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By Wantae Kim, Furnia Saito, Qiwu Zhang

"A novel mechanochemical processing technique for the preparation of zeolites from kaolinite in NaOH solution was investigated. Dry and wet mechanochemical treatments combined by subsequent moderate heat treatment could accelerate the synthetic reaction for zeolites from kaolinite. This stimulating process produced zeolite-A and zeolite-X from activated kaolinite at extremely lower reaction temperature than conventionally applied for zeolites production. Conversion to zeolite-A and zeolite-X was strongly dependent on the activated state of kaolinite. Wet mechanochemical treatment modified the chemical composition of activated solids. Rapid dissolution of AIO species rather than SiO ones in the reactant solution was accelerated by wet milling together with NaOH that promoted the formation of zeolite-X of high specific surface area.IntroductionZeolites are a family of hydrated alumina-silicate minerals contains alkali and alkaline earth metals. They have a framework structure that encloses inter-connected cavities occupied by large metal cations and water molecules. Zeolites are characterized for their ability toward ion exchange and reversible dehydration. Properties of them are exploited through commercial productions of particular structural and chemical features. Zeolites are used as commercial uses for catalysis for FCC (fluidized catalytic cracking) of petroleum refining, drying reagents of gases and liquids, and selective adsorbent for pollution control [1-3]. In such purposes, artificially synthesized zeolites are employed, although natural ones are associated with hydrothermal and hot spring alteration of volcanic materials. Commercially, a hydrothermal process has been used for the preparation of zeolite synthesis. This preparation method gives zeolites of high chemical homogeneity and purity, however, this wet-chemistry-based processing is significantly influenced by reaction temperature, pH, concentration, and composition of starting substances [4]."

Jan 1, 2000

By Thamiris Auxiliadora Gonçalves Martins, Isabela Falconi Brandolis Alves, Viviane Tavares de Moraes

Reverse flotation process is a method used for remove impurities from the most abundant iron ore; the itabirite. In this process, amines surfactant are used which may prevent the reuse of water in processes. The Fenton oxidative processes and the synthesis of nanoparticles are highlighted in catalysts application and in organic substances degradation. This study performed the synthesis of copper nanoparticles (CuNPs) to employ them as catalysts of the modified Fenton reaction to degrade an amine surfactant used in reverse flotation and compared with the classic Fenton (Fe2+) reaction. CuNPs were synthesized by chemical reduction, pH 11 with copper sulfate and ascorbic acid. They were characterized by UV-Vis, DRX and DLS and Zeta potential. The nanoparticles had diameters of 125.00 to 17.22nm and stability during 50 days. The tests were prepared with 180mg/L of amine and 1890mg/L of H2O2 in 150 minutes. The degradation was assessed by UV-Vis and FT IR. The results showed that CuNPs degraded 84% of the surfactant while Fe2+ reached 89%. In this way, both processes can be used for surfactant degradation, although the CuNPs method is easier to operate at neutral pH.

