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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'-dimethylformamide (DMF) as reaction and crystallization solvent, highlighting the possibilities of aerobic condition metal purification through chelation.

Jan 1, 2014

By Chuan-fu Zhang

Li(Nil/3Col/3- xMnl/3)MxO2(M=Ti, Mg) cathode materials were prepared from LiOH?H2O and oxalate precursor. The physical and electrochemical properties were studied by XRD, SEM, cyclic volt-ampere (CV), AC impedance and constant current charge-discharge. The results show that crystal volume of Ti4+ or Mg2+ doped sample is increasing and the electrochemical reaction resistant Rct is decreased at high rate, improving the cyclic performance and rate capability. The effect of Ti4+ doped is better than Mg2+. The sample is well crystallized and simple pure phase with a-NaFeO2 layered structure when doping quantity x=0.025. The second specific discharge capacity of Li(Nil/3Col/3- 0.025Mnl/3)Ti0.025O2 is 143.2mAh/g at 1C,128.0mAh/g at 2C in the voltage of 2.75-4.3V,and still has 140.7mAh/g and 121.7mAh/g after 20 cycles, respectively, keeping 98.25%, 95.07% capacity.

Jan 1, 2009

In order to avoid impurity problem and enhance absorption/desorption kinetics of Mg-based compounds, nanostructured Mg-based compounds were synthesized from Mg, Ni and other elemental nanoparticles produced by hydrogen plasma-metal reaction. XRD and TEM results demonstrate that homogeneous nanostructured Mg-based compounds with less impurity were successfully synthesized by this method. DSC in hydrogen atmosphere, pressure-composition isotherm and the kinetics of hydrogen adsorption/desorption were investigated at different temperatures. The results show that the nanostructured Mg-based compounds can absorb hydrogen in a high speed at a low temperature.

Jan 1, 2005

By B. Q. Xiao

In surfactant flooding, surfactants added are often a mixture of the same type of molecules with different lengths of carbon chains. The relationship between a single, pure surfactant solution and crude oil is seldom studied. Additionally, up to now, alkylbenzene sulfonates are applied widely in surfactant flooding, such as Daqing oilfield, China. A factory producing alkylbenzene sulfonates will enlarge its yield to 20 000 tons per year over there. For the purposes of widening the alkylben-zene sulfonates? application, 16 kinds of pure alkylbenzene sulfonates were synthesized through Friedel-Crafts acylation and Wolff-Kishner reduction reactions, and the compounds? molecular structures were confirmed by 1HNMR and 13CNMR spectra. The factors affecting interfacial tension (IFT), such as, surfactant type, oil composition, electrolyte concentration, and alkali concentration were considered. The synthesized pure surfactants? critical micelle concentration (CMC) and optimal salinity were measured through interfacial tension technique. According to lab experiments results, heavy alkylbenzene sulfonate (2SY) was synthesized in magnifying scale in Jinzhou Wash Chemical Plant and the coretests were conducted using it. The results showed that the homemade heavy alkylbenzene sulfonate (2SY) flooding can improve oil displacement efficiency 20% more than water flooding at surfactant?s concentration from 0.05%(wt) to 0.2 %(wt).

Jan 1, 2014

By Yu-ren Jiang

Novel compounds of hydroxycarbamoyl carboxylic acids, including 2-hydroxycarbamoyl -3-methlcyclohexane carboxylic acid (HCMC), 2-hydroxycarbamoylmethyl decylen-4-yl carboxylic acid (HCDC) and 2-hydroxycar-bamoylmethyl tridecylen-4-yl carboxylic acid (HCTC) were synthesized. The flotation behaviors of diaspore, kaolinite and illite using these compounds as collectors were investigated. The flotation results revealed that the floatability of the minerals was, in descending order, diaspore and kaolinite, followed by illite, and the ability to collect the minerals was, in ascending order, HCMC and HCDC, followed by HCTC. At a dosage of 2×10-4 mol/L, both HCDC and HCTC show a strong ability to collect diaspore and a weak ability to float kaolinite and illite. The flotation recovery of diaspore is over 90% and that of kaolinite and illite less than 30%. Moreover, Fourier transform infrared spectroscopy (FTIR) spectrum and zeta potential, as well as the adsorption amount, indicated that the adsorption interaction between HCTC and diaspore was primarily a kind of chemisorption in the form of chelate rings, while the interaction between the collector and aluminosilicate mineral was dominated by physisorption. It was concluded that the novel hydroxycarbamoyl carboxylic acid compounds are highly selective collectors for the flotation of diaspore vs. aluminosilicate minerals.

