a good control over the molecular weight. Based on double thiol-ene coupling (d-TEC) a post-functionalization of DA-PMOx end chains gave in good yield polyoxazoline cross linker (Si–POx–Si). Glass and various polymer substrates (PP, PEI, POM, etc.) were spin coated by the organic–inorganic hybrid films through sol–gel process. AFM, SEM, visible reflectance spectroscopy and contact angle experiments allowed the full characterization of targeted surfaces and demonstrated the efficiency of the polyoxazoline coating.     

Sequencing coagulation–photodegradation treatment of Malachite Green dye and textile wastewater through ZnO micro/nanoflowers

Sequencing coagulation–photodegradation over ZnO micro/nanoflowers was assessed for Malachite Green (MG) dye removal and followed by the MG-containing textile wastewater treatment. The ZnO micro/nanoflowers were prepared using a facile reflux route and analyzed by various characterization techniques. The flower-like morphological structures of ZnO were witnessed through microscopy analyses. X-ray diffraction findings showed that the prepared ZnO samples were highly crystalline with hexagonal wurtzite structure. The operational parameters including type of coagulant, coagulant dosage, solution pH, photocatalyst dosage and light power exerted their individual influences on the removal of MG dye. The CaCO₃ was the best coagulant among the three coagulants tested due to its high formation of precipitates and adsorption of cationic dye molecules. Using CaCO₃ as a coagulant, 88.3% MG removal was obtained at coagulant dosage of 160?mg and solution pH of 9.0. Complete removal of MG was found with 0.5?g?L^?1 ZnO micro/nanoflowers and 105?W light power. The kinetic analysis showed that a Langmuir?Hinshelwood model was in good agreement with dye removal data. Moreover, a complete removal of MG dye and 80.0% of chemical oxygen demand removal over sequencing coagulation–photodegradation were observed for MG-containing textile wastewater treatment. The sequencing coagulation–photodegradation process using ZnO micro/nanoflowers indicated much promise to be an attractive method for textile effluent treatment applications.     

Preparation of scratch resistant superhydrophobic hybrid coatings by sol–gel process

Organic–inorganic hybrid coatings on glass substrates with superhydrophobic properties and with improved scratch resistance were obtained by means of applying a multilayer approach including multiple sol–gel processes. The coatings exhibited a water contact angle (WCA) higher than 150°. Ultraviolet (UV)-curable vinyl ester resins and vinyltriethoxysilane (VTEOS) as coupling agent were employed to increase the adhesion between substrate and the inorganic layers. The surfaces were characterized by means of dynamic contact angle and roughness measurements. Indeed, the occurrence of superhydrophobic behavior was observed. The scratch resistance of the hybrid coatings was tested to evaluate the adhesion of the coatings to the glass substrate. The proposed preparation method for scratch resistant, mechanically stable, superhydrophobic coatings is simple and can be applied on large areas of different kinds of substrates.     

Effect of peptiser species on crystallisation of alumina gel produced by sol–gel process

The present work reports a study on the effect that a peptiser species has on the crystallisation of alumina gel produced by a sol–gel process to help develop a method for producing α-Al₂O₃ at low temperature. The white precipitate of aluminium hydroxide, which was prepared with a homogeneous precipitation method using aluminium nitrate and urea in an aqueous solution, was peptised using various peptisers at room temperature to form a transparent alumina sol. The alumina gel obtained from the alumina sol, which was produced using formic acid as the peptiser, was most dominantly crystallised into α-Al₂O₃ by annealing at 900°C. The optimal [peptiser]/[Al³⁺] (P/A) molar ratio for the crystallisation into α-Al₂O₃ was 0.2. The alumina gel began to crystallise into α-Al₂O₃ with annealing at as low as 500°C when formic acid and a P/A ratio of 0.2 were used.     

Feasibility of manufacturing of Al2O3–Mo HTCC by hybrid additive process

Additive manufacturing processes make it possible to produce increasingly complex 3D parts. In addition, these numerical processes can be usefully used to manufacture ceramic/metal parts of high dimensional resolution with thermal, electrical and electronic properties of interest for applications in the field of power electronics.In this context, a hybrid additive machine was developed to manufacture ceramic/metal parts. This machine consists in the combination of two additive manufacturing processes: stereolithography and robocasting.Using this hybrid process, the feasibility of HTCC components has been demonstrated by building dielectric alumina by stereolithography and molybdenum conductive network by robocasting. Molybdenum-based metallic formulation adapted to the process and allowing to obtain a high conductive metallic network has been developed. The co-debinding and co-sintering cycles have been optimized to minimize the content of residual carbon and to prevent the oxidation of molybdenum. The alumina/molybdenum interface has also been observed to conclude about a possible delamination between these two materials with different thermal expansion coefficients (CTE). Sintered HTCC parts have been characterized in the domain of hyperfrequency. The frequency responses deviate from the simulation due to a lack of dimensional accuracy of the metallic network.     

