Preparation and characterization of nano-NaX zeolite by microwave assisted hydrothermal method

In the present work, nano-NaX zeolite crystals were synthesized via microwave and conventional hydrothermal methods. The effects of reaction time, temperature and heating method on the characteristics of zeolite nanoparticles such as particle size, crystallinity, morphology, size distribution and surface area were investigated. The prepared NaX zeolite nanoparticles were characterized by the XRD, SEM, DLS, BET and XRF analysis. The results showed that both heating methods produced the NaX zeolite crystals with nano-in size. The microwave heating produced smaller zeolite nanoparticles with relatively narrower particle size distribution, required much shorter heating times and did not significantly change composition or crystallinity, compared with the conventional heating method. It was also observed that the time and temperature of microwave heating had significant effects on the prepared zeolite particles and the pure zeolite X nanoparticles or a mixture of zeolite X and A can be synthesized using the microwave heating method by control of the crystallization time and temperature.     

Synthesis of type A zeolite from mechanoactivated metakaolin mixtures

The zeolite A was synthesized from the mechanically activated solid mixtures of metakaolin, sodium hydroxide and aluminum oxide. The stages of both thermal treatment and hydrothermal crystallization were investigated and optimized. The size of zeolite A particle was directly measured by scanning electron microscopy as well as calculated using the X-ray diffraction spectroscopy data. The thermal stability of the zeolite A was studied by the differential thermal analysis. It was shown that the optimum thermal treatment temperature providing the zeolite A yield of about 65 wt% and the particle size in the range of 0.2–0.3 μm is 600 °C. The furthermore increase in the thermal treatment temperature results in decreasing amount of zeolite A crystalline phase as well as in the formation of nepheline. It was also found that the optimum NaOH concentration providing the zeolite A yield of about 90 wt % and the particle size more than 0.7 μm after the hydrothermal crystallization stage is 2–4 mol/l. The higher alkali concentrations result decreasing amount of the zeolite A phase and cause the recrystallization into the sodalite. The use of KOH in the hydrothermal crystallization stage allows one to obtain the potassium-containing zeolite A by direct synthesis.     

Synthesis of small crystals zeolite NaY

Zeolite NaY with small crystals was hydrothermally synthesized using a two-stage variable-temperature program without the presence of organic templates, structure-directing agent, seeding crystals and other additives. The as-synthesized samples were characterized by X-ray diffraction (XRD), laser particle size analyzer, scanning electron microscopy (SEM), and Fourier-Transformation Infrared (FT-IR) spectroscopy and Raman spectroscopy. The temperature was found to be a crucial factor for the control of the crystal size.     

Synthesis of LSX zeolite by microwave heating

Low silica X (LSX) zeolite was synthesised by traditional and microwave heating. In both syntheses the X zeolite showed high crystallinity and purity, low silicon/aluminium molar ratio and a potassium content per unit cell of around 7 wt.%. Microwave heating decreased the time of synthesis respect to the traditional heating under the same conditions. The reduction of the synthesis time was due to uniformity of the heating stage by microwaves. Microwave heating decreased the nucleation and crystallisation time. Basic catalytic properties were checked in the toluene alkylation with methanol. There were no differences in the catalytic activity for toluene alkylation between both LSX zeolites.     

Mechanochemical synthesis of granulated LTA zeolite from metakaolin

LTA zeolite can be prepared from dry mixes in a vibratory mill with an impact-shear loading conditions. For the synthesis of LTA zeolite, it is necessary to use the anhydrous ingredients (Al₂Si₂O₇–metakaolin, γ-Al₂O₃). The process of synthesis is controlled by X-ray diffraction, IR-spectroscopy, and atomic-force microscopy. The presence of structural water in the initial ingredients (Al₂Si₂(OH)₄–kaolin or Al(OH)₃) leads to the formation of feldshpatoids (nepheline, sodalite). It was established that the process of mechanical activation requires the synthesis of sodium aluminate of cubic and/or tetragonal crystal systems with a lattice parameters close to those for LTA zeolite. These sodium aluminate acts as a steric template for an “assembly” of the zeolite. The presence of sodium aluminate with some other crystal structure results in the formation of sodalite. There is an optimal time of mechanochemical activation, which is determined by the synthesis of sodium aluminate with cubic or tetragonal crystal structure. A model of the mechanochemical synthesis of LTA zeolite was proposed.     