Jan 1, 2011

By Pingchao Ke

A crystalline polyferric sulfate (PFS) adsorbent was synthesized by oxidizing and precipitating ferrous ions under atmospheric conditions. The morphology, structure, composition and specific surface area (SSA) and adsorptive efficacy to As (III) of the adsorbent were characterized by SEM/EDS and TEM images, XRD patterns, FT-IR spectra, BET SSA analyses and adsorption experiments. The adsorbent presents as morphology of near-spherical aggregate and good crystallinity. A small amount of goethite co-precipitated with PFS in the case of the initial ferrous concentration of 1 mol/L and increased the SSA of the aggregates. The absorbent with co-precipitation of goethite showed good adsorption to As(III) and good filtering performance in the high As(III)-content solution of 10–100 mg/L under acidic, neutral and alkaline conditions (pH 2.09–9.01), and its maximal adsorption capacity and adsorption efficiency were 7911 μg/g and 96% separately. After Adsorption, the stability of the absorbents adsorbing As(III) were evaluated by TCLP tests, and the results indicated that the absorbents adsorbing As(III) were extremely stable, and the concentration of arsenic in all leaching solutions were less than 0.01 mg/L.

By Hung-wei Liu, Kevin Plucknett

Early attempts to manufacture titanium aluminides using blended elemental powders, through powder metallurgical processes, have been obstructed due to serious swelling during sintering. Although the use of pre-alloyed powder can avoid this undesired expansion problem, there are limited commercial powder sources available. Therefore, in the present research, fundamental studies on the synthesis of dual-phase (? plus a2) Ti48Al intermetallic materials is undertaken, in particular assessing powder manufacture. In order to produce pre-alloyed powders, highly porous Ti48Al pieces are initially sintered from elemental Ti and Al powder blends, and subsequently pulverised into powders. The powder size is then further reduced by use of either dry or wet milling processes (i.e. shatterbox grinding, attrition, or ball milling). Among these methods, shatterbox grinding has shown the highest efficiency, with a slight mechanical alloying effect observed. The manufactured powder morphologies and phases, as well the sintered material, will be discussed.

Jan 1, 2015

Al2O3,-WC Composite powder for cutting tools was synthesized by self-propagating high-temperature synthesis using A1 powder as a reducing agent. WC, W2C and Al2O3 were concurrently formed in WO3Al-C system. It was found that the complete reaction was achieved with excessive addition of carbon and appropriate processing parameters such as degree of dilution, particle size of aluminum, compaction pressures of green pellets and carbon source. The final product which was leached by 50% HN03+HF diluted solution was consisted of Al2O3-55wt% WC having 2-3um of mean particle size.

Jan 1, 1999

By S Serp, M Duchateau, P Chevreux

Molten salt reactor (MSR) is a promising advanced reactor system aiming to the transmutation of minor actinides such as americium in order to reduce the inventory of ultimate nuclear waste. The fuel is a molten salt in which actinides are homogeneously dissolved in the liquid phase. A chloride salt may be retained for this concept, as it provides low melting point, high solubility of actinides, harder neutron spectrum. To avoid corrosion and precipitation issues, molten salt composition has to be carefully controlled with impurity content as low as possible. Obtaining pure actinide chlorides without contaminants such as oxide, oxychloride, hydroxide and water is still a challenge. To prepare actinide-bearing salt, the chlorination of actinides oxides was investigated in an unstirred reactor under flowing gas as solid-gas reaction. The carbochlorination of PuO2 were performed in the temperature range of 600 to 800°C with chlorine gas as a chlorinating agent and the presence of solid carbon. PuCl3 was successfully synthesised by this method and characterised by X-ray diffraction measurements but some impurities such as oxide phase remain inside the formed product. Refinements of anhydrous and hydrated PuCl3 phases by Le Bail method were also performed for crystalline materials definition. Conversion mainly depends on the chlorinating temperature and the contact between the oxide and the chlorinating agent. A conversion value of 70–80 per cent was achieved at 700°C from PuO2 with quite high specific surface area. The conversion rate was not improved with increasing the chlorination time. The volatilisation of Pu was observed during the carbochlorination experiments. To avoid a loss of Pu caused by sublimation, the chlorination temperature should be limited to 650°C despite that the conversion of PuO2 to PuCl3 was enhanced by increasing temperature. Both carbochlorination and hydrochlorination of AmO2 were also carried out leading to the formation of AmCl3. These first results suggest that americium oxide was chlorinated more readily than plutonium oxide. The purity of produced PuCl3 and AmCl3 still deserves further investigations.