Oct 3, 2019

By Liu Yulin, Zhao Yi, Tan Qi, Liu Lei

"Hydrotalcite is one kind of layered double hydroxides, and has special crystal chemical characteristics. Due to its good thermal stability, hydrotalcite used as the PVC heat stablier has attracted scientists’ attention. In this study, nano-hydrotalcite was synthesized by the method of mechanochemistry/crystallization, using brucite, Al(OH)3 and Na2CO3 as raw materials, and added into PVC to investigate the effect of hydrotalcite on thermal stability of composites. The synthesis mechanism was suggested by virtue of XRD, FE-SEM, FT-IR. It has been indicated that at the first of dry milling process, the parical sizes of brucite and Al(OH)3 decrease, while specific surface areas of them increase by the action of mechanical force, until produced amorphous particles. In the process of wet milling, metal ions in the amorphous body, which has high surface energy, can easily react with H2O, and produce the precursor of Mg6Al2(OH)18•4.5H2O, which has the same crystal structure as hydrotalcite. Under the hydrothermal condition, anions of OH- in the interlamination of precursor are exchanged by CO32- in the solution and nano-hydrotalcite is generated at last. The thermal stability was characterized by Congo red method. The results have revealed that hydrotalcite is one kind of long-term heat stabilizer, and residual stability time increase with the rise of added hydrotalcite amounts.INTRODUCTIONHydrotalcite, one kind of anionic clays, has been attracted a great interest for researchers because of their unexpected physical and chemical properties. The general formula is Mg6Al2(OH)16CO3·4H2O, where Mg2+ and Al3+ occupy octahedral positions in the brucite-like layers, and CO32- is an interlayer anion (Hoyo, 2007). Hydrotalcite is widely used in the fields of chemical engineering, materials engineering, environmental protection, medicine, and so forth, owing to its unique capability of adsorbability, ion exchange and thermal stability (Rozov, Berner, & Taviot-Gueho, 2010; Iwasaki, Yoshii, & Nakamura, 2012; Ay, Zümreoglu-Karan, & Temel, 2011; Cavani, Trifiro, & Vaccari, 1991; Li & Duan, 2005; Lin, Wang, & Evans, 2006). As a result, the study on synthesis and application of hydrotalcite has received considerable attentions."

Jan 1, 2016

By Huimin Lu, Min Li, Jinghua Zou

"Zeolitic imidazolate frameworks (ZIFs) are new type of porous materials, form inerratic polyhedral in three-dimensional with large cages and small apertures, and appear structural diversity. Their hole size can be adjusted. These materials have high selective adsorption capacity to carbon dioxide. In this paper, zeolitic imidazolate frameworks were synthesized by solvothermal synthesis method with dimethylformamide (DMF) as solvent and structuredirecting agent, divalent metallic ions as cation, and imidazole as ligand. The crystals were characterized with XRD, SEM for their crystal structures and physical properties, the adsorption of the crystals for carbon dioxide was also tested, and the result suggests that these porous materials have a capacity of 1.35ml/g for storing carbon dioxide at 273 Kelvin under ambient pressure.IntroductionGlobal warming caused by the increase of carbon dioxide in the atmosphere has become one of the main environment problems, contemporary research has focused on ways to slow or stop this trend. CO2 capture has attracted attention due to the potential to trap and sequester large amounts of CO2 from concentrated sources such as power plants [1]. Traditional technologies in capturing CO2 include absorption by aqueous amines [2]. However, utilization of this process is energy intensive and expensive. Carbon dioxide storage materials investigated so far can be divided into two categories: chemical storage adsorbents and physical storage media [3]. The first kind of materials can chemically adsorb carbon dioxide within their structures and need thermal energy to release the adsorbed carbon dioxide. The examples of the chemical adsorbents include aqueous amines, gas-hyperbranched aminosilicas [4]. The physical adsorbents store carbon dioxide by physical adsorption of carbon dioxide at elevated pressure and release the adsorbed carbon dioxide at low pressure. The physical adsorbents that have been investigated for carbon dioxide storage include zeolites, carbonaceous materials and other porous materials. Until recently, a new type of microporous material, known as zeolitic imidazolate frameworks (ZIFs), has been reported as promising adsorbents for carbon dioxide storage [5 ~ 10]."

Jan 1, 2010

By Celaletdin Ergun, Ibrahim Erden, Gurbuz Gunes, Thomas J. Webste, Huinan Liu, Abdurrahman Bahadll

"B, Ti, Ag, AI and Cu substituted hydroxyl apatites were synthesized via precipitation method. Then the samples were air-sintered at 1300°C for 2 hrs and characterized with XRD, SEM, FTIR, and cell adhesion behaviors.IntroductionSynthetic hydroxylapatite (HA, Ca10(P04)6(0H)2) has a similar composition and structure to biological apatite. Therefore, it has been safely and extensively used as an implant material for bone substitute. However, synthetic HA has been used for a various applications including medical or non-medical applications, such as matrices for drug release control, bone cements, tooth paste additive, blood purification agent, monolithic implants or coatings on metallic implants, packing media for column chromatography, gas sensors, catalysis and host materials for lasers and luminescent materials, etc. [1-9].The major factors affecting the performance of HA on these applications are crystal morphology, density, porosity, pore size and distribution, chemical composition, and surface structure. As provided by the high flexibility of the apatite structure a great variety of cationic and anionic species can be substituted into HA structure which is specifically considered as an effective method to modify the properties of HA [10,11]."