FAU-type zeolite membranes synthesized by microwave assisted in situ crystallization

FAU-type zeolite membranes were prepared by an “in situ aging-microwave synthesis” (AM) method using a clear solution with the molar composition of 70Na₂O: 1Al₂O₃: 20SiO₂: 2000H₂O. After two-stage AM synthesis, a defect-free FAU zeolite layer consisted of uniform zeolite crystals was formed on the support surface. The Si/Al ratio was ca. 1.5. The single-gas permeation and single-liquid vapor permeation properties of the as-synthesized zeolite membranes were investigated. The permselectivity of H₂ and N₂ was as high as 4.25 for FAU-type zeolite membranes. Pervaporation measurements were carried out for the dehydration of ethanol and isopropanol aqueous solutions. FAU-type zeolite membranes displayed relatively high permeation flux and water-selectivity.     

Synthesis of zeolite Li-ABW from fly ash by fusion method

The zeolite Li-ABW was synthesized by fusion method using fly ash as raw material. It comprised alkaline fusion followed by hydrothermal treatment in LiOH·H₂O medium. Crystallinity of zeolite as high as 97.8% was attained under the following conditions: LiOH·H₂O concentration, 3 M; hydrothermal temperature, 180 °C; the corresponding aging time, 12 h. The content of Li-ABW increased at the expense of lithium aluminum silicate or quartz with an increase of LiOH·H₂O concentration. With increasing hydrothermal temperature and aging time, the soluble species re-crystallized and crystalline phase transformation between different zeolites was observed. Scanning electron microscopy (SEM) observation revealed that the obtained zeolite Li-ABW was a rod-like crystal. The pore size distribution curve indicated the presence of mesopores.     

Synthesis of zeolite NaY in anionic, cationic and nonionic emulsions

Zeolite NaY has been first synthesized respectively in the anionic, cationic and nonionic emulsions. The emulsion systems can accelerate zeolite NaY crystallization and in some cases retard the growth of impurity. Compared to the conventional zeolite NaY synthesized in the absence of emulsion, the emulsion-mediated NaY samples show different morphologies, larger surface areas and higher pore volumes depending on the charge nature of the surfactants involved. In particular, the NaY sample synthesized in the nonionic emulsion system presents a hierarchical pore structure with the highest BET surface area of 646.85 m² g⁻¹. The increase of surface areas for the NaY products made in emulsion media is due to the removal of emulsion components occluded in the pore structures through calcination. These features of the NaY zeolites synthesized in emulsion media, such as various product morphologies and high surface areas, may bestow the materials unique catalytic properties in their potential applications.     

Synthesis of KNbO3 nanostructures by a microwave assisted hydrothermal method

One-dimensional nanostructures of KNbO₃ have attracted a great interest in the scientific community, mainly because of their promising application as nanoelectromechanical systems (NEMS). However, the synthesis of KNbO₃ structures becomes complex due to the natural tendency to form non-stoichiometric potassium niobates. In this context, we report on the crystallization of one-dimensional KNbO₃ nanostructures through the reaction between Nb₂O₅ and KOH under microwave-assisted hydrothermal synthesis (M-H). The use of this synthesis method made possible a very fast synthesis of singlecrystalline powders. Based on SEM, TEM and XRD characterizations, the influence of the synthesis time and the reactants concentration in the structure and morphology of the resultant KNbO₃ was established. The conditions that favor the crystallization of nanofingers were determined to be small amounts of Nb₂O₅ and short reaction times.     

Synthesis of wurtzite ZnS nanorods by microwave assisted chemical route

ZnS nanorods were synthesized by microwave assisted chemical method. Polyvinylpyrrolidone (PVP) was used as a capping agent to stabilize the nanostructure. Synthesized ZnS nanorods were characterized by X-ray diffraction (XRD), Energy dispersive X-ray analysis (EDAX), Transmission Electron Microscopy (TEM), UV-visible spectrophotometry (UV), photoluminescence spectroscopy (PL) and Fourier transform Infra-red spectroscopy (FTIR). The results showed that the nanorods have wurtzite phase crystal structure and exhibits near band edge luminescence in the ultra violet region. The diameter of the synthesized PVP capped ZnS nanorods is about 600 nm. The possible growth mechanism of the ZnS nanorods could be attributed to the oriented attachment effect.     