Jun 19, 2024

By Shigehito Deki

"A new wet process has been developed for the synthesis of various kinds of oxide thin films on various kinds of substrates, even which have complex surface morphology, from aqueous solution. The process was named as the LPD, Liquid Phase Deposition, method, which has some advantages over the conventional dry processes. This process can be applied to an on-site synthesis of advanced materials in the thin film technology. In this paper, some current topics on the synthesis of the composite thin oxide films by the LPD method, are presented.IntroductionGenerally, metal oxide thin films have been made by different preparative processes such as r.f. sputtering, chemical vapor depositon, CVD, laser ablation and sol-gel method, etc [1-3]. Each method has it own advantages and disadvantage. In some cases, the process is not suitable for the preparation of thin film on substrate with large surface area or complex surface morphology, and makes the deposition apparatus complicated and expenisve. By using Liquid Phase Deposition, LPD, method which overcomes some of those problems, metal oxide or hydroxide thin film can be formed on the substrate with large surface area and complex surface morphology, which are immersed into the aqueous solution only at ambient temperature and under atmosphere without any special equipments and high energy. And also, multicomponent oxide thin films can be formed readily by mixing solutions containing the objective metal ions, because it is performed in the aqueous solution which is typically a homogeneous mixing system. This process utilizes ligand-exchange, hydrolysis, equlibrium reaction of metal-fluoro complex species, MF x (x-2n>-, and F consumptive reaction. In the aqueous solution, MFx<x-2n>-is hydrolyzed with water to release F ions by a ligand exchange equilibrium reaction as following;"

Jan 1, 2000

By Hong Ro Lee, Seang Suk Cho, Byung Sun Chun, Chang Whan Won

"The preparation of Al203-SiC-TiC composite powders was studied by SHS process using silica (source of Si02) powder instead of Si which is expensive. And, aluminum powder was used as reducing agent of silica and charcoal activated was used as carbon source. Effects of the molar ratio in raw material mixtures and compaction pressure and initial temperature of reactant on the products and combustion process were studied. The most important variable affecting the synthesis of Al203-SiC-TiC was the molar ratio of carbon. The combustion reaction generated in powder state without preheating. But the unreactants exist in the product on all molar ratio. When the preheating temperature is over 400 °C, the combustion reaction was able to be generated in pellet state. Without preheating, the combustion reaction was possible by Ti02 addition. The optimum condition in this system was the molar ratio of Si02:Ti02:Al:C=2.5:0.5:4:3.1. INTRODUCTIONCeramics have demonstrated a capability as a cutting tool, especially in competition with WC-Co cermets (ceramic-metal composites) as inserts for metal turning and milling operation. The advantage of ceramics compared with carbides is retention of high hardness, strength, and chemical inertness to temperatures in excess of 1000 ·c . This allows use of the ceramics at much higher machining speeds than can be tolerated by carbides. However, the ceramics have lower toughness than the carbide materials, and have only been used successfully in the limited operations of turning and milling. There are several classes of cutting tools. The addition of TiC or PSZ, or both, and reinforcement with SiC overcame the poor fracture toughness and thermal-shock resistance that limited Al203 use in the past [1]."

Jan 1, 1998

By Sutham Niyomwas

Keywords: Al2O3-SiCW, Ceramic Matrix Composite, Carbothermal Reduction, Kaolin The formations of Al2O3-SiCw composite have been obtained in situ by carbothermal reduction of a mixture of kaolin and activated carbon. The reaction temperature was controlled at between 1400°C to 1600°C. The synthesized products were mixtures of alumina and silicon carbide in the form of whiskers. The effects of milling time of precursors and reaction temperature are presented. XRD and SEM analyses indicate complete reaction of precursors to yield Al2O3-SiC as product powders, with the SiC having porous and whisker morphology.