Jan 1, 2012

By Lorna Ortiz-Soto

A series of titiania- and silica-supported Au, Pt and Pt-Au catalysts prepared through different synthetic routes have been investigated in terms of their structural properties, adsorption of CO, and catalytic activity for the selective catalytic reduction of NO by propylene and the oxidation of and CO. Catalysts prepared by incipient wetness impregnation from individual Pt and Au precursors, exhibited characteristics very similar to those of monometallic Pt catalysts. This behavior is consistent with a model in which the two metals remain segregated due to their miscibility gap, and only Pt participates in the adsorption of CO and the reactions under consideration. In contrast, catalysts prepared from a Pt2Au4(C=CtBu)8 organo-bimetallic cluster precursor exhibited different behavior both in terms of CO adsorption and their catalytic activity for the three reactions examined. The combination of the kinetic, spectroscopic and structural characterization data suggests that in this case Pt and Au remain intimately mixed in the form of Pt-Au bimetallic particles, and that the presence of Au modifies the behavior of Pt.

Oct 1, 2003

By Gurinder Kaur

Selenium (Se) based materials find wide applications in rectifiers, solar cells, photographic exposure meters, data storage devices, xerography and anticancer agents. They are also used in the glass industry to eliminate bubbles and remove undesirable tints produced by iron. In addition, Se is highly reactive towards a wealth of chemicals that can be potentially exploited to convert Se into other functional materials such as CdSe, ZnSe, Ag2Se. Here, we report a review of structural investigations of Se based materials in glassy and nanostructured forms. Glasses having varying amounts of Se and Tellurium (Te) were doped with group IV and V elements such as antimony and tin. Structural changes accompanying the composition variation were characterized with x-ray photoelectron spectroscopy, differential scanning calorimetry and x-ray absorption near edge spectroscopy. At the same time Se-Te nanoalloys were synthesized in aqueous micellar phase using Na2SeO3/Na2TeO3 as the Se/Te source. Morphology change from nanoparticles to nanoribbons was investigated using Scanning and Transmission Electron Microscopy (SEM/TEM) techniques. Structural investigations were also done for well defined morphologies of Se based nano-biomaterials obtained in the presence of water soluble protein bovine serum albumin (BSA).

Aug 1, 2013

By Youqi Fan

Complicated copper oxalate precursor powder was prepared using ammonium oxalate as precipitating agent in the Cu(II)-C2O42--NH3-NH4+-H2O system. The composition and morphology of the powder are characterized by chemical analysis, X-ray Diffraction (XRD), scanning electron microscope (SEM), infrared spectroscopy (IR). The effects of temperature, copper ion concentration, pH value are investigated. It?s indicated by the experimental results that precursor of copper oxalate is prepared below a critical pH value, whereas the precursor turns to be a complicated copper salt combined with NH3 while over the pH value. Probable chemical formula CuC2O4?x(NH3)?yH2O can be assumed which x and y are relation to experimental conditions. Technological parameters, such as temperature, initial copper concentration and solution pH value, have significant effects on particle size, morphology and dispersion of precursor powder. By controlling certain technological conditions, various morphologies of precursor, pie shape, spindle shape and rod shape can be synthesized.