Use of a design-of-experiments approach for preparing ceria–zirconia–alumina samples by sol–gel process

In this work we successfully obtained ceria–zirconia–alumina samples by the sol–gel technique. These materials were prepared under acidic or basic conditions, using either nitric acid or ammonium hydroxide as the catalyst. A design-of-experiments approach was used in order to optimize the specific surface area, pore structure, and thermal stability of the prepared samples. It was observed that the addition of ceria and zirconia did not affect the formation of γ-Al₂O₃. The highest surface areas and smallest pore sizes were observed for specimens obtained under acidic conditions and with low to intermediate concentrations of cerium and water. The increase of the heat treatment temperature from 600 °C to 1000 °C led to both a decrease of the surface area and an increase of the mean pore size. This behavior is due to the coalescence of pores upon calcination. Samples with a high concentration of ceria showed an expressive thermal instability at high temperatures. On the other hand, the addition of zirconia increased the thermal stability of these materials. In general, samples with improved thermal stabilities were obtained under basic conditions.     

In situ synthesis of ZrB2–ZrC–SiC ultra-high-temperature nanocomposites by a sol–gel process

ABSTRACT

ZrB₂–ZrC–SiC is one of the ultra-high-temperature ceramic composites with excellent properties. In this research, high-purity ZrB₂–ZrC–SiC nanopowders were synthesised using a carbothermal reduction reaction at a relatively low temperature (1370°C) from cost-effective zirconium(IV) chloride by a sol–gel method. The effect of heat treatment temperature on the synthesis of ZrB₂–ZrC–SiC composite powder was studied. X-ray diffractometry results showed that the phases ZrB₂, β-SiC and ZrC were synthesised at 1370°C. The mean crystallite sizes for each of the phases were calculated using the Scherrer method. The specific surface area for the sample calcined at 1370°C was 81.479?m²?g^?1. SEM observation revealed that the particles had a size lower than 250?nm. Backscattered electron image and map analysis with scanning electron microscopy showed that a suitable phase homogeneity was achieved, as confirmed by energy-dispersive X-ray spectroscopy.     

Optimal operation of an integrated bioreaction–crystallization process for continuous production of calcium gluconate using external loop airlift columns

A kinetic model was proposed to optimize the integrated bioreaction–crystallization process newly developed for production of calcium gluconate crystals using external loop airlift columns. The optimal operating conditions in the bioreactor were determined using an objective function defined to maximize the productivity as well as to minimize biocatalyst loss. The optimization of the crystallizer was carried out by matching the crystallization rate to the optimal production rate in the bioreactor because the bioreaction was found to be the rate controlling process. The calcium gluconate productivity under the optimal conditions of the integrated process was obtained by the simulation based on the process model. The productivity of the proposed process was found to be comparable to that of the current batch fermentation process.     

Pretreatment of wastewater by vacuum freezing system in a cool–thermal storage process

Pretreatment of wastewater by freezing under vacuum in a cool–thermal storage process was investigated. Analyses of vacuum freezing and zone melting were made for the estimation of the ice thickness and the solute distribution of ice crystals from which optimum solidification thickness and operating time were determined. It was found that ice sublimation rate played an important role in determining the efficiency and the pay-off of the process.     

Reduction of nitrogen oxides from simulated exhaust gas by using plasma–catalytic process

Removal of nitrogen oxides (NO_x) using a nonthermal plasma reactor (dielectric-packed bed reactor) combined with monolith V₂O₅/TiO₂ catalyst was investigated. The effect of initial NO_x concentration, feed gas flow rate (space velocity), humidity, and reaction temperature on the removal of NO_x was examined. The plasma reactor used can be energized by either ac or pulse voltage. An attempt was made to utilize the electrical ignition system of an internal combustion engine as a high-voltage pulse generator for the plasma reactor. When the plasma reactor was energized by the electrical ignition system, NO was readily oxidized to NO₂. Performance was as good as with ac energization. Increasing the fraction of NO₂ in NO_x, which is the main role of the plasma reactor, largely enhanced the NO_x removal efficiency. In the plasma–catalytic reactor, the increases in initial NO_x concentration, space velocity (feed gas flow rate) and humidity lowered the NO_x removal efficiency. However, the reaction temperature in the range up to 473 K did not significantly affect the NO_x removal efficiency in the presence of plasma discharge.     