Jan 1, 2005

By H. Hahn, B. H. Kear, K. Kan, S. C. Danforth, G. Skandan, W. Chang

"A new chemical synthetic process for the production of non-agglomeratednano structured ceramic (n-ceramic) powders, starting from metalorganic precursors, is described. The process combines rapid thermal decomposition of a precursor/carrier gas stream in a hot tubular reactor with rapid condensation of the product particle species on a cold substrate. Critical to the success of this Chemical Vapor Condensation (CVC) process are (1) a low concentration of precursor compound in the carrier gas, (2) rapid expansion of the gas stream through an uniformly heated tubular reactor under a reduced inert gas pressure of 1-35 mbar, and (3) rapid quenching of the gas phase nucleated clusters or nanoparticles as they exit from the reactor tube. A wide variety of metal organic precursors is available commercially, all of which can be utilized in the CVC process to produce n-ceramic powders, including single phase, multiphase and multicomponent systems.The CVC process has been used to synthesize non-agglomerated n-SiCxNy and n-ZrOxCy powders, with controlled particle size in the range 2-20 nm. Heat treatment of the assynthesized n-powders in various high purity gas streams causes compositional and structural modifications, including particle purification and crystallization, as well as transformation to a whisker-like morphology. Thus, as-synthesized amorphous n-SiCxNy particles transform to (1) cubic n-SiC particles, when heated in flowing argon at temperatures> 1350 °C, (2) hexagonal n-Si3N4 whiskers, when heated in flowing NH3IH2 at 1400 °C, and (3) cubic nSiC whiskers, when heated in flowing H2 at 1400 °C.Non-agglomerated n-ceramic powders form uniformly dense powder compacts by cold pressing, which can be sintered to theoretical density at temperatures as low as 0.5 Tm' For example, full densification ofn-Zr02 powder compacts under free sintering conditions can be achieved at 1125 °C."

Jan 1, 1994

By Bhavani Kedika, Venkatagiri Noole, Krishna Thotla, Krishna Reddy Chepyala

Cationic lipids are attractive candidates for transgene delivery and expression and are safer alternatives to viral delivery vehicles. Here, we report the design, synthesis, characterization and transgene expression efficacies of a series of chrysin derived cationic lipids. A series of ten lipids of chrysin was synthesized by treating the 7-hydroxy group with dibromoalkane and further substitution of the bromo derivative with alkyl amines. The synthesized lipids were characterized spectroscopically. Parallel screening of the synthesized lipids for in vitro plasmid delivery expressing luciferase led to identification of several leads that demonstrated higher transgene expression when compared to the standard. Transgene expression efficacy was dependent on the chain length of the lipid. The influence of the various physicochemical properties on transgene expression efficacies was investigated. This study indicates that lipids derived from chrysin results in high levels of transgene expression and may be attractive for gene therapy applications.

Mar 1, 2017

By S. N. Ojha, Gouthama, R. K. Mandal

"Spray deposition processing of liquid immiscible alloys, based on AI-Pb and Cu-Pb systems have been investigated. Process variables have been optimized to generate uniform dispersion of ultrafine second phase particles in· the matrix of the primary phase. Mechanisms governing the microstructural evolution in this synthesis methodology are discussed. Results of the present investigation are used to demonstrate that rapid solidification of atomized droplets initially provides a high nucleation rate of the second phase during the liquid phase separation. The solid matrix phase nucleates at a later stage and grows with a high velocity enabling trapping of the dispersed phase. Subsequent alteration in the size and size distribution of the second phase is suggested to arise further during deposition of high velocity droplets. Possible reasons for this effect are brought out. Microstructural features of atomized powders and spray-deposits of these alloys are presented to support the present approach of synthesizing composites. IntroductionIn recent years, synthesis of advanced materials with metastable microstructures and ultra fine dispersion of second phase particles has led to the development of novel techniques of materials processing. The other requirement of such a processing methodology is to achieve near-net shape geometries in less number of processing steps. The solidification processing method via spray deposition route qualifies these criteria. This process primarily involves atomization of a melt by high energy gas jets into spray of droplets which are subsequently propelled by the kinetic energy of the gas towards a deposition substrate to build-up a thick high density preform. Although the concept of spray deposition was pioneered by Singer [1] in the early seventies, the fundamentals of the deposition process has been understood only recently [2-4]. Several benefits of spray deposition processing are by now well established [5,6]. Rapid solidification effects are inherent in spray deposition processing due to high heat exchange rate at the droplet-gas interface and also on the deposition surface by force convection. Since considerable heat extraction occurs from the atomized spray prior to droplet consolidation, a relatively low processing temperature is ensured in this process. As a result deleterious coarsening phenomenon can be minimized. In addition, controlled maneuvering of the substrate provides the capability of the process in producing disc, sheet or tube shape preforms of difficult to work materials in a single operation. A significant improvement in properties, resulting from microstructural homogeneity and refinement in grain size induced by spray deposition has been reported for several alloy systems [7,8]."

Jan 1, 1994