Jan 1, 2009

By Saurav Kumar, Akshay Kumar, Vinayaka R. Kiragi, M. K. Banerjee, Amar Patnaik, Vinod Kumar

Today’s industrial technology offers to optimize and reutilize the resources available in terms of scum that remains after hot rolling in steel rerolling mills in Rajasthan, India. Vast reserves of low-grade coal exist and tons of mill scale are produced everyday after hot rolling in steel rerolling mills in Rajasthan, India. The present research work aimed to optimize the various parameters of solid-state reduction of mill scale using low-grade coal from Rajasthan, India. This study investigates the effect of reduction temperature (850–950 °C in steps of 50 °C), reduction time (60 to 180 min, in step of 60 min), mill scale size (800– 300 μm), and mill scale to coal ratio (1:1, 1:2 and 1:3) on achievable metallic iron percentage and its metallization. A higher percentage of iron content is obtained at a lower particle size of 300 μm. The structural analysis is carried out on 300 μm mill scales using XRD analysis, which shows the percentage of iron is approximately 63%, and metallization above 80% can be obtained under the reduction temperature at 900 °C for 180 min, for 1:3 ratio (mill scale to coal ratio). The chemical composition of the mill scale is obtained using X-ray fluorescence (XRF), and particle sizes as well as distribution of mill scale are determined by scanning electron microscopy (SEM). The elements present in the mill scale are also verified using EDS, which indicates the presence of a major portion of Fe, followed by Fe2O3, Si, and C, respectively.

Aug 14, 2020

By M. L. Cao

In this study, a montmorillonite organo-intercalation compound (MOIC) was synthesized by using a Na-modified bentonite (NaB) as a matrix and hexadecyltrimethylammonium (HDTMA) bromide as an intercalating reagent under microwave irradiation. The synthesized products were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), organic carbon content measurement, and adsorption density determination. The results show that, at 10% suspension concentration and 10 minutes irradiation in a 130-W microwave oven, the basal spacing d(001) of the synthesized MOIC increases to 2.209 nm from the original 1.218 nm of NaB. The MOIC has much higher adsorptive densities to nitrobenzene and aniline from aqueous solution than the NaB. The adsorption isotherm of nitrobenzene on the MOIC is linear, and the adsorption is mainly the result of nitrobenzene?s preferred partition in MOIC over aqueous solution due to MOIC?s hydrophobicity. The adsorption isotherm of aniline on MOIC follows the Freundlich equation and the increased adsorption is not only the result of aniline?s preferred partition in MOIC over aqueous solution but also that of the MOIC?s surface adsorptions.

Jan 1, 2014

By Sesha S. Srinivasan

Mechanochemical synthesis has been employed to prepare new light weight complex borohydrides, Zn(BH4)2. The thermal calorimetric and gravimetric analysis of these complex borohydrides shows the hydrogen decomposition temperature (Tdec) of about 100° C with theoretical capacity of ~8.0 wt%. This advanced materials based technology is considered to be suitable for attaining the US-DOE grand challenge technical targets. The powder x-ray diffraction analysis of the mechanically milled Zn(BH4)2 exhibits the presence of zinc borate and NaCl phase. The FTIR spectra of BH4-ion in NaBH4 has a characteristic band at 2290 cm-1,whereas in Zn(BH4)2, it occurs at ~2061 cm-1 (bridging B-H bonds) and ~2451 cm-1 (terminal B-H bonds) as well. The reversibility of hydrogen decomposition and recombination process is carried out by PCT measurements with multi-cycling procedure.

Jan 1, 2006

By J. Finch, Wei Zhang

In this paper we describe the synthesis of a new homologous series of linear Polyglycol-based frothers that consist of Ethylene Oxide (EO) and hydroxyl as hydrophilic groups and Propylene Oxide (PO) and alkyl chains as hydrophobic groups. The synthesized frothers were of two types: Alkyl-Ethoxy-Propoxylate (abbrev. CnEOlPOm) and Alkyl-Propoxy-Ethoxylate (CnPOmEOl) giving: (a) different number of groups and chain length, and (b) different locations of the groups. The identities were confirmed by proton nuclear magnetic resonance (NMR) spectroscopy and total organic carbon (TOC) analysis. The characterization of the products was carried out in a bubble column. At steady state, bubble size, gas holdup and water overflow rate were measured as a function of frother concentration. The results indicate that increasing number of PO groups led to significant decrease in bubble size, and increase in gas holdup and water overflow rate. Increasing the alkyl chain length, gave similar but less pronounced trends. There was no impact of increasing the number of EO groups on bubble size but there was an in increase in gas holdup and water overflow rate. Changing the location of the PO and EO group had a significant effect on all three parameters.