Photoluminescence of ZnO layer on commercial glass substrate prepared by sol–gel process

Amorphous ZnO thin film on soda–lime–silica glass substrate was prepared by the sol–gel process at low-temperature processing, i.e., 100 °C. No distinct grain structure was observable in the surface of the film. The photoluminescence spectrum of the ZnO thin film with an intense near band edge emission was observed while the defect-related broad green emission was nearly quenched.     

Formation of nano-ZrO2 by laser surface treatment of ZrB2-SiC–based composite

This study aims at reducing the oxidation by forming a prior-protective-oxide scale by laser-surface-treatment of two ZrB₂-SiC based composites namely ZrB₂-20v/oSiC-2v/oB₄C-0.24v/oC_f (ZSC) and ZrB₂-20v/oSiC-2v/oB₄C (ZS). ANSYS 15.0 was used to determine laser processing regime. Rigorous theoretical calculations provided temperature distribution, laser parameters and resulting laser power densities required to produce tetragonal ZrO₂. Both the theoretical prediction as well as experimentation show that the laser-surface-treatment with the laser power densities of 31.85 and 56.61 W/mm² for 20 and 30 s render formation of nano-tetragonal-ZrO₂ (100–130 nm) at room temperature (RT). Morphology and size of the nano-tetragonal-ZrO₂ grains depends on the laser exposure time. Nano-grain size helps in stabilizing tetragonal ZrO₂ phase at RT without the need of Y₂O₃ addition. Nano-tetragonal-ZrO₂ may facilitate better ability for pegging, prevent scale-spallation and act as thermal barrier coating (TBC).     

Optimization of coagulation–flocculation process for papermaking-reconstituted tobacco slice wastewater treatment using response surface methodology

A coagulation–flocculation process was used to treat papermaking-reconstituted tobacco slice wastewater with polyaluminium chloride (PAC) as coagulant and a cationic polyacrylamide (CPAM) as flocculant. To maximize the reduction of chemical oxygen demand (COD) and color, the jar tests were carried out in the experiments and response surface methodology (RSM) was applied to optimize the process. A central composite design, i.e., a standard approach in RSM, was used to evaluate the effects and interactions of three factors, i.e. PAC dosage, CPAM dosage and pH on the treatment efficiency. Results revealed that the maximum reduction of COD and color could be achieved at an optimal conditions, i.e., PAC = 715 mg/L, CPAM = 4.8 mg/L and pH = 6.6, from which the reduction of COD and color were 67.8% and 77.7%, respectively. The study also showed that the regression equations could be used as the theoretical basis for coagulation–flocculation process of papermaking-reconstituted tobacco slice wastewater. They will be very helpful to flexibly select the appropriate process parameters in the engineering applications     

Enhanced electrical properties of lead-free BNLT–BZT ceramics by thermal treatment technique

Electrical properties of lead-free solid solution ceramics from the Bi_0.4871Na_0.4871La_0.0172TiO₃ (BNLT) and BaZr_0.05Ti_0.95O₃ (BZT) system have been improved by a thermal treatment technique. A modified two step mixed-oxide method was employed for the preparation of the (1?x)BNLT–xBZT ceramics, where x=0.06, 0.09, 0.12 and 0.20. After sintering at 1125 °C for 4 h, the BNLT–BZT ceramics were annealed at 825, 925 and 1025 °C. The annealing treatment caused an increase in dielectric constant of BNLT–BZT ceramics with x≤0.09 mol% and with x higher than 0.09 mol% the dielectric value dropped considerably. The ferroelectric properties of all annealed ceramic samples tend to decrease with increasing annealing temperature as confirmed by the slimmer P–E loops. The piezoelectric coefficient (d₃₃) increased with annealing temperatures and a maximum value of ～170 pC/N was obtained from the ceramic samples annealed at 1025 °C with x=0.02.