Degradation of 4-chlorophenol by a microwave assisted photocatalysis method

In this work, the degradation of 4-chlorophenol (4CP) under simultaneous microwave assisted UV (electrodeless discharge lamp) photocatalysis technique (MW/UV/TiO2) was investigated. Several factors affecting the degradation of 4CP by MW/UV/TiO2 method, such as the dosage of photocatalysts, the initial pH value of the solutions, gas bubbling, light intensity and addition of H2O2 oxidant, were studied in detail. The synergistic effects between microwave irradiation and TiO2 photocatalysis were also studied. The major intermediates were found to be chlorobenzene, phenol, hydroquinone, benzoquinone and 4-chlorocatechol. Based on the results, a general reaction pathway for the degradation of 4CP was proposed.     

制备条件对TiO2纳米管晶型影响研究

用不同TiO2作原料,在一般水热法和微波法条件下,制备TiO2纳米管,通过TEM、XRD等表征手段,研究了影响合成TiO2纳米管晶型的因素,提出了影响纳米管晶型结构的机理.结果表明,利用不同的原料在一定制备条件下可制得单一晶型的TiO2纳米管.     

Synthesis of zeolite from steel slag and its application as a support of nano-sized TiO2 photocatalyst

Steel slag, commercial waste material containing silica and alumina which are the chemical components elements of zeolite, was used as a source for synthesis of FAU zeolite (Y-zeolite, X-zeolite). Through acid-treatment to remove CaO species from steel slag and hydrothermal treatment, well-crystallized Na type FAU zeolite was obtained. Furthermore the synthesized FAU zeolite was applied as a support of photocatalyst. It was found that hydrophobic surface property of zeolite enhances photocatalytic activity for decomposition of organic pollutants and the zeolite synthesized from steel slag would be applicable as promising support of TiO₂ photocatalyst.     

Synthesis of nano-sized ceria powders by two-emulsion method using sodium hydroxide

In the present study, nano-sized ceria powders were prepared by the two-emulsion method in the presence of aqueous sodium hydroxide. The effect of the ceria precursor concentration and the addition of an aqueous sodium hydroxide on the crystallite size, the size distribution and the morphology of the synthesized powders were investigated. The precipitates were obtained by mixing two water-in-oil emulsions with kerosene containing cerium nitrate aqueous solution and sodium hydroxide aqueous solution. The synthesized ceria powders were characterized by XRD and TEM. The synthesized ceria powders had nearly spherical shape and a uniform crystallite size in a range of 10 to 20 nm depending on the concentration of precursor solution and an addition amount of mineralizer.     

Synthesis and characterization of low-cost zeolite NaA from coal gangue by hydrothermal method

Through this investigation, we have demonstrated a low-cost preparation method of zeolite NaA from coal gangue. The well-developed zeolite NaA of 87.56% crystallinity was successfully prepared by hydrothermal alkali activation method, which required low alkali concentration (1.8 mol/L) compared to other researches (3–6 mol/L). The characterization results of product prepared at different conditions suggest that the purity and crystallinity of zeolite NaA are high at low alkali concentration and longer crystallization time. The Ca²⁺ exchange value of synthesized zeolite attained 265 mg CaCO₃/g compared to commercial zeolite, which is typically 340 mg CaCO₃/g. The basic structure parameters and thermal stability have also been studied. The results suggest that the obtained zeolite has a potential to be used as hard water softening agent. Moreover, the result of Rietveld quantitative phase analysis and Box-Behnken's response surface methodology showed that the weight fraction of zeolite NaA in product can reach 71.9%, and the crystallinity can attain 88.14% at the optimal condition of n(SiO2)/n(Al2O3) of 2.60, NaOH(aq) concentration of 1.86 mol/L at 95 °C for 10.08 h.     