Jan 1, 2015

By T. V. Jayaraman, Kranti Kumar, Paul Praveen J., Dibakar Das, A. R. James

"Lead free piezoelectric ceramics with high piezoelectric coefficients are in great demand for sensor and actuator applications. Synthesis and characterization study of one such lead free system, barium zirconate titanate - barium calcium titanate [xBZT-(1-x)BCT] (x = 0.5), via solgel method have been carried out. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the formation of single phase BZT-BCT nanoparticles (<50 nm). The as-synthesized powders were calcined at 1000°C and the powders were pressed into cylindrical pellets. Solid-state sintering of the green pellets at 1550°C for 2 hrs resulted in single phase perovskite structure. Hysteresis loops were obtained which indicates the ferroelectric nature ofBZT-BCT. The bulk ceramic samples with the highest sintered density (~93%) were subjected to electrical poling and the piezoelectric properties ( d33, kp, & i:,) were measured. The structure and piezoelectric properties were investigated and correlated for the given composition of the BZT-BCT system.IntroductionPiezoelectric ceramics are widely used in various sensors and actuators and most of the piezoelectric ceramics, which are presently used, are lead based, which contains at least 60% lead (Pb) by weight. The critical disadvantage of these lead based piezoelectric ceramics is their hazardous effect related to the toxicity of lead, which poses a serious environmental concern starting from their processing to the disposal stage[l]. It is well known that a material to be a good piezoelectric it requires a morphotropic phase boundary (MPB) i.e. the composition induced phase transition between any two ferroelectric phases."

Jan 1, 2013

By S. Gundiah

Preparation of functionalized polymers from the polymerization of monomers and preformed polymers are discussed with a few illustrative examples. The methods of their characterization, with reference to their application in flocculation, are described.

Jan 1, 1987

By Rashmi Ramesh

Zinc oxide nanoparticles and nanostructures form an active area of research in the recent years. It can be doped to modify electronic, optical and other properties. Synthesis and characterization of zinc oxide is of extreme importance in order to understand the structure property relationship in this material which is now being considered of importance next to carbon nanotubes. Microstructure of zinc oxide nanomaterial is extremely sensitive to the preparation conditions. Nanocrystalline pure and Mn and Mg doped zinc oxide samples were prepared by wet-chemical method under different growth conditions. The samples were investigated for crystalline phase, microstructure, morphology and luminescence characteristics. The effect of Mn and Mg doping on the characteristics of ZnO have been discussed.

Jan 1, 2010

By Francisco M. S. Garrido, Fabiano A. C. M. Passos, Carla N. Barbato, Karoline K. Ferreira, Danielle C. Castro, Adriana A. S. Felix, Luiz C. Bertolino, Fernanda A. N. G. Silva, Karla M. A. Simões

Cancrinite and sodalite are characterized by high capacity of adsorption due to its porous structure. The aim of this work was to use kaolin from Borborema-Seridó/Brazil as a source of aluminium and silicon to hydrothermal synthesis of sodalite and cancrinite and to evaluate the best conditions to the formation of these phases. Therefore, kaolin was heated at 700 and 900 °C for 2 h in order to transform kaolinite in metakaolin. Thereafter, experiments with the calcined kaolin’s were carried out between 150 and 230 °C for 30–270 min on a stainless steel pressure vessel using NaOH, Na2CO3 and H2O. The samples were characterized by X-ray diffraction, nuclear magnetic resonance, scanning electronic microscopy, thermogravimetry, and Zeta potential. The most pure sodalite phase was obtained at 230 °C, with the kaolin/NaOH ratio of 1:1, low concentration of Na2CO3 and smaller time of synthesis (30 min). On the other hand, for the synthesis of cancrinite phase at 230 °C, it was necessary to use kaolin heated at 900 °C, a longer time of synthesis (270 min) and a higher concentration of Na2CO3.

