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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 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 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 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 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

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 A. Arenas-Flores, Pandiyan Thangarasu, J. P. Hernández-Lara, F. R. Barrientos-Hernández, J. A. Romero-Serrano, A. Hernández-Ramírez, M. Pérez-Labra

BaTiO3 doped with Gd3+, was synthesized from BaCO3, TiO2, and Gd2O3 as powders using the solid state reaction method (Ba1-xGdxTi1-x/4O3). The milling of the precursors was performed in an agate mortar with acetone as control means and compositions x = 0.001, 0.005, 0.05, 0.15, 0.25, 0.35 Gd3+ (wt%). Firstly, the powder mixture was decarbonated at 900 °C for 8 h, after it was sintered at 1400 °C for 5 h. Tetragonality of synthesized BaTiO3 doped with Gd3+ was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy (RS). Subsequently, the powders sintered were uniaxially compacted cold until to obtain pellets of about 10 mm in diameter; which again were sintered at 1400 °C for 4 h. XRD patterns and Raman spectra results revealed that the crystal phase of the obtained particles was predominately tetragonal BaTiO3.

Mar 1, 2017

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 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 Alaina Mallard, Jannette Chorney, David Hutchins, Grant C. Wallace, Jerome P. Downey

Current commercial processes for producing ceramic carbides require temperatures of 1400–2000 °C and often use extensive milling operations to produce a powder product. A process that could reduce the energy requirements of commercial carbide production could allow for these materials to be implemented in a greater number of applications. In this study, tungstate (WO4 2−) and silicate (SiO3 2−) anions were adsorbed onto activated carbon and converted into silicon carbide (SiC) whiskers and a mixture of tungsten and tungsten carbide (W/WC) crystals via carbothermal reduction using inert and reducing gas atmospheres at temperatures much lower than what is required by current commercial processes (950 °C for W/WC/W2C and 1200 °C for SiC). The adsorption process was statistically-optimized via a central composite response surface analysis using DesignExpert 9. Inductive coupled plasma optical emission spectroscopy (ICP-OES) was used to measure, and optimize, adsorption efficiency while the carburization products were characterized using X-ray diffraction and scanning electron microscopy.

Mar 1, 2017

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 Leiv Kolbeinsen, Vincent Canaguier, Ingeborg-Helene Svenum

The syntheses of stoichiometric iron chromite and chromites with chosen impurity content have been developed using the induction skull melting technique. The aim for this synthetic material is to obtain pure samples to study the carburization by methane-hydrogen gas mixtures. For each synthesis, the parameters influencing the skull melting experiment have been considered. The product phases have been analyzed using X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS). The synthetic material was subsequently pelletized and sintered in argon. The use of excess iron was found to improve the quality of the final product as well as to help the melting. The difference in magnesium content between first and last solids formed seem to indicate a segregation phenomenon, while no evidence could support a similar trend for aluminum substitution in chromite.

Mar 1, 2017

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 T. I. Arbuzova

The present work presents the original data concerning using a high pressure torsion method and a shock wave loading technique to produce compact oxide nanomaterials and investigations of the effect of severe plastic deformation on a microstructure, crystal lattice and stability of these compounds. This allowed us to compare two ways of deformation action that can be characterized as quasi-static and dynamic effect, correspondingly. Particular attention was paid to a stoichiometry and surface composition changes upon severe plastic deformations. A procedure for studying chemistry of the oxide nanomaterials by means of nuclear microanalysis and Rutherford back scattering has been worked through. For surface studies the X-ray photoelectron spectroscopy has been used. It was shown that both distortion methods permit to produce massive nano-scale oxide materials from the coarse-grained powder during a single technological cycle. Bulk nanocrystalline materials based on LaMnO3, TiOy and ZrO2:Y2O3 were obtained by the quasi-static deformation technique. Nanoscaled ceramics of CuO, Mn3O4 and LaMnO3 were produced by the dynamic deformations. The density of the nanoceramics comes to 99%. Size effects and specific imperfection of the nanoceramics obtained lead to a set of particularities of physical properties.

Jan 1, 2006