微波辅助法制备镁合金的植酸镁/羟基磷灰石复合涂层及其耐蚀性能

采用微波辅助法在AZ31镁合金表面制备了植酸镁/羟基磷灰石(PA/HA)复合涂层。利用FESEM、EDS、XRD和电化学性能测试等方法表征涂层的表面形貌、物相组成以及耐蚀性能,探究了植酸溶液的pH值对PA/HA复合涂层形貌及耐蚀性能的影响,并通过浸泡实验研究了镁合金及PA/HA复合涂层在模拟体液(SBF)中的降解矿化行为。结果表明:在植酸预处理中,植酸溶液的pH=5.0时制备得到的PA/HA复合涂层表面均匀、无裂纹,与镁合金基底的界面结合良好;并且在此pH值下PA/HA复合涂层包覆镁合金样品的交流阻抗最大,自腐蚀电流密度最小,说明其耐蚀性最好。在SBF中,PA/HA复合涂层能够快速诱导磷灰石的生成,并显著提高镁合金基底的耐蚀性能。     

Simultaneous adsorption of a mixture of paraquat and dye by NaY zeolite covered with alkylsilane

The surfaces of NaY zeolite particles were modified by the alkylsilylation of n-octadecyltrichlorosilane (OTS). Two kinds of modified NaY zeolites were prepared; one with its external surface partially and the other fully covered with alkylsilyl groups. Since the size of OTS is bigger than the pore diameter of NaY, it is attached on the external surface, leaving the internal pore accessible to adsorbate molecules. As a result of alkylsilylation, the adsorption properties of these sorbents were improved. The adsorption properties of these materials were tested by their reaction in a mixture of paraquat and blue dye. The results demonstrate that the alkysilylated NaY materials are capable of simultaneous adsorption of paraquat and blue dye. Paraquat was selectively adsorbed into the internal pore of the zeolite whereas the dye on the externally attached alkylsilyl groups of the sorbent; displaying the unique bimodal amphiphilic character of the alkylsilylated NaY zeolites.     

Synthesis of platinum nanoparticles by aerosol assisted deposition method

An atmospheric pressure aerosol assisted deposition method has been developed to grow highly oriented nanoparticles and thin continuous films of platinum on a variety of substrates for applications such as catalysts including their use in proton exchange membrane fuel cells. Pt nanoparticles with sizes ranging from 4 nm to 78 nm were synthesized on Si, silicon dioxide coated Si substrates and carbon nanotubes. The size and density of the nanoparticles was found to depend strongly on the precursor carrier gas flow rate and deposition time. The particles showed preferential orientation of (111) that was independent of substrate used. The resulting nanoparticles were characterized by Scanning Electron Microscopy, X-ray Diffraction Spectroscopy and X-ray Photoelectron Spectroscopy in order to obtain information about their morphology, crystallinity and composition. The method developed can deposit uniform coatings of highly oriented, pure Pt nanoparticles without the need of any substrate pretreatment such as surface functionalization, deposition of seed layer for electrodeposition on insulating or semiconducting substrates, and without the use of expensive vacuum equipment.     

Creep property of composite solders reinforced by nano-sized particles

In the present work the creep properties of Sn37Pb and Sn0.7Cu based composite solders with nano-sized metallic Cu, Ag and nano-sized oxide Al₂O₃, TiO₂ reinforcement particles have been studied. First, a series of volume percentages of reinforcements were selected for optimizing the content of particles. Then, the composite solder with optimum volume fraction of the reinforcement particles, corresponding to maximum creep rupture life, is selected for investigating the effect of applied stress level and test temperature on creep rupture life of the composite solder joints. In the creep rupture life test, small single-lap tensile-shear joints were adopted. The results indicate that all the composite solders have improved creep resistance, comparing to the eutectic Sn37Pb solder and the Sn0.7Cu lead-free solder. The creep rupture life of the composite solder joints is first increased with the increase in the volume fraction of reinforcement in the composite solders. Then, the creep rupture life is decreased, as the reinforcement content exceeds a certain value. The creep rupture life of the solder joints is decreased with the increase of applied stress and testing temperature. Moreover, the reinforced efficiency of nano-sized Ag particles is the best in all the tested nano-sized reinforcements for the Sn37Pb based and Sn0.7Cu based composite solders, when the particles contents are in their own optimum content.