Mar 1, 2017

By Selda Ozkan

In this study, a combination of cathodic arc physical vapor deposition (PVD) and molten salt electrolysis methods were used to obtain ZrB2 layers on AISI 304 grade stainless steel surface. Prior to boriding, steel surface was coated with metallic zirconium via cathodic arc PVD method and then the zirconium coated steel was borided by molten salt electrolysis. Well adherent, dense, ZrB2 layers are formed on the substrates. The thickness of the ZrB2 layer showed dependence on the thickness of the metallic Zr coating layer and the time of boriding. During the boriding process the alloying elements of the substrate also took part in the coating structure depending on their diffusion characteristics.

Jan 1, 2010

By Guihong Han, Duo Zhang, Yanfang Huang

Ni2SiO4 was prepared by chemical precipitation process as a novel anode material for lithium-ion batteries. The structure and morphology of further annealed Ni2SiO4 samples were characterized by XRD and SEM analysis. The electrochemical performance including cyclic voltammetric curves (CV), electrochemical impedance spectra (EIS), charge/discharge curves and cycling performances were also determined. The results demonstrated that the crystal structure of the samples is orthorhombic having space group Pmn21. The morphological structure of materials exhibited cubic particles with sizes in the range of 50–80 nm. The first cycle charge capacity of the pure Ni2SiO4 particles reached to 753 mAh g−1 with the coulombic efficiency of 63.8%. The charge capacity remained 305 mAh g−1 at a current density of 100 mA g−1 even after 50 cycles, which is nearly 208% higher than those of the Ni2SiO4 with SiO2 impurity. Ni2SiO4 can be a promising alternative anode material.

Mar 1, 2018

By Guangqing Zhang

The paper presents results of a systematic study of synthesis of titanium oxycarbide and its chlorination. Titanium oxycarbide was produced by carbothermal reduction of titania in hydrogen, argon and helium. Formation of titanium oxycarbide started at 1200°C in all gases. The reduction was the fastest in hydrogen. Formation of titanium oxycarbide in hydrogen was close to completion in 120 min at 1300°C, 60 min at 1400°C and less than 30 min at 1500°C. Reduction in argon and helium progressed at a similar rate and reached 90-95% after 300 min at 1400-1500°C. The chlorination of titanium oxycarbide was ignited at 150-200°C. Chlorine partial pressure and gas flow rate strongly affected the chlorination rate. Chlorination of titanium oxycarbide produced with carbon to titania molar ratio 2.5 at 235-400°C was close to 100% in 30 min.

Jan 1, 2009

By M. Steyn

The coordination compound tetrakis(1,3-diphenyl-1,3-propanediona to)zirconium(IV), [Zr(DBM)4], (DBM = dibenzoyl methane/1,3- diphenyl-1,3-propanedionol) was synthesized and characterized by single-crystal X-ray diffraction. [Zr(DBM)4] crystallizes in the monoclinic space group P21/c (a = 24.769(4) Å, b = 10.216(5) Å, c = 19.314(4) Å, and = 101.541(5)°). The coordination geometry around the zirconium atom, formed by the eight O-donating atoms of the four -diketonates, is found to be a near-perfect square antiprism. Crystal packing is stabilized by C?H... interactions throughout the crystal lattice. This structure is a noteworthy example of the application of ambient condition synthesis of zirconium compounds in N,N&apos;-dimethylformamide (DMF) as reaction and crystallization solvent, highlighting the possibilities of aerobic condition metal purification through chelation.

Jan 1, 2014